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UN CLA SSIFIED NAVSEA—MT—0 133 NL

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“The citation of trade names and names of manufacturers in this

report is not to be construed as official government endorsement
or approval of commerci al produc ts or services referenced herein ” .
 REPORT NO. MT—043
MARCH 1977

A PLASMA

FLAME SPRAY HANDBOOK

A P R OJECT OF TUE
MANUFACTURING TECHNOLOGY PROGRAM
NAVAL SEA SYSTEM S COMMAND

FINAL REPORT

NAVAL ORDNANCE STATION

LOUISVILLE , KENTUCKY 40214

APPROV ED FOR PUBLIC RELEA~i~

DI STRIBUT ION UNLIMITED

_ _ _ _ _ _ _ _ _ _ _
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
 ABS TRACT

The Plasma Spray ing process is a versatile fabrication

techni que used to apply a wide range of coatings on various work—
piece materials. Coatings are applied to restore or attain de-
sired dimensions , to provide electrical or thermal shielding (or
conduction) , or to improve the resistance to abrasion , corrosion ,
or high temperatures. Success in meeting intended goals by Plasma
Spray ing depends on selecting an appropriate coating material and
using cleaning and spraying techniques suitable for the materials
involved. This report provides useful , up-to-date information
about Plasma Spraying both metallic ar1d nonmetallic coatings on
steel and bronze. It discusses the principles and details the
procedures suitable for producing high-quality coatings destined
for severe service applications of interest to the U.S . Navy .

This handbook should be considered a guide , not a bible ,

for planners , designers , and production personnel responsible for
choos ing , app 1~ ing, and evaluating plasma-arc sprayed coatings.
Limitations on space and reliable information , and the variety of
types and applications of coatings , prevented covering some as-
pects of plasma spraying in detail. For such reasons , d iffer-
ences in the types of plasma-spray systems used successfully,
limiting coating thickness , and effects of specific part geome-
tries are not covered comprehensively. Most of the information
in the handbook is directed to engineers overseeing and develop-
ing expertise in plasma-arc spraying.

The handbook is based on experience, published informa-

tion , and experimental data generated on this program . The ex-
perimental work was conducted with seven types of coatings
deposited on the following types of workpiece materials:

A luminum Low-carbon steel

Aluminum bronze 316 stainless steel
K-Mon ci

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FOREWORD

This is the final report of work comp leted u n d e r NAVORDSYS COM

Work Request WR -3 --5961 issued to p r e p a r e a Plasma Sp r a y Handboo k devoted to
naval ordn ance requirements for use by: design engineers , production
engineers , metallurgists , process p l a n n e r s , shop supervisors , p lasma opera-
tors , and inspectors . The handbook was performed u n d e r the direction of the
Naval Ordnance Station , Louisville , Kentucky , throu gh Contract Number
N— 001 97 — 7 3—C—4 0 30 .

The report was p r e p a r e d by Battelle Columbus Laboratories and

has been edited b y the N a v a l Ordnance Station , Lo uisville to insure comp liance
and coordina~~on with t h e total r e q u i r e m e n t s of the N.A VORDSYSCO M Work
Statement .

F u n d i n g was p r o v i d e d by t h e In d u s t r i a l Resources and Facilities

Division ( ORD-047 ) of Naval O r d n a n c e Systems Command u n d e r the ‘d anu-
facturin g Technology Program and w a s comp leted for the N a v a l Sea Systems
Command (SEA-070) .

Acknowledgment is given to the following persons w i t h o u t whose

help this handbook would be incomp lete .

M r . T . 1 . Roseberry Battelle Columbus Laboratories

C o l u m b u s , Ohio 43201

Mr. F. W Boulger B attelle Co l u m b u s L a b o r a t o~ .r i e s

C o l u m b u s , Ohio 43201

‘ This V i a n u f a c t u r i n g T e c h n o l o g y r e p o r t has been

reviewed and is a p p r ov e d

THAD PEAKE
Director , M a n u f a c t u r i n g
Technology [) ep artm ent
N a v a l O r d n a n c e Station
Louisville , K e n t u c k y

111

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TA B LE OF CONTENTS

Section Page
Abstract
Foreword iii
Table of Contents V

L i s t of F i g u r e s and Tables ix
1. INTRODUCTION 1
1.1 Thermal Spray Processes 1
1.1.1 Gas Combustion H e a t i n g 4
1.1.1.1 Powder Flame Spray 5
1. 1.1.2 Fused Powder Flame Spray 5
1.1.1.3 Wire Flame Spray 6
1.1.1.4 Rod Flame Spray 6
1.1. 1.5 D e t o n a t i o n Spray 9
1. 1.2 E l e c t r i c Arc H e a t i n g 11
1 .1 .2 . 1 P l a s m a — A r c Spray 11
1 . 1.2 . 2 E l e c t r i c — A r c Spray 18
1. 1 . 2 . 3 Transferred—Arc Deposition 19 H
1. 1.3 Process and E q u i p m e n t Comparisons 19
2. COATING DESIGN CRITERIA FOR ENGINEERING APPLICATIONS 25
2.1 Coating Selection 25
2 .1.1 Coating Functions 26
2 . 1. 1 . 1 Therma l B a r r i e r 27
2 . 1. 1 . 2 Wear R e s i s t a n c e 30
2 . 1. 1.3 Corrosion Protection 33 H
2 . 1 . 1 .4 E l e c t r i c a l I n s u l a t io n or Conduction 35
2 . 1. 1 . 5 Salvage 36
3. SURFACE PREPA RATION 37
3.1 General Considerations 37
3. 1.1 Bonding M e c h a n i s m s 37
3 . 1 .2 C o a t i n g Stresses 38
3.2 Cleaning 38
3.3 Surface Roughening 39
3 .3 . 1 Bond C o a t i ng 39
3 .3.2 Abrasive Bl asting 40

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3 .3.2 .1 Grit Blasting 41
3.3.2 .2 Shot Peening 47
3.3.3 Macro-Roughening 51
4. MASKING TECHNIQUES AND MATERIALS 53
4, 1 Masking f o r G r i t B l a s t i n g 53
4.2 Masking f o r Plasma S p r a y i n g 55
5. PLASMA-SPRAY DEPOSITION VARIABLES 57
5.1 Arc Gases 58
5.2 Arc Power Level 62
5.3 Powder Sizes and Feeding Rates 64
5.4 Gun-to-Work D i s t a n c e 66
5.5 Spray A n g l e 67
5.6 S u r f a c e Speed of D e p o s i t i o n 70
5 .7 Process Temperature C o n t r o l 71
6. POST-SPRAY FINISHING AND TREATING OPERATIONS . 73
6.1 Sealing 73
6.2 Surface Finishing 76
7. HEALTH AND SAFETY 81
7.1 Dust and Fumes 81
7 . 1.1 Ventilation 82
7 . 1 .2 Respiratory Protection 83
7.2 Gases 84
7.3 Arc R a d i a t i o n 85
7.3. 1 Ultraviolet Radiation 85
7.3.2 Visible Radiation 86
7.3.3 Infrared Radiation 86
7.4 Noise 86
7.5 E l e c t r i c a l Shock 87
7.5.1 Grounding 88
7 .5 .2 I n s u l a t i o n and G u a r d i n g 88
7.6 OSHA S t a n d a r d s 88
8. QUALITY ASSURANCE PROCEDURES 91
8.1 Q u a l i f i c a t i o n Procedures 91
8.2 Powder C h a r a c t e r i z a t i o n 92
8.3 Mechanical Properties 95

vi

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Section Page
8 .3 . 1 Bond S t r e n g t h 95
8 . 3 .2 Shear S t r e n g t h 100
8 .3 . 3 Hardness Tests 101
8.4 Metallographic Examinations 102
8.4.1 Sectioning and Mounting 105
8.4.2 Grinding 105
8.4.3 Polishing 105
8.4.4 Etching 106
8.4.5 Metallographic Evaluation 108
8.5 Coating Porosity 108
8.6 Shot Peening Tests 110
9. GLOSSARY 115
10. REFERENCES 125
11. BIBLIOGRAPHY 129
12. COAT ING DATA SHEE TS 13 3
12.1 Bond St rengths 1 33
12.2 Plasma Spray V a r i a b l e s 133

VT

_ •
 LIST OF FIGURE S AND TABLES
Page
Figure 1. Deformation of Molten or Semimolten Particles .. 3
Resulting From Spray Impacting on a Substrate
Figure 2. Microstruc ture of Typical High Density Spray .. 3
Coating of Tantalum
Fi gure 3 . Typ ical Flam e W i r e Spray System 7
Figure 4. Cross Section of Typ ical Wire or Rod 8
Flame Sp ray Dev ice
Figure 5. Schema ti c of De tonation Sp ray Gun 10
F i g u r e 6. Cross Section of Typical Plasma-Spray Gun . . .. 13
Figure 7. Schemat ic of Typical Electric A rc Spray Device . 18
Figure 8. Schem a t ic of Transferred Arc Depos iti on Process . 20
Figure 9. Schematic Illustrating Principle of a 41
Commo n Type of A i r Blas ting Dev ice
Figure 10. Sketch Illustrating the Princi ple Used 42
in a Suction-Type Air-Blasting System
Figure 11. Schematic Illustrating Principle of an Air . • . 42
Blast ing Sys tem That Can be Employed Wi thout
the Cabine t Ord inar i ly Used to Confine the
Gr i t and Dust
Figure 12. Relationship of Surface Roughness of a Titanium . 44
S u b s t r a t e to Gr it Blas ting T ime a nd P ressure
Figure 13. Schematic of Plasma-Spray System 59
Figure 14. Energy Content of Gases a t Different Temperatures 60
Figure 15. The Effect of Arc Gas Flow on Coating Density . . 61
for O therw i se Constan t Cond itions
Figure 16. Effect of Arc Gas Flow Rate on Spraying 62
Efficiency
Figure 17. Effect of Arc-Power Level on Density of 63
Plasma-Sprayed Coatings for Otherwise
Cons ta n t Cond it i ons
Figure 18. Typical Contour of Spray Deposit 69
Figure 19. Insufficient Pass Overlap 70
Figure 20. Pressure-Testing Apparatus 75
Figure 21. Fixtures for Aligning Specimens for Bond ... 97
Strength Tensile Tests
Figure 22. Test Specimens for Adhesion and Cohesion ... 98
Strength Tests on Thermal-Sprayed Coatings
Figure 23. Round Specimen Used to Determ ine the Shear ... 100
Strength of a Sprayed Coat ing

ix

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Figure 24. Assembled Test Strip and Holder 112
Figure 25. Almen Gage No. 2 112

Table I. Typical Particle Veloc i ties and M aximum . ... 4

Working Temperatures in Thermal Spray Processes
Table II. Properties of Coatings Applied by Detonation . 11
Spray Gun and Plasma A rc Methods
Table II I. Oxygen Contents of Metallic Coatings Plasma- . 15
Sprayed in Air and in an Inert-Gas Shield
Table IV . Properties of Plasma—Arc Sprayed Coatings . . . 16
Deposited in D i f f e r e n t A tmospheres
Table V. Bond Strengths of Titanium—Coated Tungsten .. 17
Su b s t r a t e s Pro duced by Plasma Spray ing With
Two Types of P r o t e c t i v e At mosphe res
Table VI. Effect of Spray ing in Argon-Filled Chamber . . 17
on Contaminants in Titanium Powder
Table V II . Com parison of Therm al Spray Eq u ipment an d . . • 22
Processes
Tab le VIII. Rela t ive Costs for Thermal Spray M ethods ... 23
Table IX. Some Applications of Plasma-Arc Deposits .. . 27
Table X. Thermal Spray Coa ting s A p p l ic at ion and Use . . 28
Table XI. Approximate Melting Points , in Degrees F, . . . 29
of Some M a teri a ls That can be Depos it ed b y
Plasma Sp r a y ing
Table X I I . Thermal a nd Ele ctr ical Ch ar a c t e ri sti cs of . . . 30
Som e M e t a l s Meas ured on Sol id Spec imens a t
Tem peratu res Be tween 65 an d 21 0 F
Table XI II . Some Materials That can be Deposited by .. . . 31
the Plasma-Spray Process
Table IV. Performance Summary of Cylinder Rod Coatings . 32
and B u s h i n g Ma t e r ia l s f o r Use in Hy d r a u l i c
Cylinders
Table XV. Par ti a l Se ries of th e Eleme nts A r r a n ged . . . . 35
in Order of The ir Elec tr omot ive Forces
Table XV I. Bond Strength Da ta for Alumina Coat ing s ... . 46
Plasma Sprayed onto Steel S u b s t r a t e s w ith
V arious Roughnesses
Table XVII . Effects of Surface Preparation Treatments ... 48
and P lasma Sprayed Coatings on Fat igue Life
of 4340 Steel Specimens in Rotating Beam Tests
Tabl e XV I II . T y p i c a l S p e c i f i c a t i o n s f o r Cas t I r o n 49
and Steel Shot for Shot Peening
Table XIX. Effec t of Nozzle Size , A sp ir a t o r S i z e , and .. 51
Nozzle-Work Spacing on Intensity of Shot Peening

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SECTION I

1. INTRODUCTION

1.1 THERMAL SPRA Y PROCESSES

In a thermal-spray process , a material , in the form of

wire , rod , or powder , is heated to a molten or semimolten condition ,
a t o m i z e d , p r o p e l l e d , a n d d e p o s i t e d on ~ w o r k p i e c e or s u b sL r a t e .
In most s p r a y i n g p r o c e s s e s, t h e m a t e r i a l to be d e p o s i t e d is c a r r i e d
to the desired location by a stream of compressed air or inert gas.
T h e r m a l s p r a y i n g t e c h n i q u e s of various types are useful
for apply-
ing a wide variety of materials on various metallic and nonmetallic
substrates. Most metals , oxides , refractory L~..Jmp ound s or cermets ,
and even some organic plastics , can be sprayed by using appropriate
techniques and equipment. A lthouqh ’ spray processes can be used to
build up free-standing objects on fug itive or disposable substrates ,
this report deals only with coating applications.

Coatings are of interest to the Naval Ordnance Station

because they can be used to improve the service performance of many
types of components. Coatings can be applied to restore or attain
desired dimensions , to provide electrical or thermal shielding (or
conduction ), or to improve the resistance to abrasion, corrosion ,
or high temperatures. This report concentrates on Plasma-Arc Spray-
ing because it is a versatile techni que well suited t.o producing
coated components destined for severe service app lications. Almost
any material can he ulasma sprayed. Because the operating tempera-
tures are so high , the process is esuecially appropriate for apply-
ing coatings of refractor’; m aterials such as intermetallic compounds
and ceramics. It is expected , however , that the most common Naval
Ordnance applications will be for restoring dimensions and apply ing
wear-resistant coatings. The information on Plasma-Arc Spray ing
was obtained from publications , experience , and experiments con-
ducted on this proqram. The substrates used in the experiments
included low alloy steel , stainless steel (Type 316) and 606l—Tl
aluminum . The inf orm ~ tion is exuocted to be of interest to de—
si qners in choosino coat in qs and useful for p lanninu and production
personnel responsible for al2p l y i n~ and evaluating coatings on speci-
mens and end items .

This handbook emphasizes the orecautions to be taken in

plasma—spray processes i n order to obtain high-quality coatings .
The basic factors determining the quality of a coatino applied by
any of the common therma l spray processes are

(1) The temperature of the material in the spray,

(2) The velocity of the material in the spray when

it imp inges on the substrat e , and

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 (3) The severity of oxidation of the sprayed mate-
rial and of the substrate during heating,
s p r ay i n g , and c o ol i n q .

Figure 1 shows deformed particles r e s u l t i n g f r o m d i r e c t -

i n g a w e l l — h e a t e d s p r a y o n t o a s u b s t r a t e at a s u i t a b l y h i g h velo-
city. The resultant coating as shown in Fiou re 2 displays a high
theoretical density, a characteristic favoring very strong particle—
to-particle coherence.

A combination of low particle velocity and minimal

particle heating results in less particle deformation U~~ Ofl impact
and c o n s e q u e n t l y low particle-to-particle coherence and in voids
between adjacent particles.

It follows that oxidized spray material particles will

not cohere nearly as well as a clean unoxidized material.

There are seven commonly used thermal—spray processes

that utilize two basic forms of enerv y for melti no materials to be
sprayed. These energy forms are gas combustion and electric arc.

Gas Combustion Heating

( 1) Powder F l a m e Su r a v
(2) Lire F l a m e Sura”
(3) Rod F l a m e S ur a y
(4) D e t o n a t i o n Sp r a y

E l e c t r i c A r c H e a t in 9 ~~~~

( 1) P l a s m a- A r c S p r a y
(2) Electric—A rc Sor ay
(3) Transferred-Arc Deposition

The maximum workinq temperature attainable differs among

therma l spray methods. Furthermore , the typ ical particle velo-
cities of the different methods vary in a threefold range. Both
factors affect the suitability of gas-combustion and arc-heating
m e t h o d s f o r s p e c i f i c a p p l i c a t i o n s . T a b l e I lists typ ical particle
velocities and maximum working temperatures for the principal ther-
mal spray methods.

Oxidation of spray particles is undesirable in the case

of many metallic materials. F’or that reason, rap id heating and
high particle velocities are desirable . Both characteristics are
typical of electric-arc heating and the detonation spray processes .

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FIGURE 1. DEFORMATION OF MOLTEN OR SEMIMOLTEN PARTICLES
RESULTING FROM SPRA i I M P A C T I N G ON A SUBSTRATE

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- Coating

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Steel
Substrate

lOOX 5G0 85
FIGURE 2. MICROSTRUCTURE OF TYPICAL H I G H
DENSITY SPRAY COATING OF TANTALUM

I
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TABLE I. TYPICAL PARTICLE VELOCITIES AND MAXIMUM WORKING

TEMPERATURES IN THERMA L SPRA Y PROCESSES

Particle Working
Velocity, Temperature ,
fp s F
Gas Combustion Heating
Powder Flame Spray 80-120 4600-4800
Wi re Flame Sp r a y
Ceramic Rod Flame Spray 800 5000—5200

Detonation Spray 2400 6000+

Electric Arc Heating

Electric Arc Spray 800 10 ,000—12 ,000
Plasma Spray 1600 20 ,000+
Transferred Arc 1600 20 ,000+

1.1.1 Gas Combustion Heating

The on ly industrially common tvoe of gas combustion pro-

cess used for therma l spraying utilizes oxygen and acetylene to
provide heat to the material to be deposited. The compressed
gases are ord in arily supplied to the tor ch from storage tanks or
cylinders. Acetylene (C2 H 2) burns to provide a hot flame and an
atmosphere suitable fcr welding and spraying applications . Oxygen
is supplied to support combustion. Ordinarily about 60~ perce nt of
the total oxygen comes from pressurized storage and the rest from
the air surrounding the flame . The ratio of acetylene and oxygen
at the tip of the torch controls the temperature and atmosphere
in th e f l a m e .

A low ratio of oxygen to acetylene produces a comparativel y

low flame temperature and a carburizing atmosphere . Conditions of
that type ar e used for solderin g and si lver b raz ing . Com bu sti on
of a n e q u a l ra tio of gases produces a flame temperature near 5400 F
and a reducing atmosphere sometimes used for melting and welding
low—alloy s€ee l . A slightly higher ratio of oxygen to acetylene ,
around 1.1 , produces a neutral flame and slightly higher tempera-
tu r e s , around 5500 F , better suited to processing steel. Flame
te m p e r a t u r e s u p to 6000 F and o x i d i z in g a tmo s p h e r e s res u l t f r o m
increasing the oxygen/acetylene ratio up to 1.75. That ratio can
be u sed for weldin g cop per an d i t s alloy s , but produces oxide slags.
Oxidizing gas-combustion flames are unsuitable for welding steel
or for thermal-spraying materials other than oxides.

F l a m e s pro duced by t h e combus ti on of pro pa ne , n a tural g as ,

or hy d rogen , w it h oxy g en , are seldom used for thermal spray processes.

4
Even under highly oxidizing conditions , flame temperatures are too
low , a r o u n d 5 0 0 0 F .

1.1.1.1 Powder Flame ~pray

Torches for powder flame spray ing have provisions for
adding powder to the gas stream . The powder , carried by a stream
of compressed air , is injected in the flame before it leaves the
torch. The flow of powder is started , by operating a lever on the
handle of the torch , and the material is carried by the compressed
gases through the tip of the torch where the particl es are heated
by t h e f l a m e . I n illOSt cases compressed air is used to carry the
powder. The presence of powder and the propelling air stream
lowers the working temperature of oxyacetvlene flame sprays to
approximately 4600 to 4 8 0 0 F.
Deposition rates for oxyacetylene flame spraying are
relatively high , compared to plasma-spray methods. This gas-combus-
tion heating method is best suited to depositing thin coatings , on
the order of 0.02 in. in thickness. The process is widely used
for hard facing steel and cast iron components. The equi pment for
oxyacetylene flame spraying is relatively inexpensive , on the ord er
of $ 1 00 0 for a manually operated unit.

The major shortcominqs of the powder flame method result

from the hi gh proportion of heat transferred into the substrate or
workpiece during spraying. The marginal available working tempera-
tures and minimal velocities necessitate that the flam e impinge on
the substrate. This is most undesirable because it promotes oxi-
dation of both substrate and coating and requires the utmost care
to avoid cracking and/or spa llinq of the coating .

As a consequence of these conditions inherent in the flame

powder-spray process , coatings produced by this process exhibit a
bond , density, and overall strength that is inferior to coatings
produced by other thermal-spray techni ques. In view of the criti-
cal nature of performance required f rom Naval Ordnance hardware ,
it is recommended that flame powder sprayed coatings be restricted
to dimensional restoration applications where wear or spalling
would not result in malfunction .

1.1.1.2 Fused Powder Flame Spray

This term is used to denote a variation of the conventional

flame spray practices. Certain alloys can be applied with a flame
powder spray device and subsequently fused to the substrate. The
treatment produces a very dense, cast structure with a metal-
lurgical bond to the substrate. These alloys are available as
either nickel- or cobalt-base materials in hardnesses ranging from
Rc 20 to Rc 61. In all cases , the fusible alloys contain approxi-
mately 3 percent of boron , which acts as a flux to minimize oxida-
tion of either the spray alloy or substrate during the fusion

I
treatment. F u s i n g may be a c c o m p l i s h e d by e i t h e r t o r c h h e a t i n g ,
induc ti on hea t in g , or in fu rnaces w i th a vacuum or dry hy dr ogen
atmosphere. The fusion temperature ranges from 1865 F to 2080 F ,
depending upon t he type of alloy use d . Care is neede d in fu sing
to avoid d i s t o r t i o n and contamination of coated components.

1.1.1.3 Wire Flame Spray

This thermal-spray process utilizes an oxyacetylene flame

as a heat source and spray material in wire form . Figure 3 shows
the components of a wire-spray facility and Figure 4 shows the
cross section of a typical wire flame-spray device .

In the process , the spray material in wire form is pulled

or drawn into the spray device by drive rolls that are powered by
an air turbine or in some cases by an electric motor. In both
cases the rate of wire feed is adjustable .

The wire is pushed into the spray nozzle where it is

melted by the oxvacetylene flame . A stream of compressed air
impinges on the molten tip of the wire , atomizing the molten
material and propelling some to the substrate.

In the wire flame—spray process , the oxy ace ty l e n e f l a me

is restricted to a considerabl y smaller diameter than in powder
flame spray , which results in more effective utilization of the
energy (heat) produced by t h e oxyacetylene flame . Consequently,
higher spray rates and , in most cases , coating of superior quality
may be obtained by use of the wire flame-spray process than are
possible with the powder flame—spray techni que. Comparative spray
ra tes , deposit efficiencies , and coating densities are ,not avail-
able; the wire version is more common , especially for coatings
thicker than 0.03 in.

1.1.1.4 Rod Flame Spray

In concept , this thermal—spray process is virtually iden-

tical to the wire flame-spray technique ; the basic difference is
that the spray material is in rod form. Figure 4 shows the arrange-
ment used for feeding a rod into the flame . Sr~me hard facing and
other metallic materials are too brittle to be formed into wire .
Such materi ’als are fed into the torch as cast rods or sometime~ a~
tubes filled with appropriate powders.
The rod spray process is specifically desiqned for the
deposition of oxide coatings. For the most part , th e ceramic rod-
spray process has been replaced by powder flame-spray and plasma—
spray techniques because of monetary and technical considerations.

11

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1. 1 . 1. 5 Detona tion Spr a y

Note : It is believed that Union Carbide Corporation is the

princ ipal u s e r and c o n s i d e r s propr ie ta r y man y of the
deta ils of the process and equipment for detonation
spray ing. (1)

The detonation gun or spray process utilizes the heat and

veloci ty of shock waves cr ea ted by explo ding me te red amou nt s of
oxygen and acetylene in a device similar to the breech of a gun.
The design and operation of the detonation gun has been described
in technical and patent literature. (2,3)

The operation of a detonation spray gun can be described

by reference to Figure 5. That schematic shows that the powder to
be melted and sprayed is injected into the chamber where the con-
trolled detonation takes place. The following sequence of opera-
t ions takes place :

(1) Injection of oxygen , acetylene , and powder

simultaneously ;

(2) Ignition and detonation of the oxyacetylene

mixture by a spark plug ;

(3) Purging the chamber with nitrogen, to pre-

vent premature ignition of the next charge.

This sequence is repeated at a rate of eight cycles per second and

is continuous until the required coating thickness has been
ach iev ed .

The spray material is heated to a molten or semimolten

state as a result of being transported down the barrel of the
detonation device at sonic or supersonic speeds. It is estimated
that temperatures in excess of 6000 F can be generated in this
m anner.

The molten or semimolten particles of spray material in—

p inge on the substrate at a velocity of approximately 2400 fps ,
producing a bond that may be classified as metallurgical.

The characteristically high operating temperatures and

par ti cle v e l o c i ties of the de tona tion spr a y me thod , indicated in
Table I , resul t in unusually high quality coatings. The higher
k i n e t i c e n e r g y of t h e s p r a y p a r t i c l e s causes more d e f o r m a t i o n on
impact. The - thinner particles develop a finer structure and better
particle interlocking . The coatings have higher densities and
stronger bonds to the substrate. Table II p r e s e n t s d a t a support-
ing t h a t view .

The detonation process is primarily utilized for the

deposition of relatively thin (0.004—0.008 in. ) wear or hard surface

~~~~~~ ~~ ~~~~~~
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 TABLE II. PROPERTIES OF COATINGS APPLIED BY DETONATION
SPRAY GUN AND PLASMA ARC M E T H O D S ( 4 )

Spray Method : Gun Plasma Gun Plasma

Coating Composition
Tungsten carbide , percent 85 88 - -
Cobalt , percent 15 12 — -
A l2 0 3, minimum percent — - 99 99

Properties
Vickers hardness 1050 750 1100 825
l
Bond strength (a ) , l O psi > 12 10 10 7.5
Rupture modulus , l0~ psi 100 55 20 20
Elastic modulus , l0~ psi 31 22 14 5.7
Density, q/cm ~ 13.2 12.5 3.4 3.38
Porosity (b) volume p e r c e n t
, 1 2 2 3

(a) V a l u e s d e t e r m i n e d on st -I or a l u m i n u m by ASTM m e t h o d

(b) P o r o s i t y e s t i m a te d ~ ror~ n e la ll o qr ap hic examinations.

coatings. A l t h o u g h t h e q u a l i t y of a d e t o n a t i o n c o a t i ng i s u n s u r -
passed , the cost is nearly twice that of its closest process com-
petitor (plasma spray). Because of economics , coating thicknesses
of approximately 0.010 inch are the norma l limits. Due to these
monetary and te c ’hn ical consideration , the ~etonation coating pro-
cess should be considered only in the event other thermal-spray
processes pr nv to be i n i d e ’ i a t e .

1.1 .2 Electric Arc lh

1.1.2.1 Plasma— Ar c ~ r rr,

The p lasma-arc spray ing me t hod is a modification of the

plasma -arc welding process. A l l ele c t r i c a l a r c s i o n i z e t h e g a s in
the conducting channel separating the two electrodes and form a
plasma . The ionized form of m atter known as nlasma consists of
free electrons , electrically neutral atom s , and positive ions. The
plasma is heated by resistance to the current passing through it.
Compared to gas flames , plasmas have three important advantaqes for
heating particles to be sprayed . The plasma temperature is higher ,
in excess of 20 ,000 F , it provides better heat transfer to other
ob jects , and a nonoxidizing atmosphere is easier to achieve.

Plasma-arc welding and spraying methods are refinements

of gas t u n g s t e n- a r c w e l d i n g p r o c e s s e s . In g a s t u ng s t e n - a r c w e l d i n g

11

L
. .
~~~~~~~~~~~~~~~~~~ --
.
_ _ _ _ _ _ _ _ _ _
 — -_ _ --_ _ -- _ _ _ _ _ _

the arc is e s t a b l i s h e d b e t w e e n t h e t u n g s t e n e l e c t r o de and t h e w o r k ;

the uncons tr icted arc transfers mos t of the hea t need ed for w e lding.
In p l a s m a - a r c processes the a r c is e s t a b l i s h e d between t h e t u n g s t e n
e l e c t r o d e and the n o z z l e or or i f i c e body of the torch (Figure 6). The
arc is c o n s t r i c t e d w i t h i n the torch and t h e p l a s m a d e l i ve r s t h e h e a t
to the work . The constricted arc used for plasma-arc welding con-
f e r s seve ral a d v a n t a ges ove r un co n str ic ted a r c s:

(1) The energy is more concentrated ,

(2) Arc stability is better and dimensional control
is easier , and
(3) Plasma has a higher velocity and heat content.

The same a d v a n t a g e s f a v o r t h e p l a s m a s p r ay p r o c e s s o v e r o t h e r
approaches.

The pl asma-spray process is a well developed , reliable

thermal—spray process for the deposition of coatings. The inherent
versatility and easy contro l of the process permits the deposition
of a wide variety of spray materials including metals , ca rbides ,
ox ides , borides , nitrides , and su icides. ~7ith proper control , t h e
plasma-spray process is even capable of depositing organic plastics
and certain glasses. In general , it may be stated that any material
that does not decompose within 200 F of its melting point may be
plasma sprayed. Of course , precautions must be taken to prevent
the plasma from overheating and degrading the properties of the
substrate.
-

The plasma—arc spraying process can be described by refer-

ence to the sketch in Figure 6. The working region of the spray
gun is watercooled and the orifice body A , constituting the posi-
tive electrode , is made of copper. The nonconsumable electrode B ,
made of tungsten or of tungsten alloyed with thoria or zirconia ,
is t h e c a t h o d e . The copper anode ( p os i t i v e ) a l s o s e r v e s as the
spray nozzle. The plasma arc is produced by direct current supplied
with straight polarity from a c o n s t a n t - c u r r e n t power s up p l y . Recti-
fiers having an open-circuit voltage of 80 to 160 volts and capable
of supplying 50 to 1000 amperes are usually suitable.

The gun also contains channels for supplying two streams

of g a s . The s t r e a m of gas d i r e c t e d t o w a r d t h e t u n g s t e n e l e c t r o d e
forms the plasma arc and leaves through the spray nozzle. That gas
c o n s t r i c t s t h e a r c to f o r m a s t r e a m of ex trem e l y ho t p lasma l e a v i ng
the gun at a h i g h v e l o c i t y . The s k e t c h shows t h a t t h e t e m p e r a t u r e
v a r i e s a p p r e c i a b l y , f r o m a b o u t 14 , 000 to 24 , 000 F , a t d i f f e r e n t loca-
tions in the stream. The gas fed to form the arc-plasma must be
i n e r t and is u s u a l l y r i c h in a r g o n . H e l i u m can be used , but is
seldom t h e p r i m a r y a r c g a s . N i t r o g e n is commonly used , b u t not
when n i t r o g e n a b s o r p t i o n can c a u s e e m b r i t t l e m e n t of t h e c o a t i n g
or s u b s t r a t e . H i g h e r t e m p e r a t u r e s can be a t t a i n e d by a d d i n g 5 to
25 p e r c e n t of h y d r o g e n to the nitrogen or argon arc gas. Flow
r a t e s f o r the a r c gas used f o r p l a s m a sp rayin g ord i nar i ly range

12

- -_ _ - - . - - -. - - .
~~ ~~~~~~~
 - ~~~~~~~~~~~~~~~~~~~~~~~~~~~
_. ~~~~~~~~~~~~~~~~~~~~~~~
— -— --- --
~
- ... -__ -__ _ -. > - —

S P R A Y NOZZL E
OR
ORIFICE BODY
COPPER
ELECTRODE
HOLDER f

-1
~~~~~
TUNGSTEN —
ELECTR O DE

APPROXIMAT E
PLA S MA T E M P E R A T U R ES
1 24 .000 F and up
I
2. 18 .000 to 24 .000 F
.
~~ 3.14 .000 to 18.000 F

ARC GAS
/

ELECT rn CAL ELEC TRICAL

CONNECTION CONNECTION
AN D WATER O UT A N D WAT E R IN

FIGURE 6. CROSS SECTION OF TYPICAL PLASMA-SPRA Y GUN

13

.
_ _ _ _ _ _ _ _ - --- - -
— — _________ — - —.-- -— -

from 80 to 100 cubic feet/hour The second stream of gas ,

(cfh) .

usually ar gon , carries the powder particles to be sprayed . Typi-

c a l l y , the flow rates of the carrier gas range from 15 to 30 cfh .

The plasma spray system includes two other devices not

shown in F i g u r e 6. S i n c e t h e p l a s m a a r c used f o r s p r a y i n g is n ot
s t r u c k to t h e w o r k p i e c e , some other method of initiating a pilot
arc between the two electrodes must be used. For high current
a p p l i c a t i o n s, t h e a r c is u s u a l l y i n i t i a t e d by s u p e r i m p o s i n g a h i g h
frequency current on the main direct current to the electrodes.
The h i g h f r e q u e n c y c u r r e n t is p r o v i d e d by a separate power supply.
In some t y p e s of e q u i p m en t t h e e n e r g y f o r i n i t i a t i n g t h e a r c is
s u p p l i e d by a c h a r g e d c o n d e n s e r .

Plasma spray systems also contain devices for adding con-

trolled and preselected amounts of powder to the carrier gas. The
feeders are calibrated and adjustable to provide powder at the
desired rates from approximately 1 to 20 pounds /hour.

The operations requirod for plasma spraying are:

(1) Start flow of cooling water

(2) Activate suoply of direct current
(3) Start flow of plasma—forming arc gas
(4) I n i t i a t e an a r c
(5) S t a r t i n j e c t i o n of powder—carryin g gas

The controls of commercially available plasma spray systems are

i n t e r l o c k e d so t h a t s p r a y i n g does n o t s t a r t u n t i l t h e f i r s t f o u r
operations have been compieted .

Plasma-arc powder spraying produces much higher qualit y

coatings than the common oxyacetylene processes and can be used for
a wider variety of materials. Oxygen contamination is less of a
problem t h a n i t is i n gas c o m b u s t i o n p r o c e s s e s . The p l a s m a p r o c e s s
is only half as expensive and more widely used than the gas d e t o n-~
tion process. It produces coatings with densities and bond strengths
approaching those of the detonation process and is applicable to
thicker coatings. Plasma-sprayed coatings range from approximately
0 .0 0 5 to 0 . 0 6 0 i n . in t o t a l t h i c k n e s s d e p e n d i n g on t h e a p p l i c a t i o n .
The coating .efficiency, the ratio between the weight sprayed and
the weight deposited , ordinarily ranges from 30 to 80 percent.
With careful control , the metallurgical disturbance to the substrate
can be limited to about 0.005 in. The princi pal drawbacks of plasma-
arc spraying are related to the facts that the equipment is usually
not portable and that the process requires considerable skill and
knowled ge.

Plasma torches are usually adjusted , and nozzles chosen ,

to produce deposits with appropriate widths and a maximum thick-
ness of 0.005 in ./pass. Deposition rates can be varied from 1 to
20 lb/h r , depending on the ma terials and the coating applications.

14

_ _ _ - - -
 _. - _ _ _ _ _ _ _ _ _

In g eneral , deposition rates used for meta ls , on a wei gh t bas is ,

are twice those used for non metals . Because of the high arc tem-
peratures , the plasma torch is particularl y well suited to spraying
oxides and refractory ceramics. Plasma-arc and gun detonation
me tho d s ar e th e on ly f l a m e sp ray ing methods considered acceptable
f?r air craft components , with the possible exception of restoring
dimensions.

Table II shows that properly deposited plasma-sprayed

coatings exhibit usefully high bond strengths and reasonably hi gh
values for elastic modu li and rupture modu li. Nevertheless , until
recently the properties attainable by plasma spray ing were not quite
so good as those produced by the gun detonation process. However ,
the gap in capabilities between detonation gun and plasma spraying
processes has narrowed . The plasma spray equipment has been improved
so particle velocities are two or three times as high as those
typical of older devices. The new supersonic plasma guns produce
higher quality coatings and are especially desirable for spraying
ceramics. The improvements affect costs. Until recently, plasma
spray equipment cost on the order of $10 ,000 , but the new higher-
velocity guns cost twice as much.

Plasma—arc spray ing is ordinarily conducted in air. How-

ever , the powder-carry ing gas mixes with the surrounding air and
increases the oxygen content of the stream and of some metallic
coating materials. The severity of oxidation of molybdenum during
spraying in air has been shown to increase linearly with the dis-
tance between the gun and the substrate. Coatings with little or
no oxygen contamination can he deposited in an enclosure with an
inert atmosphere or by using an inert stream of shielding gas.
Tucker quoted the data in Table III to illustrate the benefits of
the shielding technique . (5) Shroudinq the spray with an inert gas
apparently prevented oxygen pickup by nickel , tungsten , and titanium
coatings and lowered the oxygen levels in the case of copper and
molybdenum deposits.

TABLE III. OXYGEN CONTENTS OF METALLIC COATINGS PLASMA -

SPRAYED IN AIR AND IN AN INERT-GAS SHIELD (5)

Oxygen Content , percent

Conventional Gas-Shielded
Coating Material Powder Coating coating
Copper 0 . 12 6 0.302 0 .092
Nickel 0.172 0.456 0.151
Tungsten 0 .027 0.274 0.030
Molybdenum 0 .4 1 9 0.71 0.160
Titanium 0.655 2 .0+ 0.730

1 5 I
- - I-

Table IV indicates that densities and strengths of aluminum ,

s t a i nl ess steel , and tungsten coatings were better for coatings
sprayed in an i n e r t a t m o s p h e r e t h a n those f o r c o a t i n g s s p r a y e d in
air. Presumably the degradation in properties was caused by oxida-
tion during spray ing .

TABLE IV. PROPERTIES OF PLASMA-ARC SPRAYED COATINGS

DEPOSITED IN DIFFERENT ATMOSPHERES (6)

Tensile Modulus
Atmos- Density , (a) Strength , of Rupture ,
Coating phere percent psi psi

Aluminum Argon 86 5 , 600 -

Air 76 4 , 000 —

Stainless Argon 91 33 , 900 —

Steel Air 84 19 , 2 0 0 —

Argon 90 — 51 , 0 0 0
Tungsten
Air 86 — 29 ,000

(a) Density expressed as a percentage of theoretical value .

Plasma—arc spraying in an argon-atmosphere chamber gives

even better results than using a protective shroud of the same gas.
Suitable spray chambers , made with double walls to permit water
cooling during service , can be evacuated to pressures of 10~~ m m o f H g .
After evacuation , the chamber is back filled with an inert gas to
a t m o s p h e r i c p r e s s u r e b e f o r e s p r a y i n g . T a b l e V shows t h a t such
p r a c t i c e s produce b e t t e r bond s t r e n g t h s t h a n s p r a y i n g in ~~a i r u n d e r
a s h r o u d of a r g o n g a s . When g a s s h r o u d i n g was e m p l o y e d , t h e average
s t r e n g t h of t h e bond b e t w e e n t h e t i t a n i u m c o a t i n g and t h e t u n g s t e n
substrate was 3940 psi. The average bond strength for specimens
s p r a y e d in a c h a m b e r f i l l e d w i t h a r g o n was a t l e a s t 6 9 0 0 p s i . Since
some bonds w e r e s t r o n g e r t h a n t h a t v a l u e , t e n s i l e f a i l u r e s sometimes
occurred in the epoxy cement used to fasten the coated specimens to
t h e tabs used f o r g r i p p i n g .

T a b l e VI shows t h a t s p r a y i n g in a c h a m b e r can even remove

most of the oxygen, nitrogen, and hydrogen originally present in
titanium powder material. It is generally believed that spray ing
a truly protective atmosphere will not only improve the apparent
density and bond strength, but also reduce the average pore size of
a coating deposited under otherwise similar conditions.

16

1~
 - - -. . _ -..- -
-- _ _ _ - -

TABLE V. BOND STRENGTHS OF TITANIUM-COATED TUNGSTEN SUBSTRATES

PRODUCED BY PLASMA SPRAYING WITH TWO TYPES OF PROTECTIVE
ATMOSPHERE S

Gas-Shroud Protection Argon Chamber Protection

Bond Strength , Type of Bond Strength , Type of
psi Fa i l ure (a) psi Failure (a)
4170 I 6750 I
4180 I 6500 I
3160 RI 7280 E
4170 RI 6670 E
3740 RI 6800 E
4200 RI 7400 E
Average 3940 ±420 6900 ±360

(a) Type of Failure : I , at substrate interface

RI , random to substrate interface
E , failure in the epoxy adhesive

TABLE VI . EFFECT OF SPRAYING IN ARGON-FILLED CHAM BER

ON CONTAMINANTS IN TITANIUM POWDER

Material Oxygen , Hydrogen , Nitrogen ,

Condition ppm ppm ppm
As received 2872 630 1485
As sprayed in
inert atmosphere 892 357 57
chamber

17

_ _ _ _ _ _ _
- . .
~~~~~~~~
1.1.2.2 Electric—Arc Spray

A common technique for electric-arc spraying of metals or

other conductive materials is illustrated by Figure 7. Two wires
or rods of the material to be deposited are fed through electrical
contacts to form the positive and negative electrodes connected to
a source of direct-current power. When the wires form a sufficiently
narrow gap, an arc forms and temperatures in excess of 10 ,000 F are
attained at the tips of the electrodes. A s the consumable electrodes
melt , the li quid drops are atomized and carried to the substrate by
a blast of compressed air or inert gas. By using electrode wires
of different compositions , this type of electric-arc spray in
~ is
capable of deposit iii~ alloy coatings.

The electric—arc spraying method is less versatile than

the plasma—arc process because it is applicable only for materials
with adequately high electrical conductivity.The lower working tem-
perature and lower particle velocities result in coatings with
poorer characteristics than those appli ed by p lasma sprayinu . Since
oxidation is less of a problem and working temperatures are higher ,
electric—arc spraying offers a sliuht advantaqe over flame spraying
by the powder , rod , or wire gas combustion methods.

INSULATED R E F L E CTOR S U BS T R A T E
HOU S ING PLATE /
SPRAYED J
_ _ _ _ _
MATERIAL ~f )
WIR E WIRE GUIDE

________
- ARC
L -
POINT
~~~~~~~~~

AI R - _ _ _

~~~~~~ _ _ _

•
ii NO Z ZLE
,,
WIR E

FIGURE 7. SCHEMATIC OF TYPICAL ELECTRIC ARC SPRAY DEVICE

18
 -

1.1.2.3 T r a n s f e r r e d - A r c Deoosition

The transferred arc deposition process , used for depositing

welded overl ays , is mentioned here because it bears some similarities
to plasma-arc spraying . In transferred-arc processes the discharge
of electrical current occurs between the electrode and the work-
piece. Since most of the heat is delivered by the arc , rather than
by the plasma as in the plasma-arc spraying process , the method is
called the transferred-arc deposition process.

As indicated in Figure 8 , the sub~ trate is connected to the

positive side of the electrical circuit. In that respect , it differs
from the plasma-arc spraying method which requires no electrical lead
to the substrate or workpiece. In both cases , the tungsten—alloy
nonconsumable electrode forms the negative (cathode) electrode. In
the transferred-arc process , the arc to the workpiece heats and
melts material near the surface of the substrate . The material
needed to form the overlay is added to the molten poo l of substrate
material by a filler wire, or as shown in Figure 8 , by sprayed powder.

A p p l i c a t i o n s of t h e t r a n s f e r r e d- a r c d e p o s i t i o n p r o c e s s a r e
limited to electrically conductive workoieces. There are other
serious limitations. Since the arc extends to the work~~iece to
form a molten pool , great care must be taken to avoid undesirably
high substrate temperatures and excessive dilution of the coating.
By precise contro l of the arc current , the transferred-arc deposi-
tion process can deposit 0.015—in. -thick o. thicker coatings while
holding the depth of substrate melting and ~ oatinu dilution to ,
respectively, 0.007 in. and 6 percent.
F u l l y a u t o m a t e d v e r s i o n s of t h e t r a n s f e r r e d — a r c d e p o s i t i o n
system have the following capabilities:

W i d t h of a o n e - p a s s d e p o s i t - 0.05 to 1-1/4 inch

Thickness of a one-pass deposit - 0 . 0 1 0 to 0 . 2 5 inch
Deposition rates - up to 15 l b/ h r

The transferred-arc process is suitable for depositing relatively

heavy coatings on substrates which can tolerate some metallurgical
damage and distortion. The characteristic melting of the surface
material results in a smooth coating and an unusually strong bond
between the deposit and the substrate.

1.1 .3 Process and Equ ipment Comparisons

All therma l spray processes can deposit coatings with a

wide range of characteristics , depending on the operating conditions
employed . Therefore , the in f o rma ti on l i s ted in Ta b les V I I and V I I I
are only rough generalizations. For instance , the rise in tempera-
ture during processing varies considerably with the mass of the sub-
strate , c o a t i n g th ickn ess , de posi ti on r a t e , ma ter i als in v o l v e d , and ,
especially, the precautions taken to control temperatures.

19

-. --~~ .- - - — - - - — -~~~~~~~ - - - - - - - ----

 _ -- -—. --_=--— .- .-- -----.---- -- ----—- -.—- _ — ________________________________
!P.. . _ ;.
. _
~~~~~~~ ~~~~

Water cooled co er velocity

~~ High
molten particles
~~~~

-
~~~~~~~~~~
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~
,

-
_
_ _
_
_ Substrate
Ar
~ ~~~~~

Pbsmo
~~~~~~ ~~~~~~~~~
J

f
Arc p~~,er Fusion power
supply supply

FIGURE 8. SCHE MATIC OF TRANSFERRED ARC DEPOSITION PROCESS

20
— _ .— ..
.. . . ...~~~~~~
~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~ - —

-
T a b l e V II indicates that flame spraying equipment fueled
w it h oxy gen an d ace ty l e n e is co n sid era b l y l ess ex p e n s i v e than equ ip-
ment based on arc or plasma heating. It also shows that the two-wire
electric-arc and wir e flame-spray processes are used to deposit
coatings atmuch faster rates than the other methods.

Table VII I give s some estimates of the relative costs of

depositing coatings by six thermal spray methods. The data avail-
able on the detonation-gun spray method were insufficient to include
that process in the comparison. The estimates in Table V III indi-
cate that , for equal operating periods , the plasma-arc and trans-
ferred-arc methods are the most expensive of the processes considered .

Other factors influencing the selection of the thermal—spray

process are sometimes more important than those listed in the table.
Mani’ desirable coatings have to be sprayed under conditions which
will not cause contamination. The ease of doing so is a big advan-
tage for the plasma-arc and detonation processes. The same processes
are capable of hi qher spray temperatures and spray-particle velo-
cities. Proper control of those features results in stronger bonds
and more appropri ate densities. For all of those reasons , and some
mentioned earlier , Plasma Spraying and Gun Detonation methods are
the only processes considered suitable for most severe service
applications of interest to the U.S. Navy .

21

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L i 0~ e-4 0~ ~~
>~ r i T i — c --i - o --i
~~~Li ’O ‘- 4 0 - - i 0 —~~ O - ~~ c~ c~~~~c 0
< 0 ’4-4 Li .O Li ’O .O .0Li ’C - -4 . 0 L i’ O -‘- 4 0 - - ’ ‘-4
(Ti (Ti 4~) (TI J -4 0
~~
4~)
O~ > 00 . 4-I C ) 4j . _Q )
~4~
) CJ 4-J O) 4-~ - C .) .C U ) B (Ti 4-JO)
E~~~U ) W ~ t~~Li •HmLi --4 (TI ~‘ (---4T I.0
WW
.4 - -4C --I TI
~~ Li
U)
~~
(-4 c.c c.c -
~~~~~~
c .ri -
~
c.c --4 ’- l Li -4
-i . c o o e~~.o
~~ ~ ~~~~~ ~~
~. u -.-44- J 0- 4 -i-I ~2 - - ~~~
J 0 . 0 ~~~~~
-- i -i-
~
‘—4
A

Li ‘4-~~L i Q J i-
O C.) N 0)~ 0) 0)
4 J - ,-4 ‘0 ‘0 Li I
‘0
0 ( 0 ,-I - ‘-4 0 -o

.
~
c~ c- .z--- ~ a a ---
o >~ -i-i ~
~
C o
0.)
0 0.)
U)
U) 0
0 ‘
0
4-0 (0
‘0 ‘0
0
U) . .( 0 (0
0 ) 4~) O - U ) ’ C T 0 0) 00) U) 0 u 0 0) u w
o BQ --4 0 0 0 -- ~~ o e c~ ~~~0’ 0 m --i cr --i a) r- .- o-
0 ~0 —4 -~ -4 -’.l 0 -4 -‘- 0 - 0 - --4 .4~ ) o c —i c —~~ ~ c
-i
Q
~ ~~~
~
‘-4 -~-l —4 E 4) ~ B .0- ‘.4)
-4 ‘.-4 ‘.4 B C.) - — —9 - -
~~~
‘- LI - ‘-4 —~ E - —4
1 ,-4 (0(Ti U ) Q ( 0 ( 0 - , - 4 4~
(0 4~) (0~~~~~ J 0 4) (0-’ J
O’ O., L i ( 0
~ 4) L i U ) ( 0 4 J (0
~4 - o 4~) (0 .iJ u) (0
0)~~0)~~0
4J
~~~~
Li CJ C J ’- - 4 0 0 0) 0 0 (DO 00 0)0 0 (DCi 0
4-4
~~ ~~~ O Q . ~ O Z O ~~4-4 O Z O 0 0 0 ~~~ 0 Z 4-4 0 ~~~ 0 0
0)
LI 4 ) 4~) 0
-~ (0 0 4~) 0
B C.) C 0 0 0
< -‘-~~B 4 ) C C 0 4.) 4.) .4~) C Li
X Q . U) CC 4iC C C C C C 0
O --4 0 C - C C C C C C C C .
~~~
0)
Li 0 0 - in C CO C (N C (N C ~~ C IC,
C (N C (N r’ r’l (N
0’
(r ~ ~~ r’
(N ~ CO - C--I 4)
Q
LI (N V
~
0. 4J
~~ — (r> ~~ U~ C U- U)
(1> (N Z
4-) (TI
o ~~ >1

0) 0) C OLi Li --I
BC. ) (TI ,,,3. I-i -‘.4 C1~ - .-4 Li l’O (0
c~ c~ — W C ) >i 0 > i BU ) ~~~
4) 0) 0.) 0
~~ - 4) V B r T i 0 oc
0--I ~~~( 0 L i L i ( 0 L i L i ’0 0 0) 0 ( TiLi0 4J 0Li
0’ 0 L i 0 0— I c-, ~~4 Q
~
(DO ~~ ~~ Li
— L i Ü ) Li
U) 0 < ~~~ O~~L~~U) ~~~L . U ) 0~~~ E-~~L I < E- ’4) ”~ 0 4.- U)

22

L - ~~~~~~~~~~~~~
..
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
.
- ~~~~~~~~~.
~
_____ - -- —
=- - -~ - --- --- -~~~~~~~~- -=-- --- -----= - - —-— ---—--

0 CO C CO C in C-) — C
‘.4 ‘.0 C C (N N C N in
. 1 1 1 • I I . . C
(0 0 Li C C in in C (N — C- C N N . -
Li Q~ N N
IC- in ( ,-4 — — —4 4_) .2
0.) U) Cs) r ( N ’ . 0
~~ 0 C)
0 (N 0 C

‘Ci 0)
(1) N (N Li
. .
in C C ‘.0 — >4
Li N C in If ) —4 — C’ (T) Ti
Li • • I I •I I I • ~~~ ‘0
0) 0 C C C C ‘.0 (N in C C CO ~~ • U) I

— —
tl.4 Li C C in in , — (N ~—4 4-) if)
W~~~~
o
(0
Li
----
i n i n ( NN

(N~~~~ (
(N
N ¼0
0
(I)
B
4)
>4
(0
-

El (0 0
(TI C) ‘
00 0) C C i n in Li Li
(I) Li - .-4 CO C ‘.0 N r~) (N -4.) C .)
O - .-4 Li • - 1 1 1 1 1 • - I • . C.
0 5 ~~ 0 C C C C — (N — C • .4-)
0 Li C ‘-0 C-) 0) -~~ C (1) .4~)
E 0 Q ~~~ m ( N ’.o CO C
LI~ 3. 0 ’.-I
‘. .—I C. ~~
-
Z E4~~~
LI
(1)
‘0
. -
>1 C C CO C in C-)
(0 a.) aj CO C C (N N C CO (0 Li
Li~~~~~TI . . . •~~~ I I • I I C C
c..
~~
-‘.4 Ti Li C C IC- in C (N .—I C-) C N N . - C
U) ~~ — in C-) ‘.0 C
~ — —I ‘—4 ‘-4 0
~L4 (J~J ‘.. O i n( N N a
i-i (N -— CO
)
~4~
Z Li 0) 0
.‘ C C) if) C ~~ ‘ C U C
C.) 5 (0
~
LI ‘ 3.0 .—4( 0 L i C C If) IC- .
in
. .
C 0) —4

(N C (N
• I
~~
I - I l l
-
~~
.
C
C)
0.)
C.
0
C
X C C In ‘.~ • U)
El 0 L~ U) in N CO in .-4 —‘ 0 0 Li
C O C - ) ,-4 in -— C
— 14-a
0 0 4-) -
Li - — in C in C-) — C-) 0) (j) 4~)
0 N C (N —i
~~ —4 C) ‘.0 C) 0
U) • • I I • I
• I • C.)
(0 ~~~~~~~
El C C C C ‘.0 (N CO C ~ -4 C —.4 0) 0 E
U) 5 5 0 0 in in —4 (N (N • 4.) C.
o ~~ in In (
N N —4 U~ -—
0 (0 - - - - -- C
—4 C (N ~~ (N ‘.0 0’
C.)
LI l~~~~~~~~~ (N
>
4-4 U) ‘-4-4
El 0’ 0
L i L i -—
(0(0 -r-
’ O L i
Li 0.1 0.) U> 0(0
>-~~>4 -
- 0
Li a

-- .0 - -4 N O)
— — .
~ .
4) -- 4 Li
I—I (4) 4-) (N - (0 ‘—4 0
4-4 L i0 —4 (1)- .0
~~~
Li -~- 4 Q
( 00 ) (1)- (1> (TI 4). 0
00 — Li - U> .2 Li C. C
LI > ,L i .0 - LI Li (1) C
--
0 4J U> —. .
0 </> —~ 0(0 .‘4-4 0)- - - -
~~~
~~ LI Li 4) 0
.0 - 0-
~~~
U> in C1~ Li ‘4— --- in 0)- ~~—
- .0
~~~
. ~~~0 ’1-4
‘0 — . -. N U)-
El - L i C L i - ..- - .) - - -~~~~~ 0U ) C-)
L i ( 0 t i ~~ - 0.) 0
.)- —. 0
4J 0 ,-4 (0 0)-
~ .
0 0 0 0 4) - L i L i
(0 Q) Q
0> 0 ~~ i n 0 C O <~ - . (4) .4.)
- Li~~~~~ C — . ( N ( N L Ci 0 0) 4-4
B (TI C) - W i n .~~~~~C C ’ . 4 ~~~ 0 Li 0 Li
Q 0 Li4- .4J > , — I C i n • -(TI .0 0 0 LO
Li
- - 4 0 0 0 ( 0~ 0 ) O C — i nC C >4 ( 4 ) . (0
0 r-4 0 0. Li 0 • C - ”-- 0 ’ 4J 0 U) - 0.) .‘~~~0
‘ 0 0
O ’O C C.) • 0 - _ -I ---I > 0.) 0 >-s4
L i ( 0 ( T I 0 C . ) 0 - O C O O U ) 0 U > 4.) -~~4 ‘ ‘Ci -.
N 0 0 ’ 0 ’ 0’ (T I 0 — ( D C ) U. ) - ’ - 4 4.) 0) ~~~~ ‘ 00 )
4 -’-I Q J L i L i 0 ( O~~0 ’ 0 L i - Li (TI (TI 4) 0.2
0 4 ) 4 ) ( 0 ( 0 - - - I L ~~~~
( i ( D > , 0 0 0 L i 4 JLi 0 ) 4 ) — 0)0 0)0
0 L i C . 0.0 4J O 0) 4 J O L i L i ~~ Q0 0 0 0 0) 00 (0 0
--4 0 - 4 0 0 ( 0 L I > 4 W 0 ” 0 4 ) E 0 4 )0 El ~~ 0 --~ ~~~~
0) 5 ( 0 (0
L i ( 0 X 0 L i > -’.4
i 0 ’-.4
(D~ - I 0 < ~~~ Z Z 0 L i~~
Li (TI .0
0 0 — —

23

“
-- - -
~ _ _ _ _ _ _ _ _ _ _ _ _ _ _
-
---
--
_
- --- =__ - - - - - - - ---
~~—

24

--,-
. - .‘- - -
—--—— - - — - — ~~~~~~~~~~~~~~~~~ --- -
 -- --
- -
- --- -
- - - - - - -- -- -
- - - -
rp
~~ ~~~ ~~~~~~ ~~~~~ ~~ ~~~~~~~~ ~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~ ~~~~~

SECTION II

2. COATING DESIGN CRITERIA FOR E N G I N E E R I N G APPLI CATIONS

2.1 COATING SELECTION

The s e l e c t i o n of a c o a t i n g f o r a s p e c i f i c end use i s n o t ,

as it may seem , a m a t t e r of s i m p l y c h o o s i n g a coating material
with certain desired properties , for application to base material.
Rather , the selection of the coating material should be approached
as a design problem , taking into account such factors as the func-
tion the coating is to perform , the conditions under which it will
be operating, and the physical and chemical properties of both the
coating material and the base material. Careful evaluation of
these factors may indicate the need ~for a graded or composite coat-
ing and will have a bearing on the coating application technique
to be used. Final selection of the coating must be based on care-
ful testinq and evaluation of a suitable number of test specimens.

The selection of a coatinq for a new application is far

more complex than selecting struc~ ural materials produced and fab-
ricated by more conventional processes. In those cases , the
p hy s i c a l and m e c h a n i c a l p r o p e r t i e s of t h e work p i e c e m a t e r i a l a r e
w e l l e n o u g h e s t a b l i s h e d that service performance is reasonably
predictable. This is far less true of thermally sprayed coatings
because the process affects the characteristics of the material
deposited . Probably because of the difficulty of testing , rela-
tively little information on prooerties of sprayed coatings is
available. It is universally accepted , however , that the proper-
ties of sprayed coatings may be appreciably different from those
expected of the powder-feed material in the virc lin condition and
tested in larger sections.

The properties of the deposit can be aff ~’cted by various

parameters of the spray ing process. Kuijpers and Zaat , for example,
showed that molybdenum will absorb some oxycien a n d ~ i t ro a en d u r i n o
plasma spraying, with argon arc gas , in an air atm os~ -her ~~. (7) In
their experiments , the oxygen content of the deposit i icreased
from 0.5 percent to 2.5 percent as the noz z1e—t o-substrat~ ’ distance
increased from 2 to 8 in. Because the spray particles are quenched
so quickly by contact with the cold substrate , the microstructural
characteristics are quite different from bulky specimens of molyb-
denum . The compositional ranges for homoc eneous solid solutions
are much wider and the grain sizes are smaller. Those effects in-
fluence rnicrohardness and can be appreciable. Microhardness
m e a s u r e m e n t s showed t h a t t h e h a r d n e s s of t h e m o l y b d e n u m coating
varied from approximately 660 Vickers at the bond interface to
360 Vickers at a distance of 0.007 in. from the substrate. Similar
v a r i a t i o n s i n m i c r o h a r d n e s s of t h e p l a s m a - s p r a y e d m o l y b d e n u m coat-
i n g s w e r e f o u n d to be associated with differences in the thermo-
physical properties of the substrate. For example , faster quenching

25

- -
~~~~~~~~~~~~~~~~~ - - -~~~~ - - - - -
 - —-—- - — —-- — -- — ~~~~ — , - —— —------- - -- — --

of molybdenum droplets associated with thinner deposits on a silver

substrate resulted in twice the hardness of coatings on alunhina
substrates.

For such reasons and because of the critical nature of

Naval Ordnance Equi pment , it is recommended that performance in
full scale or simulative tests be used as the primary criterion
for validating the selection of a the rmally sprayed coating for a
specific application. That recommendation is not unusual; it
re sembles th e p racti ce comm on ly followed fo r novel p roce sses , com-
ponen t s , or equipment before using them in critica l applications.
That practice , of full-scale coating evaluation , is followed by
aircraft eng ine manufacturers, the main users of plasma-sprayed
coatings.

Regardless of the specific function a coating is intended

to perform , the total operating environment should be considered
when choosing a candidate material. For instance , though the pri-
mary function of a particular coating may be wear protection , it
must be considered whether that coatinu will be subjected to ex-~
cessively high (or low ) temperatures or whether it will be exposed
to any corrosive media. In selecting materials for thermal protec-
tion , questions of corrosive environments and exposure to abrasion
or impact must be addressed . Definition of the total operatinq
environment is essential for successful coating performance .

S e l e c t i o n of a c o a t i n g m a t e r i a l m u s t be b a s e d n o t onl y on
its properties as related to its end use and service environment ,
but on factors related to its compatibility with the substrate as
well. P r o b a b l y the most i m p o r t a n t such f a c t o r is t h e r e l a t i o n s h i p
between the respective coefficients of thermal expansion (CTE) of
the coating material and the substrate . Larger differe ces in
t h e r m a l c o e f f i c i e n t s of e xp a n s i o n c a u s e h i g h e r s t r e s s e s between
the substrate and coating . Although they can be minimized by
proper preheating or temperature control , and by using bonding
coats with intermediate properties , it is good practice to employ
coatings with thermal—expansion coefficients close to that of the
substrate if other characteristics are approximatel y equal.

-
2 .1.1 Coating Functions

The versatility of the plasma-arc spraying process -permits

it to be used for depositing over 200 different materials. Coat-
ings of metals , alloys , oxides , a nd o th e r comp oun d s , either singly
or in combination, have been used to solve many material problems.
Some of the applications are suggested in Table IX and types of
coatings used for specific purposes are identified in Table X .

26
 —- -- -~~ —-- — ---
~~~~~~~~~~ -~~~~
:-— -
~~~ =— - -— --- -—

TABLE IX. SOME A P P L I C A T I O N S OF PLASMA -ARC D E P O S I T S

A n t i - W e t t i n g (stop o f f s ) N u c l e a r Moderator
Catalyst Nuclear Shielding
Corrosion Resistance Oxidation Protection
Electrical Conductivity Parting Agents
Electrical Resistance Salvage
Electromagnetic Shielding Thermal Barrier
Em issivity Wear Erosion
Fabrication of Freestanding Shapes Wear Fretting
Wear Friction

For N a v a l O r d n a n c e a p p l i c a t i o n, p l a s m a - s p r a y e d c o a t i n g s
a r e of i n t e r e s t m a i n l y f o r t h e f o l l o w i n g p u r p o s e s : (1) t h e r m a l
p r o t e c t ion , (2) wear resistance , ( 3 ) c o r r o s i o n p r o t e c t i o n ,
( 4 ) e l e c t r i c a l i n s u l a t i o n or c o n d u c t i o n , or (5) salvage. Some
m a t e r i a l s h a v e s u i t a b l e p r o p e r t i e s t o pe r m i t u s e in several of
these classifications. However , there are instances where a corn—
b i n a t i o n of m a t e r i a l s must be used to achieve a particular property.
The design of a coating for a g iven application should begin with
the consideration of those materials whose properties are known to
be useful within the desired range of temperature, hardness , elec-
trical resistivity, etc. It is then necessary to take into account
t h o s e f a c t o r s , s u c h as thermal expansion or conductivity, suscep-
tibility to oxidation or reduction , electrical properties , etc.,
which would make them unsuitable for the application at hand.

2.1 .1.1 Thermal Barrier

The prime requisite for a thermal barrier coating is a

high melting point. T h i s i s not , however , the onl y r e q u i r e m e n t .
Low thermal conductivity and high r e s i s t a n c e to t h e r m a l s h o c k ar e
needed as w e l l . Z i r c o n i u m o x i d e and a l u m i n a a r e p r o b a b l y the most
commonly used thermal barrier materials , though this class of mate-
rials could include most of the refractory metal oxides.

The approximate melting points of some thermal insulators

and metal oxides are listed in Table XI . Table X II lists the
coefficients of thermal expansion of some materials that may be of
interest as substrates or bond coats. The table also lists thermal-
conductivity coefficients for bulk (solid) samples of metals , but
none were found for thermal barriers except the one shown for
magnesia. There is little doubt , however , that the oxides have
thermal conductivity values much lower than any of the metals.

27
 in
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ a~~~~~~_ . z - --
~~~~~~~~~~ ~~~

TABLE X . THERMA L SPRA Y COATINGS A P P L I C A T I O N AND USE

Service Deposition
Requirement Coating Material Method*
Bond C o a t i ng ~s Nickel Aluminum (95:5) P/A ; P-F/ S
Nickel Aluminum (80:20) P/A ; P -F/ S
Nickel Aluminum (83:17) W-F/S
Molybdenum P/A ; W-F/ S

Clearance Control
Abradable Nickel Graphite (85:15) P—F/ S
Nickel Graphite (75:25) P - F/ S
Aluminum ( 99 .0 ’+ ) P/A
Silicon Aluminum (l2Si) P/A
Silver Copper Zinc Alloy W/F/S
Abrasive Aluminum T i t a n i a P/A
Cermet (A l ~~O 3 + NiAl)
P/A

S a l v a g e and Nickel Chromium P/A ; W - F/ S

Repair Nickel Chromium Aluminum P/A; P-F/S

-
Nickel Aluminum P/A; P - F/ S

Environmental FeCr Alloy P/A

Zirconia P/A
Aluminum E/A

Instrumen- Nickel Chromium Alloy W-F/S

tation Nickel Aluminum (83:17) W-F/S
Nickel Aluminum (95:5) P/A
Nickel Chromium Silicon Boron Alloy P/A
Alumina B-F/S

Fretting Tungsten Carbide + C o b a l t ( 9 8 : 1 2 ) P/A

and Wear Tungsten Carbide + Cobalt (35:15 ) D—Gun
Protection Titanium Carbide P/A —
Chromium Carbide + Nichrome P/A
Molybdenum W-F/S; P/A
Copper Nickel Alloy P/A
Copper Nickel Indium Alloy P/A
Nickel Silicon Boron Alloy P/A
Chromium Silicon Molybdenum Cobalt All oy P/A
Cobalt Chromium Nickel Tungsten Alloy P/A

Special Purpose
Sacrificial Molybdenum W-F/S ; P/A
Component P/A
Nickel Aluminum (95:5)
Bal ance
Speed Nickel Iron Alloy (Mu Metal) P/A
Sens ors
* P/A - Plasma Arc ; W-F/S - Wire-Flame Spray; P—F/S — Powder-Flame
Spray ; R-F/S - Rod-Flame Spray; E/A - Electric Arc;
D-Gun Detonation Flame Spray .
-

28

- - - ~~~~~~
. - -- - - - - - - — - - -.
~~~~~~~~ -- - .—
-
_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _- _
- _ _ _

‘0 ‘0

— —
C C 0 in C C C C 0 in 0 0 in C C C If) in Li) IC-’ if) 0 0 0
in in ( ) (N 0 in CO 0 — C) (N 0) ‘.0 N (N ~~ C-) c’ N N — C C) C
in in C-) C) - 0) ‘.0 C (N 0
‘. N CO (N CO N
~~ — CO ~~ C
CO (N ~~ (N C-) (N (N in ‘.0 C-) in in C-) C-) ~~ C-) N N Li) in ‘.f -
~~ ~
CC -~
L)Z i ni n —0
Win - - 0
0>4 ( N( N — -~ 0 O C — -- C~ H
.-
-
o — 0 L i U -~~~~(~~ 0 0
C- C c’ — C _) ’.4--
0 (1) (0 --4 -4
El E-. E-’ - - — ‘ 0 ’ 0 C.)
-< U) -
~~
- —-
~~~ COO ) - --4 ---’ C ) C ) C ’ 0

-
(4) -~
(1) 0 0) 0)0 ~~ - --I 0’
L i L i - - - ---- --- L I H
— — ‘ 0 ---0’’0 - -
-C
LI -) >4 0 N- ’.4 Li
~~ -‘.4 - ‘-I “ ‘0 Li LI 0 0 4.- Li Li (0
LIC. o- O~~~ O X ~~~~O~~1 ( 0 ( 0 ( 0 0
-, - 4 ( 0 L i
5 ‘—4 (0 - -4 0 L I0 0c i) - - (4) . 0 0 ( 0 5 50 0 0
U> ’ 05 —4 4.) U) El >4 C.) Li 0 0 0 5
LICO 0 0 5( 0 0 ) 5 0 — 5 - -- 5 5 - --- T I ‘0 (
0 5 0 05 5 5 0
- -
O C) --’ O 00) 0 0 0 -— --4 0 0 5 0 0 0 C 0 - - 4
O ‘-4 0 0 0 ~~~4 4 ~
) (0 , - 4 ( 0 - - 4 --4 (TI 0 LI
0 ( 0 - -- 4 0 0 - - 0 Li 0 E - . H L I L I ( 0 W 0 0
‘— E
l . 2 > —~~4 ) C C 4 J ~~~ - - - 4 4 ) L 0i (( 0 L i 0 (0 0 0 0 > 4 > 44 ) 0 ( 0 0
‘ — 4 0 0 4 ) 4 ) 4 - Li
-

~~
-U) --4 0 ( 0 — . 4 4 - J 4 ) c i C -H r )L -
I. -.-) 4J - ,
~~ 0 . 0 ( 0 0 0 ( 0 0 ( 0 - —
- a 0~~~~~~~~~E l E l > c -
U)
1)) fl C)
‘—‘ C C) ‘0
‘0
4-) -
CO C~ 4.)
U c -—
zz z
-4 <
E l0 -
If )
- - -(‘ . ( ‘ . C - .
*
C.) — -- - -- - — - - (4)
‘0 (4 ) 0 ) C)
0’ --4 5
Li --4
F- ~~~~ X~~~~~~
I 0 ~~~~
< U) CO LI
0 0 0 0 i C n L C - 0 D C i n CL C - C C i n CO 0 0C C 0
—‘ (N
~~~
- ~~~ C-) C-) N 0) ‘.0 CC — — C) N C) C-) if) 0 C-) ‘—4 0 (1)
>0 . 4 - ’ (N C) — -~ in N C’ CO ‘.0 in N ‘.0 C C N ~~ 0 ~~ N ~~
o 00. — —~ 1 C-) (N — (N C-) ~~~
~~ C-) If) ii) C-) in C-) if) If) ~~ In I

C E-’
- .
-
~~~~~~
- (4)
-
Z — - -- --CO
0— COCOCO Li
- - - -‘ Li (0 --— ’ Nz
• ‘.— :‘
~~~- — C/) O E-’ E-’ -- C!)
-- 0~~-
_
0 Z— ~~~~~
— - C.)
>0. -~ CO 0) (1)
~~~~~~~
I
— 0 0C) C.) ’0 0
N ‘ — 0 — -— ‘0 ‘0 ’ 0’0 - - 4 C.
0 00 0 0 C) - -‘ Li
-‘.l -’-i --i B
CO 0 - C.) --- --4 ’0 -) ‘ 0 ’J . L i L i L i 0 0
Li ~~CO - X —~~~~ 0 ’ 0 -~~- 4 . 4~~ 0 0 0. 0 0
H LI < —0 0 X--— Li --4 .0 .0 .0 0)
B 0 C X 4) 0 5 ‘0
55 50 O U S 0 -- 5 5 5 0
0 0 5 0- - I ( 0 - ’~~~~~~ 0 E - - 4 C C
~
000.-I I
0 0 0 — I Q .4-) Li 0 .—I 0 U) - 0 -— — -— C
--4 - - - ’ 0 - - 4 E ~
--4
E.-4 C) -. --4 (0 E - - - 4 C ) C - 0-0 5 ( 0 0 0 —
5 E 0 5 0 0 0 C . C E > . --- ~~0 C C ~~ 0. C- -—’ 0 4 ) 0 0 ‘0
0 0 L i’ 0 L i’ — 4 L I C . 0 0) LiLi ’4- 0 L L i . -4
- L i C - 4 J Li
—~ -- O r T I L I 0 0 0 L i — 4 ~~
0 0 . 0 ( ~~
00.- - ’ 0 --- ~ .0 ( 0 - 4 -4
<<CO 0 0 0 0 0 4 - l < C O U 0~~~~~~ 7) COW ’ -~
U E l E -~~

29

-- .
_ _ _ --

TABLE X I I . THERMA L AND ELECTRICAL CHARACTERISTICS OF SOME

METALS MEASURED ON SOLID SPE CIMENS AT
TEMPERATURES BETWEEN 65 AND 210 F (8)

Coefficient
Electrical Thermal of Thermal
Material R e s i s t a n c e( a ) C o n d u c t i v i t y (b ) E x p a n s i o n( c )

Aluminum 2.8 0.57 23.8

Aluminum bronze 12.0 0.18 17.0
Brass , yellow 6.4 0.28 19.0
Copp er ( 99.5% ) 1.7 0.93 16.8
Iron 9.7 0.20 12.3
M a g n e s i a( d ) - 0.05 -
Manganese bronze 7.2 - 22.0
Molybdenum 5.2 0.34 4.9
Nickel 9.5 0.14 14.0
Steel , carbon 14.0 0.11 13.0
Steel , stainless 74.0 0.35 6.~ )
Tantalum 12 . 5 0 .13 6.7
Titanium ( 9 9 ~~) 58.0 0.45 9.0
Tungsten 8.0 0.38 4.6

(a) E l e c t r i c a l r e s i s t a n c e in u n i t s of m i c r o h m s— c m .
(b ) T h e r m a l c o n d u c t i v i ty i— u n i t s of c a l/ s e c .c m . ° C.
(c) The unit for coefficient of thermal expansion is the ratio
of the change in lenoth per °C (1.8°F) to the length at 0 C
(32 F) multi plied by one million.
(d) The t h e r m a l c o n d u c t i v i t i e s of m aqn e s ia and a l u m i n a a r e simi-
lar and about twice the values for CeO ~ nd Th ~

2 .1.1 .2 Wear Resistance

W e a r — r e s i s t a n t c o a t in g s a r e m o s t o f t e n ~ c c ) ) 1 ir e d t o w i t h -
s t a n d t h e e f f e c t s of a b r a s i o n . T h i s a b r a s i v e wear is usuall y ac-
companied by elevated temperatures , either resulting f rom friction
or associated with the operating environment. Often , wear-resis-
tant coatings are required for a p p l i c a t i o n s w h e r e i~~:~ ict wear is
encountered or in corrosive environments. Consequently, wear-
resistant coatings , as a class , must be hard , though not brittle ,
and possess considerable thermal— and chemical-resistant qualities.
Materials with this combination of properties are generally found
among the carbides and the nickel or cobalt-base alloys. Some
such materials are listed in Table X and as cermets in Table X III.

30

-.
.- - - --- -- --- -
--
- - - -- -- - ~~~~~
- -
~~~ ~~~~
 - .-
-- - --— -- -- - - - - -
- -
--
- -

n ~~~ ~~~ ~~~~~~~ ~~~~~~~~~~~~ ~~~~~~~~ ~~~~~~~~~~~~~~ ~~

TABLE X I I I . SOME M A T E R I A L S THAT CAN BE DEPOSITED

BY THE PLASMA-SPRA Y PROCESS (10)

Cermets Plastics

Aluminum oxide - cobalt Chlorinated polyether (Penton)

Aluminum oxide - nickel Epoxies
A l u m i n u m oxide - nickel aluminide Nylon
Magnesia - nickel Polyoxymethylene (Delrin)
Titanium diboride - chromium P o l y t e t r a f l u o r o e t h yl e n e (Teflon)
Titanium diboride - n ickel
Zirconium diboride - chromium
Zirconium diboride - nickel
Zirconia - nickel
Zirconia - nic k e l a l u m i n i d e

Among o t h e r s , R o s e b e r r y , O n e s t o , a n d D u f r a n e s t u d i e d t h e
friction and wear performance of plasma-sprayed coatings and bush-
(9)
~ ng m a t e r i a l s . They f o u n d t h a t t h e p l a s m a - c o a t e d components
c o u l d be u s e d i n h y d r a u l i c c y l i n d e r s to o b t a i n p e r f o r m a n c e s expected
by using conventional materials of similar design in the same mode
of operation. Table X IV is a summary of their friction and wear
d a t a . The a u t h o r s u r g e d t h a t t h e f i n d i n g s i n d i c a t e d in t h e t a b l e
be treated wi th c a u t i o n in t r y i n g to i n t e r p r e t t h e m for other slid-
ing applications for the following reasons :

1. The results were obtained from complete hydraulic cylinders ,

which prevents a rigorous m easurement of friction and wear
b e c a u s e of the possible influences of misalignment and varia-
tions in geometry from component to component in the various
cylinders.

2. Wear performance is strongly influenced by the presc-nce of

lubricants . The tests were all conducted usinq ~ IL-F—l 7ll l
hydraulic fluid as the lubricant. The use of an alternative
lubricant may alter the performance of the various combina-
tions , while operation with no lubricant would probably in-
validate the results completely.

3. The extension of any wear data from one sliding application

to a n o t h e r i s valid o n l y i f t h e same wear mechanism is main-
tained . Dramatic performance differences are experienced
when the combination of sliding speed , contact pressure , at-
mosphere , and temperature result in operation in a different
wear reg ime .

31

_
- --V

TABLE X IV. PERFORMANCE SUMMARY OF CYLINDER ROD COATINGS AN D

BUSHING MATERIALS FOR USE IN HYDRAULIC CYLINDERS (9)

Si n t ered
Cylinder I ron St a i nless
Rod (Conven- Steel K-Mone ]. A l u m i n u m Steel Aluminum
Coating tional) (1020) (Monel 500) B r o n z e (Type 316) (6061)

A l -~O 3 -TiO2 A C C A A B2

Cr~ O 3 A A A B2 C B2

Nichrome 31 C C C C C

Molybdenum C B1 ,2 C Bl ,2 Bl ,2 C

Key : A — Recommended c o m b i n a t i o n
B - Not recommended because of (1) h i g h f r i c t i o n , and/ o r
(2) h i g h b u s h i n g wear
C - Not evaluated.

Other conclusions based on the friction and wear results

are as follows :

1. The wear of the plasma-sprayed coatings was negligible in all

cases , which is similar to the r e s u l t s o b t a i n e d w i t h t h e con-
ventional steel shafts.

2. The two ceramic plasma-sprayed coatings resulted in superior

friction and wear performance compared with the two metallic
coatings.

3. Bonding between the plasma-sprayed coatings and the various

s h a f t m a t e r i a l s w a s s a t i s f a c t o r y; no i n s t a n c e s of blistering
or peeling were observed . (Spraying parameters are described
in data sheets included in this handbook.)

4. A l u m i n u m a n d s t a i n l e s s s t e e l b u s h i n g s e x p e r i e n c e high wear
r a t e s and a p p e a r u n a c c e p t a b l e in a c y l i n d e r - b u s h i n g
appl i c a t- i o n .

5. The p l a s m a - s p r a y e d c o a t i n g s w e r e u n a f f e c t e d by t h e AS T M salt—
fog test.

The following conclusion was drawn from the results regard-

ing the p e r f o r m a n c e of organic fillers to seal the porosity in the
plasma-sprayed coatings:

Loctite 290 sealer , a low— v iscosity, single-component poly-

ester-type resin which penetrated open porosity by means of
capillary action , acts as an effective sealant in both
hydraul ic oil and air applications. Surface porosity

32
 o b s e r v e d a f t e r g r i n d i n g i s a p p a r e n t l y d u e to t h e e x p o s u r e
of totally closed pores , which no sealant will penetrate.
A post-finishing treatment with a surface sealant , su ch as
Epon 828 epoxy provides an improved surface.

Van Wyk conducted preliminary friction and wear studies

of plasma-sp rayed coatings for bearings. (11) The laboratory
screening tests were made with a silicon-nitride slider in contact
with various ceramic coatings on titanium . Those studies and
tests on plain spherical bearings showed some promise, but it was
concluded that further development is required .

Truskov concluded that properly applied coatings of

bronze, sprayed in an ar9on atmosphere , are suitable for some anti-
friction applications. (li) Nevertheless , the bond strengths he
reported , in the range of 1300 to 2000 psi , seem low .

Levy and M o r o s s i investi gated the fatigue and erosion

r e s i s t a n c e of h a r d — f a c e d t i t a n i u m a l l o y s . ( 1 3) Erosion tests with
s a n d r a n k e d t h e c o a t i n g s i n t h e f o l l o w i n g o r d e r of d e c r e a s i n g wear
resistance:
T i t a n i u m c a r b o n i t r i d e , o v er a n i c k e l b o n d i n g c oa t
Boron c a r b i d e
Chromium overlay on a diffusion—bonded nickel undercoat
P l a s m a - s p r a y e d boron

A l l of t h e s p e c i m e n s h a d f a t i g u e s t r e n g t h s 2 0 to 80 percent lower
t h a n t h e u n t r e a t e d t i t a n i u m a l l o y , b u t shot p e e n i n g was s a i d to
c o n f e r some b e n e f i t s .

I n 1975 , Preece and h i s c o w o r k e r s s t a r t e d a f u n d a m e n t a l

study on the mechanisms of the deterioration of plasma-sprayed
c o a t i n g s by e r o s i o n and c o r r o s i o n . (14) Nost of the effort since
t h e n has been c o n c e n t r a t e d on two s i mp l e c o a t i n g s , a l u m i n a amd
a l u m i n u m , s p r a y e d on s t e e l s u b s t r a t e s . A l t h o u g h some cavitation
tests were made , data are scanty because the effort was concerk-
trated on characterization of coatings.

2 . 1. 1 . 3 Corrosion Protection

Selection of materials for corrosion protective coatings

is probably the most complex coating design task . The combinations
of temperature , environment , and the various modes of corrosion
m e c h a n i s m s p o s s i b l e u n d e r a g i v e n set of o p e r a t i n g conditions
i m p o s e s t r i n g e n t r e q u i r e m e n t s on c a n d i d a t e m a t e r i a l s . Corrosive
environments may be either aqueous or gaseous and can span a wide
range of temperatures . In some cases , ga seous p ro d uc ts such as
e x h a u s t f u m e s or u n c o m b u s t e d f u e l g a s e s r e a c t w i t h w a t e r u n d e r
the proper temperature conditions (e.g., marine turbines) to pro-
vide a very complex corrosive environment. Basically, there are
three classes of corrosion protection mechan isms . These are
(a) exclusion of the corrosive environment, (b) electrolytic

33

-I

-
-
.
-~~~~~~- - ~~
-- -
—4
r~~w
_

protection , and (c) inhibition of corrosive action . The first

mechanism is dependent on producing a coating that is impermeable
to the corrosive medium and does not react with it. The second
c o r r o s i o n - p r o t e c t i n g mechanism makes use of the p r o p e r t i e s of t h e
base m a t e r i a l and c a n d i d a t e c o a t i n g m a t e r i a l and r e q u i r e s a
knowledge of t h e i r r e l a t i v e p o s i t i o n s in the e l e c t r o m o t i v e s e r i e s .
Choice of the proper coating material will determine whether the
coating is anodic or c a t h o d i c to the base m a t e r i a l and to w h a t
degree . An improper coating—subs trate combination can result in
a g a l v a n i c e f f e c t which could a g g r a v a t e the c o r r o s i o n p r o c e s s .

Table XV gives the electromotive series for some pu re

elements. It may be a rough guide even though the potentials
vary for alloys of the elemen ts. In general , any metal will
react with a salt to replace a metal below it in the series , e.g.,

Mg + FeSO~ -
~~ Mg SO~ + Fe

Metals above hydrogen in the table will react with HC1 or dilute
H 2 SOi4 to replace the hydrogen , e.g.,

Fe + II 2 SO -* FeSO14 + H2 -
~
The voltage of a galvanic couple depends on the difference between
the standard electrode potentials of the metals involved . For ex-
ample, a zinc-copper couple generates a larger electromotive force
than the iron-copper couple. In general , the electromo tive series
seems to fit the simpl e theories of rusting or oxidation of metals
in air and of reactions w ith steam to liberate hydrogen .

Some protection can also be obta ined by using a chemical

corrosion inhibitor as a sealer for a sprayed coating. For this
approach , the porous sprayed coating is impregnated with a corro-
sion-inhibiting primer or filled with an inorganic sealer. This
may permit the use of a th inner coating than would be needed to
exclude completely the corrosive environment. The choice of a
corrosion-protective coating material must be made in light of in-
formation about the cond itions the coating will have to endure .
In some instances a corros ion-resistant metal may be applied , in
others , perhaps a ceramic oxide may be required .
Cal~ brese and Coda demonstrated the importance of prevent-
ing substrate corrosion und er hard coatings used in aggressive en-
vironmen ts. (15) They found that corrosion occurred in the sub-
strate , during storage for several months , after a shaft had been
tested as a component in steam-lubricated bearings. The substrate
contained chromium and carbides . The corrosion was attributed to
coating porosity sufficient to trap some of the water condensate .
A short investigation on twelve types of coated specimens supported
that explanation . The study also showed that corrosion could be
minimized by using a corrosion-resistant , dense bond coating adher-
ent to both the substrate and the hard coating.

34
___________________________________

TABLE XV . P A R T I A L S E R I E S OF THE ELEMENTS ARRANGED

IN ORDER OF THEIR ELECTROMOTIVE FORCES (a) (16)

Electrode
Element Ion Potential
Magnesium ++ +2.40
Aluminum +++ +1.70
Manganese ++ +1.10
Zinc ++ + 0 . 76
Chromium ++ +0.56
I ron ++ +0.44
Cobalt ++

N ickel ++ +0.23
I ron +++ +0.05
Hy d rogen + 0.00
Coppe r ++ —0.34
Copper + —0.47
Palladium ++ — 0.82
Platinum —0.86
Gold + -1.5

(a) S t a n d a r d e l e c t r o d e p o t e n t i a l s a t 77 F.

2.1.1 .4 Electrical Insulation or Conduction

Plasma-sprayed coatings are sometimes used as electrical

conductors; printed circuits and contacts for certain types of
f u r n a c e h e a t i n g e l em e n t s a r e e x a m p l e s . C o a t i n g s of o x i d es or
organic plastics are sometimes applied to provide electrical insul-
ation or as dielectrics. Although the electrical properties of
t h e m a t e r i a l s may be a f f e c t e d by p l a s m a s p r a y i n g , it is common
practice to choose the materials on the basis of their known pro-
perties and service conditions. Then the success of the plasma-
sprayed insulators or conductors is verified before the material
-
and p r o c e s s c o n d i t i o n s are a d o p t e d f o r p r o d u c t i o n .

35
___ _ - - -~~~~~~~~~~~~~

2.1 .1.5 Salvage

Plasma spray ing is often used to restore the dimensions
specified for a particular component. The salvage operation may
be desirable for parts inadvertently machined to the wrong dimen-
sions or for parts worn or corroded in service . In the first type
of application , the material to be deposited by flame spraying is
usuall y identical or similar to the base material. Corroded or
worn parts are usually machined to a suitably smooth finish , grit
blasted , and then coated . Depending on service requirements , the
coatings may be of the wear—resistant , corrosion-resistant , or
friction—reducing type s , or similar to the material in the substrate.

36

- - . S-
- --- - -~~~~ - - — - -
~

SECTION III

3. SURFACE PREPARATION

3.1 GENERA L CONSIDERATIONS

This section of the Handbook is important because over

half the tailures in thermal sprayed coatings is traceable to im-
proper surface prepara tion . Regardless of the tyne of intended
use of a p l a s m a- s n r a \ - e d d e p o s i t , a c o a t in q i s e f f e c t i v e o n l y as
long as it rvreiins firm ly attached to the base material. The
oua litv of adherence , or the bond between the coating and sub-
strate , is directl y related to the cleanliness and roughness of
the base materi a l and to its chemical affinity to the coating.
A thorough unders tanding of , and c a r e f u l a t t e n t i o n to , the details
i nvolved in nr~ - :aring a surface to accept a plasma—sprayed coat—
i re; will enhanc~ the c h a n c e s ~or successful coating . In order to
aopr eciate the n -cessitv for oroper su r f ace p r e p a r a t i o n , one
should be fam i liar with the me chan ics of coatino-to—substrate
adhesion and the factors by w h i c h it is influenced.

3 . 1. 1 B o n d i n y ~~ 1e c ha n i s m s

Ther e is no u n i v e r s a l l y acceT tab le descri p t i o n of t h e

mechanism of bend m e betw een a substrate and a thermal—spray
coating.

One school of theueht holds tha c the bond is exclusively

or m a i n l y m t - c h i n i c a l and res-jlts from sprayed particles interlock-
ing with the roughened surface of the substrate or the peaks and
valleys of p r - - v i n u s l y S rav ed coatino m a t e r i a l . The import ance
of mechan ic-U b o n d i n ; is su : norted by exp erience th at surface
rou-~ h en in q is u s u a l l y necessary for achieving useful bonds between
most p l r ~a—s ;--raved coatinq s and substrates .

The m a i n
a 1t ~~rnative exn lanation is that bonding results
:- r irna ril v from solid—state reactions. That is , a s m a l l d e g r e e of
d i f f eUon occurs between th e sprayed particles and the extremely
t h i n ocaks en t h e roughened substrat e. The existence and quality
of that type of bond depend on some mutual solubility of the
coating and substrate materials. Even for the most favorable con-
ditions , however , solidification and cooling times are too short
to allow diffusion reactions to form a measurabl y thick meta llurg—
ic a l b o n d .

V a n d e r Waa ll s f o r c e s , which cause mutual attraction and

cohesion between two clean surfaces in close contact, are a l s o
bel ieved to prov ide some bond strenqth under certain conditions.
That type of bonding accounts for the adhesion of the “ silver ’

37

--- - - - - - - --
--
~~~~~~~~~~ -- - -
 - ;;_: - — — - - —_ — -— -- —_- - — - -
~~~~~~~~~~~~~~~ —-

layer on qlass mirrors with smooth surfaces. Regardless of the

bonding mechanism, an appropriate surfac e texture should improve
b o n d s t r e n g t h , b e c a u s e t h e t r u e s u r f a c e a r ea i s a l w a y s l a r g e r t h a n
the a p p a r e n t (p r o j e c t e d ) s u r f a c e a r e a .

w i t h t h e c u r re n t s t a t e of k n o w l e d u e , i t seems s a f e s t to
a s s u m e t h a t c o a t in ~; - t o - s u b s t r a t e b o n d i n g r e s u l t s f r o m a c o m b i n a -
t i o n of ph y sical , mechanical, and chemical fac tors. Presumably
the relativ e importance of the various bonding mechanisms varies
for different combinations of coatinqs and substrates and with
processing parameters.

3 .1 . 2 Coatin q Stresses

Stresses high enough to crack the substrate can form from

rapid heating produced by the Impact of r-lasma-sprayed particles ,
or in subsequent rap id coolin g. In spray ing zirconia on tungsten
bond c o a t s , t h e cracks apparently f o r m during the instant of spray-
ing, because t h e c r a c k s a r e s o m e t i m e s g i l l e d w i t h t h e c o a t i n g
material.

However , the biggest factor working aqainst good coating

adherence is the stress produced by shrinkage of the sprayed coat-
ing as it cools. These stresses increase as the coating thickness
is increased , o u t t i n q t h e coating under increasinu tension and
ultimately resulting in the coatina crac king or breaking f r e e of
the substrate. The difference s in therma l contraction and expan-
sion that cause the stresses can be reduced to some extent by sub-
strate temperature control , but are best de 3lt with by proper
substrate preparation , which serves to localize the stresses and
limit shrinkage strains. In some cases nroper temperature control
results in stresses that can measurably improve the apparent bond
strength. This is most likel y to happen in coatings deposited on
c y l i n d r i c a l rods or s h a f t s .

.2 C I i A ~ lNG

A t t a i n in a a s u i t a b l e b o n d d e p e nd s , a m o n g o t h e r f a c t o r s ,
on an intimate contact between the sprayed p a r t i c l e s a n d a c l e a n
substrate with an adequately roughened surface. The first step
in prep ar ing a workp iece f o r t h e r m a l s p r a y in c; is to remove all
s u r f a c e c o nt a m i n a n t ~ s u c h as s c a l e , qr e a s e , and p a i n t .

V a p o r d e -d r e a s i na i s t h e m o s t e c o n o m i c a l a n d e f f i c i e n t
method of removing most surface con taminants such as greases , d u s t ,
and body oils deposited during handling. In some cases , vapor de—
greasing is precluded because the part is too larae or is attached
to another component , e.g. , armature with windin as . In such cases,
the area to be c o a t e d s h o u l d be c i c a n e d by h a n d w i t h a s o l v e n t
that leaves no residue. Although expensive , “Freon ” is recommended -
for such operations , because it leaves l i t t l e or no residue and
m i n i m i z e s h e a l t h a n d s a fe t y hazards associated with other solveats .

38

_ _ _ _ _
 O i l and o t h t - r c o n t a m i n a n t s whi ch have i n f i l t r a t e d the
surface of porou s m a t e r i a l s , such as cast iron , can bc removed by
heating. The te!uuerat- ure should be hiqh ~ noaeh to vaporize them
and above the t e m n e r a t u r & th e s u b s t r a t ~ - w i l l reach in spray ing .
Otherwise , hl e c - d i n e
er va~~o r i 7 a t 1on w i l l occur d u r i n g s rav in q.
~~
I f a w o r k p i&-ce is covered w i t h scale from heat treating ,
or rust , it should be cleaned by a b r a s i v e bl a sti n - ; with sand or
m e t a l an t. The sam - t r e a tm e n t should L- isc d for workp i e c e s
heated to remove infiltrated c o n t a n - i n a n t s b e c a u s e they ire likel y
to contain hard deposits a ft r b a k i n g . Th t- n i a s t i n ; operations
should be c o n d u c t e d in O O U i ; r n t - n t other han the un it assigned for
use in prepa rin g subs t r a t e s or - l i s n a snrav f l u . That nra cticc
should be followed to n r e v e n t c o n t - r - - i n a t i o n of b la s t i n e media used
f o r c o a t i n ~; nr eea r at io n . The -a rts shoabi t hen be reblasted to a
s u i t a b l e s u r f a c e r e u r h n v s s in t h e u n i t used f n i p repar i nci s u b s t r a t e s .

3.3 SURFACE ROUGHENING

After cleaning, one of several me t hods or com bi nations of

m e t h o d s should he used to oroduce a substrate to w h i c h a su rayed
coating w i l l adhere . The p r i n c i r a l m e th o d s are (a ) bond c o a t i n g ,
(b) qrit blast Ino , and (c) m a c r o — r c u ’h e n i n o . To a c h i e v e an op t i -
mum surface forbonding , combinations of those methods are sometimes
employed , such as bond coatin o and grit b i a s t in q , or machine rough-
e n i n g f o l l o w e d b y grit blasting. Recent investi eations indicate
that shot peening before grit blasting offers advantages in some
cases.

3.3.1 Bond Coating

Certain metals are able to adhere to a clean , s m o o t h sur-

face at moderate spray temperatures w ithout the need for prior
surface treatment. These hondi ’i-; coat materials form strong coat-
ing—to-substrate bonds and are generally adheren t over a wide ranqe
of conditions. For best results , however , it is desirable to grit
blast the substrate before a p p l y ino the bond , or intermediate coat-
ing , by plasma spray ing . Bonding coats a r e extremely useful be-
cause a thin layer of one of these materials applied to a clean,
smooth substrate can serve as a bon d—enhancinq subcoat for subse-
quently applied layers of other spray materials. Furthermore , a
bonding coating applied to a an t-blasted surface will appreciably
increase the bond strength of materials sprayed over it as com-
pared to bond strengths of those materials applied to a an t—
b l a s t e d s u r f a c e w i t h o u t a b o n d coat.
-
Molybdenum is a commonly used bonding coat material;
other materials with suitable properties, though not much used ,
are columbium and tantalum. Also very widely used i~s a commer-
cially available nickel-aluminum composite w h i c h , w h e n s p r a y e d ,
undergoes an exothermic reaction to produce a nickel aluminide.

39

I
 Certain general considerations should be observed in us-
ing a bond coat. Primarily , the decision to use a bond coat must
t a k e i n t o a c c o u n t t h e c o n d i t i o n s under which the coating will be
used , in term s of tem pera tu r es or c o r r o s ive m edi a . Molybdenum ,
f o r exa mp le , has poor oxidation resistance and would not be suit-
able for use in air at elevated temperatures. Nickel-alum inide
is susceptible to corrosion in aqueous salt solutions.

The use of a self-bonding subcoat also limits the thick-

ness of the coatings which may be applied , in that the surface it
provides is generally not rough enough to absorb the shrinkage
s t r e s s e s produced by a thick coating. The bonding coat should be
applied just thick enough to cover the substrate , usually no more
than 0.002 to 0.004 inch thick. There is no advantage to spraying
a heavy layer of bonding coat.

The selection of a bond coating is influenced by the com-

position of the substrate and the temperature the sprayed component
will reach in subsequent processing or service . lt is desirable
that the elements in the bond coating be soluble in the matrix
material of the substrate. The ap~ roximate maximum temperature
limits for several commonly used bond coatings are :

Molybdenum 600 F 3 15 C
8ONi—2 0A1 1150 F 620 C
5 .5Ni—4 .5A 1 1600 F 870 C
8ONi—2 O C r 2300 F 1260 C

The NiCr Material is superior to the other bond coatings from the
standpoint of resisting thermal shock.

3.3.2 Abrasive Blastin~

Abrasive blasting is the most common method employed for

roughening the substrate , after the wonkp iece is cleaned and/or
shot peened , p r i o r to plasma spraying. Abrasive blasting is accom-
p lished by directing a stream containing abrasive particles against
the surface of the substrate . The operation is conducted in order
to remove surface contaminants such as oxide films or scale and to
develop a surface finish suitable for bonding.

Abra ~sive particles used for blasting are classified as

grit , sand , or shot. Grit consists of angular particles of steel ,
cast iron , malleable iron , or “ sand’ , usually produced by crushing .
The term sand is applied to many nonmetallic materials in addition
to s i l i ca . A l u m i n a , si l icon carbide , pumice , and garnet are used
for grit or sand blasting. Shot is made of the same metallic mate-
rials used for grit , but usu al l y cons ists of roug h l y sphe r ical o r
rounded particles. Some shot is made by cutting steel or aluminum
w i r e and becomes more spherical during use.

40

I
 -- ~~~~~~~~~~~~~~~~~ -~~~~~~

S e v e r a l t y p e s of equ ipment are used to propel abrasive

particles in wet and dry blasting operations. Dry grit blasting
is recommended for preparing surfaces for plasma spray coating.
The operation is conducted with air blasting machines which force
the abrasive particles through a nozzle with compressed air. Air-
b l a s t devices are more economical than mechanical equipment for
pr ocess~ ng small quantities of parts and for intermittent
operations.

3.3.2 .1 Grit Blasting

M a n u a l l y c o n t r o l l e d a i r b l a s t i n g equipment is more con-

venient to use on small objects and is recommended for preparing
surfaces to be therma l sprayed . Dry grit blasting operations are
usually conducted in a cabinet that confines the abrasive dust ,
and houses the propelling mechanism and a suitable work—holding
device or platform . The equipment is available in a variety of
s i z e s . Fi g u r e 9 illustrates a common pressure type air—blasting
device schematically. The grit is fed from a pressurized hopper
to the stream of compressed , dry air and carried to the nozzle
through a flexible hose. Ficiure 10 illustrates the principle em-
ployed in suction-type blasters to introduce the grit into the
stream of pressurized air just ahead of the spray nozzle.

COMPRESSED AI R— ~~~~--’ -

~~~~“ A B RASIVE ’.~ .

II
j~ 9
BL ;O~~~

-y
~~

~~~~~
_ _

COMPR ESSED AIR

FIGURE 9. SCHEMATIC ILLUSTRATING PRINCIPLE OF A

COMMON TYPE OF A IR BLASTING DEVICE

41

I-
 COMPRESSED AI R

NOZZLE~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

FIGURE 10. SKETCH ILLUSTRATING THE PRINCIPLE USED IN

A SUCTION-TYhE AIR-BLASTING SYSTEM

Some commercially available equipment permits conducting

air—blasting operations , particularl y on larc;e components , wi thout
a cabinet—type enclosure . Durinq blasting, the device collects
and r e m o v e s t h e s p e n t g r i t a n d d u s t by suction l i k e a vacuum
sw eeper , as suggested by Figure 11. To do so , the blasting nozzle
and its hose aresurrounded by a flexible tube connected to a stror-5
exhaust system . The suction hose is partially sealed to the sur-
f a c e of t h e w o r k p iece , around the bl a sting nozzle , by a brush or
flexible plastic cup. Although the method is comparatively slow
and expensive , the approach is use ’ul for ;rit blastin u components
too large to move or to fit into the cabinet available.

FIGURE 11 . SCHEMATIC ILLUSTRATING PRINC IPLE OF AN A I R B L A S T I N G

SY~~T!
~Y THAT CAN BE PY( LOYFD WITHOUT THE CABINET
ORDINARILY USED TO CONFINE THE GRIT AND D U S T ( 1 7 )

42
 ______________ - -

Objects destined to be plasma sprayed should be grit

blas t ed in u ni t s u sed o n l y for that purpose. Blasting cabinets ,
and contaminated air lines , employed for abrasive blast cleaning
of o i l y , rusty , or m ainted parts can produce surfaces unsuitable
for plasma spraying. A blaster used for general purposes can be
co nv e r t e d b y thorough cleaning of the cabinet , replacing the abra-
sive , and putting in new air lines. The inside of the cabinet
should be abrasive blasted and wiped with a solvent.

Grit blast nozzles erode quite rapidly even though they

are made from hard cast iron , tungsten carbide , boron nitride , or
alumina. A steel nozzle lined with boron carbide is usually a
good choice , despite its higher cost , because it gives a much
longer life. Because it wears more slowly, it saves air and pro-
vides more uniform spray patterns and particle velocities for a
longer time than less-durable nozzles . A nozzle should he replaced
when the outlet area has increased about 40 percent. In general ,
a nozzie used for air blasting metal grit will last about three
times as long as one used with sand.

F o r r e a s o n s of safety , the carrier hose on blasting

equipment should be inspected frequently and replaced when neces-
sary. Hoses are most susceptible to wear at bends. The bending
r a d i i should be as generous as practical.

The e f f e c t s of g r i t b l a s t i n g d e p e n d on process parameters ,

of w h i c h size and type of abrasive , particle velocity, air pressure ,
b l a s t a n g l e , and blasting time are the mos t important.

The force of the impact of a sing le blas ting particle

depends on its change in momentum and with the mass and velocity
of the p a r t i c l e . S m a l l e r a b r a s i v e p a r t i c l e s r e s u l t in sprays giv—
ing more uniform coverace of the surface and smoother finishes.
Heavier particles and higher velocities favor more rapid removal
of material from the workniece , as do harder materials. For other-
wise similar conditions , higher air pressures produce slightly
rougher surfaces.

Figure 12 , from Golego and Panamarchuk , show s the e f f e c t

on surface roughness of variations in spraying time and air pres-
sure . (18) The data were obtained in experiments on air blasting
a titanium alloy containing 2.5 percent aluminum and 2 percent
manganese with corundum grit particles rang ing from 0.0013 to
0.0016 inch in size. Although the roughness values shown in the
sketch are not standard AA values , and are presumed to be maximum
peak to valley distances (which are ~3.5 AA values ) they i llus- ,

trate severa l points. The graphs show that varyin a the air pres-
sure for spray ing times less than 30 seconds had no effect on
roughness values. After full coverage is attained , continued
blastin i at the same pressure and grit size produces no change in
microgeometry or roughness of a workpiece . The data also show
that using higher air pressures for a particular grit size produce s

43
 -

~~~~~~~~~~~~~~~~~~~

I I I

40— - 1600
/

0
D
_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _

C
z I
0
c z
30 -
1200
~
-

j J)

-
U, ~~
U)
w C)

- 8OO

o
II ~~~
I

10— - 400

0
30
~~~~~~~~~~~~~~~~
I I
60
I
90 120

BLASTING TIME , SECONDS

FIGURE 12. RELA TIONSHIP OF SUFFACE ROUGHNESS * OF A

TITANIUN SUBSTRA-rE TO GRIT BLASTING
TIME AND PRESSURE (A 71 .1 ~asi;
B 42.7 psi; C = 28.4 psi ) (18)
* Presumabl y nonstandard method

slightly rougher surfaces. The authors also showed that the bond
strength of a nickel-base coating , containing carbon , plasma
s p r a y e d to t h e t i t a n i u m a l l o y s u b s t ra t e, varied with the roughness
values identified in Figure 12. The relationshi p was as follows :

Rou g h n e s s v a l u e , microns 400 80 1200 1600 2000

Bond strength, psi 1565 1850 2220 1960 1850

The data show that the best bond strength was associated with the
roughness dimension comparable to three-fourthn of the diameter
(1200 microinch on the system used by the Russians or probably
350 AA ) of the particles sprayed . The results seem to support the
natural expectation that there is an optimum roughness value for
good bonding and that the value should be related to the size of
t h e pa r tic les sp r a y ed .

44

I
 Grisaffe also concluded that variations in surface rough-
ness of grit blasted surfaces affected bond strengths. (19) His
wo rk , summa r i zed in Table XV I , was conducted on alumina coatings ,
plasma sprayed (0.030 inch thick) on 304 stainless steel coatings.
Although the strength values , determined with a nonstandard shear-
ing device , appear low , they illustrate a principle. Within the
ranges in roughness and powder-particle sizes investigated , the
best bond strengths were obtained on substrates with the roughest
surface tried . That surface was reported to have a roughness
value of 280 microinch on the old rms system , which is approxi-
mately 420 microinch on the standard AA system . Other studies
show somewhat similar effects , although the rate of improvement
in bond strength with roughness apparently decreases above
375 m icroinch.

Smoother finishes must be used when the plasma coating

is very thin , or for substrates that would de form if subjected to
severe grit blasting . Since the roughness of the finish depends
on the size of the grit , abrasives are furnished in different
grades. The following suggestions will serve as a guide.

Gr i t Size , Sieve openings ,

mesh inch Applications
Coarse -10 +30 0.079/0.024 For coatings exceeding
0.010 inch and best
adherence
Medium -14 +40 0 .056/0.017 For fair adherence and
smoother f i n i s h e s of
coatings less than
0.010 inch thick
Fine - 30 +80 0.024/ 0.007 For s m o o t h e s t f i n i s h e s
on coatings less than
0 . 0 10 i n c h t h i c k to be
used in as-sprayed
condition.

Even new grit is made up of a r a n g e in sizes. Ordinarily, - however ,

at least 80 percent of the particles will remain on a screen two
sieve numbers hi g h e r tha n th e s m a l l est s iz e men tione d above , e.g.,
80 percent of the grit passing through the No. 14 s c r e e n would be
expected to be retained by a No. 25 s i e v e .

Blocky, angular particles of alumina are the recommended

a b r a s i v e s f o r g r i t b l a s t i n g substrates to be plasma sprayed .
Silicon carbide grit is also suitable , but is more expensive . A
blasting pressure on the order of 80 psi is normally appropriate
for hard substrates. Lighter pressures should be used for softer
w o r k p ieces such as aluminum , copper , their alloys , a nd b ronz es.
That practice will minimize the likelihood of embedding particles
of the grit in the substrate . Dust adhering to the workp iece,
from the grit blastin g operation , should be removed by air blasting
or brushin g before sta rt in q the plasma spraying operation .

45

S
--~~~~~ --- ~~~~~~ -~~~~ ~~ ~~~~~~ -.
 --

TABLE XVI . BOND STRENGTH DATA FOR ALUMINA COATINGS

PLASMA SpRAyED (a) ONTO STEEL SUBSTRATES
WITH VARIOUS ROUGHNESSES (19)

Median
P owd er S ize , Surface Roughness , Bond
microinch microinch Strength , (e)
Powder (b) Purity Range Median rms (c) AA (d) psi

A 97. 156/1840 750 280 420 545

B 98.0 148/1580 350 115 170 270

225 340 390
280 420 440

C 99.49 292/3280 456 280 420 510

D 99.49 13 6/ 1 5 2 0 635 115 170 380

225 340 540
280 420 600

(a) Arc current, 400 amperes; arc voltage , 70 volts ; powder feed
ra t e , 2 lb/hr; torch to substrate distance , 6 in.; arc gas ,
100 cu ft dry nitrogen and 15 cu ft hydrogen/hr; nitrogen
carrier gas flow , 10 cu ft/hr.
(b ) All p o w d e r s d e t e r m i n e d to be 100 oercent alp ha alumina by
X-ray diffraction.
(c) Roughness values reported in nonstandard rms values.
(d) Roughness values converted to standard values by an
app roxima ti o n .
(e) Determined by a shearing test.

Typically , nozzle-to-substrate distances of 2 to 6 inches

are used for grit b l a s t i n g . V a r i a t i o n s w i t h i n t h a t r a n g e seem to
have little effect on roughness , but may affect coverage. Impinge-
ment angles near 90° give best results.

There is no dependable formula for predicting the minimum

time needed to produce a grit-blasted surface suitable for plasma
spraying . A suitable blasting t ime should be established by ex-
periment with the equi pment to be used in production and with
specimens comparable to the substrate of interest . The time can
be judged by v is u a l in s p e c t ion f o r un i f orm cover age a nd su r f ace
texture.

46

I
r - __

3.3.2.2 Shot Peeni~ g

Peening is a cold working process that deforms the mate-

rial near the surface of the workpiece and creates compressive
stresses in that region. Shot peening, like grit blasting, is
accomplished by a hi gh-velocity stream of metal particles suspended
in compressed air directed at the metal substrate . The impact of
individual particles of shot creates rounded depressions in the
surface and deformation to a depth of 0.005 to 0.010 inch below
the surface of the substrate. Compressive stresses are set up in
the deformed material because it has a larger surface area and is
attached to the unstrained material deeper in the substrate. Con-
t ro l l ed , severe peening can produce compressive stresses at the
surface ranging up to half the y ield strength of hard metals.
Such residual stresses are desirable when the surface layers will
be subject to tensile stress in subsequent operations or service.
The beneficial effects of compressive residual stresses in bending
fati gue are well known . It has been established rather recently
that shot peening is also a desirable and beneficial method of
preparing surfaces for plasma—arc spraying .

Data obtained by Bethke of NADC-W arminster on t h e e f f e c t s

of surface preparation methods on fatigue properties of high
strength steel , with and without pla sma-sprayed coatings , are
p r e s e n t e d i n T a b l e X V I I . (20) The data were obtained on rotating-
beam fatigue specimens (0.250 x 3.42 inch qaqe length) of 4340
s teel , heat treated to 280 ,000 psi. Precautions were taken during
plasma spray ing to avoid beating the substrates above 275 F.
F a t i g u e t e s t s were made at two stress levels in order to determine
the effects of processinq variables. As is normally the case ,
shot peening improved the fati gue life of the steel appreciably in
both short and lona cycle fati gue . Grit blasting caused much less
improvement than peening. More importantly, the data also show
that specimens coated after grit blasting had poor fati gue proper-
ties , lower than the base metal. On the other hand , specimens
that had been shot peened , then grit blasted and coated by plasma
spraying had very good fatique properties. The data indicate that
peening should be seriousl y considered as a method for preparing
surfaces of components when the hi uh e st—qua l ity plasma—sprayed
coatings are required on components subject to fatigue .

Shot peening is normall y performed by dry blasting with

cast steel shot having a hardness of Rockwell C 40 to 50. Glass
beads are often used for peenir ,q materials that would be contam-
inated by embedded iron such as alum inum , titanium , or stainless
steel. W orkpiece areas that should not be peeried should be pro-
tected from the blast by masks.

47

I
 - -
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Q 6 a) 5-i a) ‘-4 a) a) 6 .0 0 ‘0 0.) 4-4
U)~ a) O s )~~~a)~~~~~ Q-,

48

1
 Cast metal shot for peening operations is available in
d i f f e r e n t s i z e s ; those i d e n t i f i e d in Table X V I I I can be used f o r
mos t application . The sho t size number denotes the diameter , in
ten thousa nd ths of an inch , of the major fraction of the particles.

TABLE XV III. TYPICAL SPECIFICATIONS FOR CAST IRON

AND STEEL SHOT FOR SHOT PEENING (21)

Cumulative Screen
Shot Size Sieve Fraction , Opening, Scree n
Numbe r percent in. Number

S 280 0 0.0469 16
5 max. on 0.0394 18
85 m m . on 0 .0 2 8 0 25
96 m m . on 0.0232 30

S 230 0 0.0394 18
10 max. on 0.0331 20
85 m m . on 0.0232 30
97 m m . on 0.0197 35

S 170 0 0.0331 20
10 m a x . on 0 .0280 25
85 m m . on 0 .0165 40
97 in n , on 0.0138 45

S 110 0 0.0232 30
10 max. on 0 .0197 35
80 m m . on 0.0117 50
90 m m . on 0 .0070 80

S 70 0 0.0165 40
10 max. on 0.0138 45
80 m m . on 0.0070 80
90 m m . on 0.0049 120

The effects of shot peening on deformation and residual

stresses , the characteristics conferring benefits , depend on cover-
age and peening intensity. The depth of the deformed layer in-
creases with peening intensity . The lowest peening intensity pro-
viding the desired effect on the workpiece is most efficient and
least expensive . Methods of evaluating peening intensity for con-
ditions of interest , by m ea s u r ing e f f e c t s p rodu ced on a s t and a rd
specimen , are described in the section on quality control. Inten-
sity tests should be made at appropriate intervals to check whether
conditions for producing selected peening intensities with avail-
able equi pment have changed with time .

49

I
 S u r f a c e coverage , sometimes c a l l e d saturation , i s a m easure
of how c o m p l e t e l y an area has been hit by the shot particles. Un-
less coverag e is ade qua te l y complete , the full benefits of peening
will not be obtained . Various methods have been used to judge the
e x t e n t of coverage by p e e n i n g . V i s u a l e x a m i n a t i o n i s w i d e l y used
and adequate for j u d g i n g the o p e r a t i o n as a method for p r e p a r i n g a
su rf a c e f or p l a s ma sp r a y i n g . Fortu na te l y , it has been established
that the coverage for short and long spraying times follows the
following relationships (2l )

Cn 1 — (l_C 1 ) n

where C 0 = coverage, expressed as a decimal , after peening f o r

n cycles
C1 = % coverage , expressed as a decima l , after peening f o r
1 cycle.

For instance, if peening for a 1-minute cycle produced 25 percent

covera ge (C 1 = 0 . 2 5 ) , p e e n i nq for 6 or 12 minutes is expected to
give coveraqes of 82 or 96.8 percent coverages , respec tively.
A r b i t r a r i l y , 98 p e r c e n t covs~rage is considered complete saturation;
coverage values beyond 98 1 ercent are expressed as multiples of
that time . For instance , a value of 1.5 means.the specimen was
peened 1.5 times as long as the period required for full coverage.

C h a n g e s i n a i r- b l a s t i n g p a r a m e t e r s that affect particle

velocities also affect peening intensities. The experimental data
in Table X IX show that increasin ~i the spacing between the nozzle
from 4 to 8 inches decreased the peening intensity appreciably.
For the conditions investigated with the 1/ -inch nozzle, increas-
ing the aspirator s~~ze considerably increased the peening intensity.
The aspirator setting was less important for the other two nozzle
sizes.

The anole between the direction of the stream of particles

and the surface of the substrate is known as the impinaement angle.
The maximum peening intensity is attained with an imp ingement angle
of 90° . Decreasing the imp ingement angle lowers the peening inten-
sity by an amount proportional to the sine of the angle. That is ,
for otherwise similar conditions , the effect of imp ingement angles
is:

Imp ingement angle 90° 60° 45° 30°

Relative peening intensity 1.0 0.87 0.71 0.50

-o
__ ~~----~~~~ - -- - ~~— ~~~~~~~~~~~~~~~~ =-~~~~~~ - - - - -~~~~~~ -
~~~

TABLE X I X . EFFECT OF N O Z Z L E S I Z E , ASPIRATOR SIZE ,

AND NOZZLE-WORK SPACING ON INTENSITY
OF SHOT P E E N I N G ( a ) (2 1 )

Nozzle Aspirator Peening Intensity, (b) for

Diameter , Size , Nozzle-Work Distance Indicated
inch inch 4 inch 6 inch 8 inch

3/8 5/32 5 5 5.5

7/ 3 2 5 5 4

1/2 5/32 3.5 3 3

7/32 7 7 5

5/8 5/32 7.5 5.5 7

9/32 7.S 7 6

(a) Tests mad e with suction-type shot peening test cabinet ,

5 70 steel shot , on 410 stainless steel b l a d e s ; b l as t
pressure 92 psi , flow of shot to nozzle , 7—1/4 lb/mm .

(b) Larger numbers indicate greater peening intensity .

Values indicate arc heights , in thousandth of an inch ,
for A-type A lmen test strips.

3.3.3 Macro-Rou ghening

Macro-roughening is a term used to describe methods for

producing large changes in surface topography to increase surface
area and reduce stresses induced by coating shrinkage. It involves
cutting urooves or deep striations into the substrate and is used
in instances where thick coatings over 0.030 in. are required .

This method is most often used in preparing cylindrical

sections for coating. The procedure usually followed is to mount
the cylindrical section in a lathe and cut deep , clo se l y spac ed
screw t h r e a d s i n t o t h e s u r f a c e . After threading, the part is grit
blasted and/or coated with a bonding layer of molybdenum or
nickel—aluminide.

On flat surfaces , the surface may be rough milled or

grooves or slots may be cut into the edges. This would again be
followed by grit blasting and/or bond coating .

51

- -- - .
-
--—---- - - — ---- — —
~ - ---- — - :-
__ --—- — -- - —-
- —-- - --.———.---- ,-

52

I-

. - --
-~~ ~~~~~- ~~ -
r
SECTION IV

4. MASKIN G TECHNIQUES AND MATERIALS

In many applications , on l y spec i f ic areas of a wo r k p iece

may need to be coated . In such cases , the areas adjacent to the
surface to be coated must be protected , both from unnecessary sur-
face roughening and from adherence of the sprayed material. The
technique of protecting the areas adjacent to the surface to be
grit blasted and/or plasma sprayed is masking. Separate types of
masking may be required for grit blasting and for spraying,
though in m a n y i n s t a n c e s the same mask may be used for both opera-
tions. Some masking materials used with success are listed in
Table XX .

4.1 MASKING FOR GRIT BLASTING

For m o s t g r i t - b l a s t m a s k i n g a p p l i c a t i o n s, or d i n a r y one—
inch-wide paper masking tape , applied several layers thick , a f f o r d s
satisfactory protection to adjacent surfaces. It has the advan-
tages of being inexpensive and easy to cut or shape as needed .
Howev er , since it is easily cut , it may be damaged in a heavy or
p r o l o n g e d b l a s t i n g o p e r a t i o n , r e s u l t i n g in grit penetration or edge
erosion , and consequent damage to the substrate. Also , this type
of tape should be removed prior to spraying to avoid coating con-
tamination or excessive build-up at the coating edge.

Adhesive-backed cloth , plastic , or rubber tapes or Teflon

are other suitable masking mate rials. They are easy to apply, pro-
vide protection , and are less likely to be damaged by abrasive
blasting. All of these materials should be removed before plasma
spraying.
Of the v a r i o u s t y p e s of tape available for masking , the
most suitable is the heat-resistant , metallic-coated cloth . tape ,
such as is used in many furnace or heating applications. This
material is also easy to apply to the areas to be protected , it is
not severely damaged in grit blasting , and can be left in place to
serve as a mask during coating.

For high-production grit blasting , taping is too slow a

process for masking . In this case metal or rubber shields may be
us ed , provided the geometry of the workpiece is not too complex.
Of the two materials , rubber is the better choice as grit blasting
mask because it is not cut by the grit blast abrasive , whe re as a
m e t a l mask will ultimately erode. However a metal grit blasting
mask may be used as a thermal spray mask as well , while rubber can-
not. The use of metal or rubber shield is not economical except
in high production applications.

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54
 —
—--- - ----~ -—.~~ -~--------- --- — -- - — — — - -- ---—— — — --- _~ — -- _
~~~~~

The use of tape or of metal or rubber shields is generally

limited to flat or cylindrical surfaces. In instances where holes ,
slo t s , k ey wa y s , or other types of recesses must be protected ,
inserts of carbon or metal should be used. These are left in place
during grit blasting and sprayinq, and usually are not removed
until completion of surface finishing .

4.2 Maskinq for Plasma Spray i n g

Basically, the same methods are used to mask for spraying

as are used in masking for grit blas ting; the difference is in the
choice of materials. As pointed out earlier , most grit blast
masking taoes must be removed prior to spraying. They may burn or
ch ar , or the adhesive backing may run. Combustion products or
soot may contaminate the coating. The exception is glass-fiber
tape , made for high-temperature use. It can withstand the spray
temperatures encountered in most coating operations and is a con-
venient and inexpensive material.

Where geometric considerations permit , smooth metal masks

may be used. Again , this method is best suited to a high-produc-
tion operation . Provision must be made , when usino metal masks ,
to prevent coating build-up on them. This may require that they 4

be water cooled , coated with a suitable “ stop-off” ma te r i a l , or

equipped with some mechanical means of removing deposited material.

Another masking techni que suitable for thermal spray

applications is the use of li quid rnaski nq compound . These com-
pounds , when applied over blasted areas adjacent to the desired
deposit area , act as stop-offs, to prevent the adherence of the
sprayed powders to the base metal in these areas. They may be
a p p l i e d by p a i n t i n g or d i p p i no f o l l o w i nq grit blasting , making
them rather inexpensive to use.

Threaded holes , slots , and kevwavs can he protected from

thermal sprayinq by metal , T e f l o n , o r carbon in ser t s , lef t in p lace
until after completion of finishing operations. In such areas ,
particularly around threaded holes , it may be desired that the
sprayed coating not end sharply, but rather taper to the edge of
the hole or some point near the edge. In such cases a t e c h n i que
referred to as shadow masking is used . In shadow oas kinq, the
area to be sprayed is partially shielded , by ra isin q the mask a
small distance off the surface , thus per m itt m u r ; r 1e nver spray to
~
extend under the mask to prod u e a f eat h e r i n ; it the coating ed ge
rather than a dis tinct boundary .
 56

_ _ _ _ _ _ _ _ _ _ _
-J
 - —--
- - _
-- -~~~~~~~~~- — --—
~~~~ ~~~~~~~~ ~~--- ~~~~~-——--- - —--— _

SECTION V

5. PLASMA-SPRAY DEPOSITION VARIABLES

In theory at least , a th o r o u g h k n o w l e d ge of th e e f f ec ts
of parametric variables of the plasma—spray process would permit
tailoring the characteristics of a coating to a specific applica-
t io n . For ex am p l e , coatings with an appropriate amount of porosity
may be desirable for retaining lubricants and minimizing wear under
some service conditions. For other applications high-density
coatings are preferable. Unfortunately , the state of the art does
not yet permit predicting the precise process parameters necessary
for producing coatings with the optimum characteristics for speci-
f ic appl ications. The pro b lem s r e su l t f r om the f a c t th at many
variables affec t the results of the plasma—spray process and their
inter~~ctions have not been established quantitatively. For in-
stance , several types of equipment are marketed and used for the
deposition process and they differ si gnificantly in desi gn and
operating characteristics. The control settings , especially the
selection of voltages and currents , appropriate for producing
satisfactory coatings vary with the plasma-arc units as well as
w i t h o t h e r parameters chosen by the operator. Under the circum-
stances , the most practical approach for choosing the operating
conditions best suited to a particular application is to use the
recommendations of the gun and powder suppliers as a guide. For
a combination of substrate and coating new to the operator , t h e
preliminary trial is best made on a specimen rather than an actual
component. If ary serious deficiencies in characteristics of the
coating are noted on the trial specimen , it is desirable to conduct
additional experiments with s i ghtly different process parameters.
In order to be helpful , some information on the effects of changing
parametric variables on process and product characteristics are
given in this section. When the conditions considered most suit-
able have been selected , they should be closely reproduced in
p lasma spraying the components to be used in service . To do so ,
the use of automated or semiautomated control of gun movements and
other process variables is strongly recommended . The control of
process variables is too critical and difficult to be achieved by
manual sprayin~~.

In general , the information in this section is concerned

with producing coatings of the high quality needed for severe ser-
vice in aircraft and Naval Ordnance . The selection of plasma-
spray ing conditions depends more on the properties of the material
to be deposited than on the properties of the substrate. Neverthe-
less , it should be noted that the substrates of greatest interest
were identified by Naval Ordnance personnel as:

57
 Carbon steel Aluminum bronze
Low-alloy steel Valve bronzes
S t a i n l e s s steel K—Monel
Aluminum alloys Brass

The sec tion on d ata sh e e t s , in th i s repo rt , l i s t s som e spec i f ic

conditions found suitable for depositing good coatings w i t h one
pa rtic u l a r t y p e of plasma-spray gun . Those parameters should be
adjusted when other types of equipment are employed .

F i g u r e 13 shows the modules constituting a plasma-arc

s p r a y i n g s y s t e m and s u g g e s t s t h e v a r i a b l e s that must be controlled .
The power l e v e l , the p ress ure and f l o w of the ar c gases , and t h e
ra t e of f l o w of powder and carrier gas are controlled at the con-
sole of the system . The gun orientation and gun-to-work distance
are usua l ly prese t , and the movement of the workpiece is ordinaril y
controlled by using automated or semiautomated t o o l i n g . Substrate
tempera tures shoul d be co ntro l l e d by pr ehea ting and by l im it in g
the t e m p e r a t u r e changes d u r i n g p r o c e s s i n g .

5.1 A RC GAS ES

The selection of the arc gas depends on the type of mate-

rial to be sprayed and to some extent on the type of plasma-arc
equ ipment to be used. All equipment and most spray-material sup-
p l i e r s g ive recommenda tions as to t h e types of a rc g ases to be
used w i t h par ticul ar types of powders.

Generally a nonoxidizing gas is required to form the

plasma and the inert gases helium and argon are often us~ed . Nitro-
gen i s also a co mmon arc ga s , except for spraying materials that
would be e m b r i t t l e d by contamination with nitrogen . The principal
adva ntage is t h a t d i a tomic gase s such as n itr ogen a nd hy dro gen have
higher heat contents , at the same h i g h t e m p e r a t u r e , t h a n h e l i u m or
a r g o n . T h a t p o i n t is illustrated in Figure 14 , attributed to Dunham
by F is h e r . (22) Higher heat contents are particularly desirable for
s p r a y i n g r e f r a c t o r y ma te r i a l s s u ch a s oxide s , if care is taken to
preve n t overhea ti n g the s u b s t r a t e s . On the o ther hand , if the heat
content is unusually high , nozzle erosion may be severe . Therefore ,
it is common prac t ice to us e a rg on as the pri m ary a rc ga s and u se
some hydro gets or nitrogen as the secondary gas to form the plasma .
Frequently mixtures of 5 to 25 percent hydrogen are used for the
arc gas , with the primary gas being argon or nitrogen. Argon is
preferable to avoid trouble from contamination or excessive
porosi ty .

The compos it i o n of the arc ga s i n f l uences t h e a r c v o l t age

and the power level. A higher current is needed for maintaining
a part icular power level for pure-argon arc gas than for mixtures
of argon with hydrogen or nitrogen .

58
 - _

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_ _ _ _ >. r

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59

_ _ _ _ _ _
-- --- ~~~ --~~~~~~~~~~~~~~ --
-.
_ _ _ _
 - ________ ___________

0H

Te mpercture ,K x IO~

FIGURE 14. ENERGY CONTENT OF GASES AT D I F F E R E N T

TEMPERATURES , ADAPTED FROM DATA BY
DUNHAM BY FISHER (22)
(Temperature °K = °C + 273)

The initial and partial control for the flow of arc gas
is provided by a two-stage, hi gh-pressure regulator at the gas
supply , as suggested in Figure 13. The finer and more critical
c o n t r o l is established by setting the flow meters on the plasma
system console. Those flow meters are calibrated to operate from
specific input pressures specified by the system manufacturers.
T h e r e f o r e , it is essential that the two-stage regulators be set
prope r l y . I t i s , of course , equally important to set properly
the flow meters to deliver the flow specified by the parameter or
process instructions for spraying a given material. It is of par-
ticular importance to obtain the proper flow of secondary arc gas ,
as this setting controls the voltage value.

Excess ive f l o w ra tes of t h e a r c gases a nd , in particular ,

the primary -arc gas will remove useful heat from the plasma stream
and at the same time increase spray particle velocity which , in
turn , reduces the dw el l time of the s p r a y par ti c l e s in the p lasma
s t r e am . As a consequence , m uch of the s p ray m a t er ia l w i ll no t
attain the semimolten or plastic state necessary to achieve the
deformation which permits the powder particles to adhere to the
base me ta l and to co h e r e to one ano the r . The r e s u l tan t coa ti ng
w i l l lack p roper b ond s tr en gt h , coating strength , de nsity, and
hardness. Add itionally, there will be a marked decrease in deposit
efficiency.

60

IL - - - -
 —- - - -
- _ _ _ _

Co n v e r s e l y , low arc gas flow r a t e s r e s u l t i n im pro p er

volta ge values and greatly reduced particle v e l o c i t i e s . In ex-
treme cases , in s u f f i c i e nt arc gas f l o w can r e s u l t in o v e r h e a t in g
of the spray m a t e r i a l p ar ti cles to th e po int tha t the m a t e r i a l
will be vapor ized or the spray material will melt prematurely and
p lu g the p owder in j e c t io n par t at the po int of inj e c t i o n in to the
plasma s t r e a m . In a ddi t i o n , a very low arc gas flow can resul t
in the collec t io n of mol te n powde r p a rti cles in the spray no z z l e
or powder injection port and subsequently depositing this material
into the coating as a large globule. Upon grinding or masking the
coating, this globule will result in a rather large coating void.
If the spr ay oper at or obs er v e s a la rge glo bu le of s p r a y m a t e r i a l
being deposited onto the coating, he may be a b le to remove i t , pro-
viding the spray operation can be stopped before a great deal of
additional material is deposited over the globule.

Finally, under the proper circumstance , a ve ry low a r c

gas flow will resul t i n damage to the spray device in the form of
extremely heavy ero ”lnn of the spray nozzle or destruction of the
spray gun housing as a result of internal arcing .

The qua li t - it ive effects of varying the flow rate on de-

position efficiency and on coating density are shown in Figures
15 and 16. The sketche s illustrate the effects expected when
other spraying varma bles are held constant. It should be noted
that there is an o~ t m u m rate for gas flow and that the optimum
rate varies with other spraying variables .

- o ’ i 0W, 0 ; .
~ ~~ ~

FIGURE 15. THE EFFECT OF ARC GAS FLOW ON COATING

DENSITY FOR OTHERWISE CONSTANT CONDITIONS (23)

61

I
.
- -~~~~~~~~ -
-

00

Incre as ing Arc Gas Flow Rate

FIGURE 16. EFFECT OF ARC GAS FLOW RATE ON SPRAYING EFFICIENCY ,

ADAPTED FROM DATA BY ATKINS BY FISI-iER~ 22)

After the arc gas and cooling water are turned on and the
f l o w rates adjusted to the desired levels , the arc can be initiated.
Nost control systems are interlocked so the equi pment will not
operate without a flow of coolant. The voltage of the d-c arc
depends on the gun design and the plasma forming gas.

5.2 ARC POWER LEVEL

The maximum power rating of a plasma gun is limited by

its design , principally by the efficiency of the system for cool-
ing the electrode. The power level of the arc , expressed in kW ,
is the product of the voltage and the current in amperes. T~~
power leve l controls the temperature and influences the heat con-
tent of the arc. Higher power levels are useful in spraying
materials with higher melting points.

The control of voltage is a function of the type and flow

ra t e of t h e ar c g ase s , p r ima r i l y of the se c o n d a r y a r c g as. The
voltage can be raised or lowered by increasing or decreasing the
flow rate of the secondary gas which is usually either hydrogen
or helium. Some authorities do not recommend increasing the
hydrogen flow rate to increase the voltage.

Failure to attain the voltage value specified by the pro-

cess ins tr u c ti on shee t w ith in t h e arc gas f l o w l im its es ta b l ished
by t h e process ins tr u c ti on shee t u s u a l l y in d ic a t e s th a t th e a r c

62
le ng th is too lon g an d t h a t the ~ :ont and rear electrodes in the
plasma gun should be replaced because of erosion . Since the arc
length is proportional to voltage , rotating the nozzle will some-
times res tore the vol tage to th e desir ed level be c a u s e the a r c
will travel to an uneroded spot.

If the voltage is within the recommended range but the

power l e v e l is outside the desired range , the current should be
adjusted. Figure 17 indicates that there is an optimum power
leve l for otherwise constant spray ing conditions . The o p t i m um
power is particularly sensitive to powder composition and particle
size because those characteristics set the heating requirements.
Even though the desired power level is attained on starting the
plasma-spray system , the console indicators should be monitored.
This prevents undetected changes caused by fluctuations in line
voltage, changes in flow of the secondary arc gas , or erosion of
the electrodes . Settings should be chanqed when necessary.

FIGURE 17. EFFECT OF ARC-POWER LEVEL ON D E N S I T Y OF P L A S M A - S P R A Y E D

COATINGS FOR OTHERWISE CONSTANT CONDITIONS (23 )

U s i n g power l e v e l s b e l o w t h e o p t i m u m r e s u l t s in inadequate
heating of sprayed particles , lower bond strengths , coating strengths ,
h a rd ne sses , and deposition efficiencies .

Exceeding the optimum arc-power levels raises costs by

wasting power and accelerating deterioration of gun components.
Excessive power can vaporize some of the spray material and cause
changes in composition. Condensation of the vapor on the substrate ,
or between layers of laminated coatings, results in poo r bonding.

63

I
 --
_

5.3 POWDER SIZES AND FEEDING RATES

The size of the particles used for plasma-arc spraying is

i m p o r t a n t . The s i z e a f f e c t s t h e o p t i m u m power l e v e l se t t i n g and
gas f l o w r a t e because l a r g e r p a r t i c l e s r e q u i r e mor e hea t and
l o n g e r d w e l l t i m e s for melting . Particle size also influences
coating quality because it affects the kinetic energy of the moving
p a r t i c l e s at t h e t i m e t h e y h i t t h e substrate. Excessively fine
p a r t i c l e s d e c e l e r a t e r a p i d l y d u r i n g s p r a y i n g and produce coatings
w i t h lower d e n s i t i e s and poorer deposition efficiencies .

Experience indicates that the optimum particle size is

ordinarily in the range of 140 to 325 mesh (0.0041—0.0017 inch) .
Some investigators report that larger particles in that size
r a n g e are preferable because they are better able to hold heat
and to d e f o r m a r o u n d surface irregularities to give better bond
strengths. Any supply of powder consists of particles of differ-
ent sizes. Whether the particle—size distribution should be wide
or narrow within the limits mentioned is not known with certainty.
Contradictory results have been reported by different investi ga-
tors. Some favor a narrow range to promote chemical uniformity.
Others prefer a more uniform distribution of different sizes and
recommend blending of powders to achieve it , in an effort to obtain
better densities and bond strengths. Table XX I lists the particle
size ranges of some powders used successfully for plasma-arc
spraying .

In establishing suitable plasma-arc spraying parameters

for a particular material , a consistent feed rate is of the utmost
importance . This factor must be controlled to determine the level
of power required to provide c~dequate particle melting . Should
the powder feed rate exceed the value used to establish the power
setting , the particles will not be heated adequately, resulting in
a weak , porous structure and a lower deposition efficiency . Con-
v e r s e l y , lower material feed rates will result in overheating
and vaporization of the spray material.

All commercial feed devices are capable of rather precise

contro l (within 2 percent) of the amount of spray material fed
through the unit in a given period . The feed rate is generally
expressed in pounds per hour (lb/hr) . Powder feeders use wheels
or sc rews ~to deliver a fixed volume of material from the hopper
to the stream of carrier gas. Consequently, the weight of powder
fed at a particular setting increases with the bulk density of
the material. Variations in composition , shape (spherical , f l a k e ,
or an gu l a r pa r ti c l e s ) and size of powders a f f e c t bu l k de n s ity and
,

feeding rates based on weight.

It is extremely important to blend the spray material

properly to eliminate segregation or stratification by particle
size , wh ich can occur dur ing sh ipment or storage. The finer par-
ticles will generally settle to the bottom of the container , form-
ing layers characterized by different particle sizes. Proper

64

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65

— I

- .
 -

~~~~~~~~~~~~~~~

blending eliminates t h i s condition , which o t h e r w i s e produces a

g r a d u a l change in b u l k d e n s i t y f r o m top to b o t t o m of the powder
hopper , and t h u s a change in a c t u a l f e e d r a te .

A l t h o u g h one can be r e a s o n a b l y c e r t a i n of r e p e a t a b i l i t y of
the m a t e r i a l d e l i v e r y r a t e at th e p o i n t the m a t e r i a l leaves t h e
feeder , o t h e r f a c t o r s can s e r i o u s l y a f fe c t both t h e q u a n t i t y and
c o n s i s t e n c y of t h e feed r a t e at the po i n t of in jec tion in to the
plasma s t r e a m :

( 1) L e n g t h and d i a m e t e r of t h e powder feed l i n e , and

(2) Spray m a t e r i a l f o r m and s i z e .

Ge n e r a l l y spe ak ing , i f the s tan d a r d sp ray ma teri al feed

lines supplied by the spray dev ice m a n u f a c tu rer are u t il i zed , the
powder feed line will probably not cause feeding problems , provid-
in g there are no sharp bends in the l i n e as a r e s u l t of the manner
in which the uni t is set up.

Fr e q u e n t l y , it has b een no ted tha t spray equipmen t users

will improv ise material feed lines. Changes in either the length
or interior diameter of the powder feed line will result in either
or bo th a lowering of the f e ed ra te or , wo r se , a pulsation in the
feed rate . Should the spray material be injected into the plasma
strea m in b u r s ts , relatively improperly heated particles will be
deposited into the coating, resulting in a loosely bonded porous
structure with areas of varying hardness.

Feed rates are affected by moisture contents of the powder

and by erosion of the injection ports or other components. Powder—
feeding rates are influenced to a minor extent by the flow rate
of the carrier gas. More importantly, if the gas flow rate is too
h i g h , transit times are shorter and particles w i l l not be heated
thoroughly by the plasma stream .

5.4 GUN-TO-WORK DISTANCE

The gun-to-work or spray nozzle-to-work distance primaril y

affects the following plasma-arc spraying parameters :

(1) Spray particle velocity at the point of impinge-

ment on the substrate or coating .
(2) Spray particle temperature at the point of
impingement on the coating or substrate.
(3) The temperature of both substrate and coating .

The characteristics of the coatings are very sensitive to the gun-

workp iece distance . Depending on the equipment, power level , mate-
r i a l comb i na ti o n s , and other conditions , there is an optimum spac-
ing that must be determined by experiment. Most materials are
sprayed at gun-workpiece distances ranging from 2 to 5 inches; the

66

— —
$

-: .
~~~~~~ -~~~~~~~~~~~ -
- - -- — -~~~~~ - _ - --- -— - - — --
~ - -~~~~~~~~~~~~ -~~~~~~~~~~~~

spacing considered suitable should be controlled within 0.2 inch

for critical applications . Such precision is difficult or impos-
sible with hand-held guns.

It can readily be appreciated that the spray particle

velocity will diminish as the particles travel from the spray
no z z l e to the work pi ece. They a l s o sta rt to cool as they l e a v e
the stream of plasma . Therefore , excessive spray nozzle-to-work
distances result in less particle deformation and , consequen tly ,
in loosely bonded , porous and weak coating structures , and a sub-
stantial loss in deposition efficiency .

Too short a spray nozzle-to-work distance is probably more

destructive to coating properties than an excessive distance .
Certainly it can be stated that the results are more pronounced
and instantly obvious. Severe oxjdation of the substrate and coat-
ing will occur. This , in turn , weakens or , depending on the degree
of oxidation , completely destroys the substrate-~ o-coating bond .
Additionally, the substrate would naturally expand as a function
of coefficient of therma l expansion and , depending on the match
between the coefficients of therma l expansion between substrate
and coating, spalling could occur.

It should be noted , h owev er , that if adequate coating and

substrate cooling can be maintained , extremely dense coatings will
r e s u l t f r o m u s i n g t h e m i n i m u m p r a c t i c a l spray nozzle-work distances.
One of the more effective methods of cooling for very close gun
distances is the use of liquid CO2 sprayed onto the part both
immedia t ely p r e c e d i n g and f o l l o w i n g t he p oin t of s p r a y imp i ngement.
It is strongly recommended that the spray nozzle-work dis-
tance be controlled by mechanical fixturing. Only by the use of
automated spray tooling can consistent coating quality be assured.

Table XX II illustrates the effect of different gun—to-work

distances on the porosity of plasma-sprayed coatings when other
deposition variables are held constant. The data were obtained
by Nimvitskaya and Fishman in experimental coating of carbon steel
with aluminum oxide , using Russian equipment. (24) The porosity of
t h e a l u m i n a c o a t i n g was measured by filling the pores with a stand-
ardized procedure and weighing . That technique probably determines
only the vnlume of interconnected voids open to the surface.

5.5 SPRAY ANGLE

The spray angle designates the attitude of the spray

nozzle in relationship to the substrate. As indicated in Figure 18 ,
the plasma stream is ordinarily directed at the substrate at a
spray angle of 90° . Spraying perpendicular to the substrate gives
better deposition efficiencies. In theory , that spray angle should
also result in better bond and coating strengths , bu t tho se poin t s
have not been investigated extensively. Unless it is substantiated

67

_ _
-- ~~~~ -- - ~ - - - - -. -.
~~~~~ ~~~~~~~~~~~~~
-
-
- - -
-
 TABLE XXII. EFFECTS OF ARC GAS AND OF GUN-WORKPIECE
DISTANCE ON POROSITY OF PLASMA-SPRAYED
ALUMINA COATING (24)

Gun-Work Coating
D i s tance , Porosity ,
Arc Ga s and Pressures (a) in. percent

Argon , 28.5 psi- 4 7.7 5

+ Nitrogen , 25 . 7 ps i 6 21 6
8 44 :3

Nitrogen , 28.5 psi 6 27.6

N i t r o g e n , 2 8 . 5 psi 4 4.35
+ Hel ium , 14.3 psi 8 9.8

N •i t r o g e n , 2 8 . 5 psi- 4 12.1
+ Helium , 28.5 psi
6 9 7
8 25.8

(a) Pressure in powder feeder , 1.46 psi.

by t e s t i n g f o r a g i v e n a p p l i c a t i o n or r e q u i re d f o r a p a r t i c u l a r
w o r k p i e c e c o n f i g u r a t i o n , t h e s p r a y n o z z l e s h o u l d not be set at
greater than a 15-degree angle from the perpendicular to the
workpiece .

For some applications where maximum coating and density

is not r e q u i r e d , satisfactory results have been obtained with a
spray a n g l e as l a r g e as 45 degrees. Decisions on spray angles
should be based on tests with appropriate specimens and metal-
lographic examination.

The prime concern in spraying at too great an angle is

that the spray particles will tend to skid rather than flatten
upon impacting .

68

1
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g i l I
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FIGURE 18. TYPICAL CONTOUR OF SPRAY DEPOSIT

69

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.
-- - _ -_ _ - _ _ -- -
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- - - -
5.6 SURFACE SPEED OF DEPOSITION

The term s u r f a c e speed of d e p o s i t i o n is a n a l o g o u s to t h e

s u r f a c e c u t t i n g speed in m a c h i n i n g o p e r a t i o n s . S p e c i f i c a l ly , i t
is the speed at which t h e s u r f a c e of the s u b s t r a t e passes the spray
gun n o z z l e and is c o n t r o l l e d by the r a t e of gun movement and either
the rotational or sliding movemen t of the s u b s t r a t e. I t is essen-
tial tha t au toma ted or semiautoma te d tool ing b e employed to control
p r o p e r l y the s u r f a c e speed of d e p o s i t i o n .

A b a s i c c r i t e r i o n t h a t may be used to e s t a b l i s h t h e proper

s u r f a c e speed is t h a t t h e t h i c k n e s s of the s p r a y m a t e r i a l d e p o s i t e d
in a s i n g l e pass should not exceed 0.006 inch . Should the required
c o a t i n g t h i c k n e s s be in t h e 0 . 0 0 6 to 0.008 inch range , the coating
should be a p p l i e d in a minimum of two passes. An appropriate sur-
face speed of d eposit ion can b e c a lcula te d from k nowl ed ge of the
densi ty of the coa ti ng mat e r ial , the recommended rate of deposition
in weight/unit time , and the wi dth and th ick ness of the d e s i r e d
coating.

The two primary concerns in choosing the surface speed of

deposition are that the speed be sufficient to prevent overheating
of the substrate and/or coating , and that the gun-work distance
and t h e l ate r a l feed of the gun or subs tra te prod uce a s p r a y ed
deposi t f l a t and f r e e of r id ges -- in o t h e r words , the proper spray
pa tt e r n o v e r l a p . Figu re 19 il l u s trates the e f f e c t of in s u f f ic ien t
pass o v e r l a p on sur f a c e co nto u r . I t ca n read i ly be se en th at
i n s u f f i c ie nt pass ove r l a p , which is greatly magnified in the figure ,
would res ul t in a lack of f in i s h stock in some a rea s , although a
micrometer reading would not detect this condition.

rw Y / / / /’/)/ ’x’)) ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

— 0

~~ ~

FIGURE 19. INSUFFICIENT PASS OVERLAP

70
 - -- - - - -
- ~~~~~~

5.7 PROCESS TEMPERATURE CONTROL

The t e m p e r a t u r e g r a d i e n t developed d u r i n g spraying influ-

ences the residual stresses in the coating and substrate. Further-
more , the effective temperature of the substrate affects the time
for mol ten particles to freeze, to react with contaminants in the
gas stream , or to react with the substrate . Therefore , it is com-
mon prac tic e to p r ovide some means of process temp era tu r e c o n t r o l
in addition to that characteristic of the other plasma-arc deposi-
tion variables employed . Usually, the substrate is preheated
b e f o r e spray ing and cooled during the deposition operation .

Substrates are preheated for several purposes. Heating

substrates to 250 F will prevent condensation of water vapor in
the gaseous environment. More importantly, preheating minimizes
t he therma l sho ck of mol ten par ti cles s tr ik i n g the colde r su bstra te
and the res id u a l stresses in c o a t i n g s a nd coa ted com ponen ts. For
the l a t ter reaso n , preheating is par ti c ul a r l y d e s i r a b l e when
depositing thicker coatings. The maximum preheating temperature
depends ma in ly on th e b ase mater ia l an d th e tempera ture r i se tha t
w i ll occur d ur ing spray i n g . For ins tanc e , high-strength steel
workpieces will soften if heated to temperatures above those used
for tempering them during heat treatment. High preheating may be
undesirable when the differences in therma l expansion coefficients
of the coating and substrate are large enough to cause high
stresses from cooling between the preheating and room temperature .

I t is us ua l l y desi ra b l e to prov ide some cooli ng in o r d e r

to p r e v e n t the t e m p e r a t u r e r i s e d u r i n g p r o c e s s i ng f r o m e x c e e d i n g
300 F . C o o l i n g is especially desirable for substrates with low
m e l t i n g p o i n t s , and f o r c o a t i n g s e x t r e m e l y s u s c e p t i b l e to o x i d a t i o n .
Th in su b s t r a t e s are of ten cl amped to mass ive com ponent s in o rde r
to provide a better heat sink , faster cooling , and low er av era ge
process t e m p e r a t u r e s . R ac i d c o o l i n g is desirable for some coating
materials , molybdenum for instance , because it results in a smaller
grain size and higher strength. Cooling is usually provided by
directing blasts of compressed , clean, d r y a ir , carbon dioxide ,
or inert gas at the substrate or at positions just ahead of or be-
h i n d t h e plasma strea m .

71

I
72
 SECTION VI

6. POST-SPRAY FINISHING AND TREATING OPERATIONS

Two features common to all “as-deposited” plasm a-sprayed

coatings are their surface texture and their porosity . The sur-
face roughness of a typical plasma-sprayed coating measures in
the range of 225—450 microinches (AA ) -- a fairly rough , abrasive
surface. The porosity usually ranges from 3 to 15 percent by
volum e , depending on the material sprayed and the intended use
for the coating . In most cases , plasma-sprayed coatings are
applied to machine elements and the coated part must conform to
close dimensional tolerances or have a smooth configuration or a
particularly a c c u r a t e s h a p e . I n s u c h a p p l i c a t i o n s, c o a t i n g s a r e
often exposed to machine oils or other industrial fluids , which
can infiltrate a porous coating, resulting in fluid leakage or
corrosion of the substrate. Consequently, many applications re-
quire plasma-sprayed coatings to be sealed and surface finished
after sprayinc .

6.1 Sealing

I n m o s t t h e r m a l s p r a y e d c o a t i n g s , t h e p o r o s i t y , wh ich
m a y r a n g e as h i g h as 15 percent by volume , is interconnecting,
making the coating pervious to gases or liquids. This permea-
bility can leeve the substrate vulnerable to corrosive attack or
• can result in undesired fluid leakage in certain machine element
a p p l i c a t i o n s ( e . g . , a coated piston in a hydraulic cylinder).
F u r t h e r m o r e , s u r f a c e p o r o s i t y i n c r e a s e s the difficulty of produc-
ing a smooth finish by machining or grinding .

To prevent corrosive attack or fluid leakage , it is nec-

essary to seal the pores prior to surface finishing. Wax , phen-
olic ,or inorganic sealers are readily available and easily applied .
Waxes are useful in preventing infiltration of liquids at low
service temperatures , resin—base sealers are effective for service
ib~ ve t h e boiling point of water to 500 F , and some silicon—base
s~~ i l e r s h a v e p r o v i d e d e f f e c t i v e p r o t e c t i o n in salt-spray tests
~- 1 € ’ according to military standards up to 900 F. Epoxy and
--

~;~~~ n 1 ic scalers a r e g e n e r a l l y e f f e c t i v e w i t h i n t h e temperature

~~ i . s of stability.
Th~ m o s t e f f e c t i v e m e t h o dof s e a l e r a p p l i c a t i o n is v a c u um
- . , w h i c h may be u s e d to fill all accessible porosity.
~
• ~~~~ is immersed in a container of epoxy resin and the
- r : 1 iced in a vacuum chamber. A vacuum is drawn , pulling
‘ -
~
~~. ‘ c~o i ’ i r ~~ porosity. When the vacuum is released ,
- -~~

ss :re forces sealer into the evacuated pores. Most

(C(
!
~ ~u ire such thorough penetration. Commercially
-
‘
-
- --
~ us i t scalers , which set by an anaerobic reaction

73

I
o r by h e a t c u r in g can be b r u s h e d or sp ray ed on to a coated s u r f a c e
at room temperature and are drawn into pores by capillary action.
The dep th of penetration may be as much as 0.030 in. in some
instances. It is important that the sealer penetration be suffi-
ciently deep that it is not removed during the subsequent finish-
ing operation.

Other methods of impregnation are sometimes suitable for

filling pores in sprayed coatings to prevent infiltration of air
or fluids during service. Roseberry and his colleagues investi-
gated the efficacy of pressure impregnation and a simpler treat-
ment for sealing or filling porosity . ( 9 ) Two metallic coatings ,
molybdenum and the 8OCr-2ONi alloy , and two oxides , blended
Al 20 3 _ l3TiO and Cr~ O~ were used in that work. The coatings ,
0.022 and 0.030 ~n. in thickness , had been plasma sprayed on the
following substrates:

1020 steel K Monel

316 stainless steel brass
molybdenum 6061-T 1 aluminum -

The process parameters used for s r r a v i n ~ a r e r e c o r d e d by d a t a

sheets in Section IX .

Rods for hydraulic cylinders ‘.‘~ere treated with sealing

materials to prevent infiltration of the coatings by air or hy-
draulic fluid during service. Two types of sealer were evaluated
for filling the as—surayed coatings: a low-viscosity, single—
component polyester resin ([- .ocktite 290) and a c l e a r , s y n t h e t i c
,

phenolic resin (Metco Type BP) -

The phenolic sealer was applied to the as-sprayed coatings

b y i m m e r s i n g t h e c o m p o n e n t s i n a bath of the resin enclOsed i n a
pressure chamber. The vessel was then pressurized with air to
250 psi and held for five minut es. After removal from the chamber ,
the impregnated components were beatec ~ in an oven at 350 F for one
hour to cure the phenolic resin.

The polyester resin sealant was aup lied by brushing the

coated shafts as they were rotated in a lathe. Because of its low
viscosity, the resin was drawn into the open pores by capillary
action. It hardened by an anaerobic process (oxygen not required
for curing) . A f t e r b e i n g w e t t ed t h o r o u g h l y by t h e p o l y e s t e r, t h e
sealing material was allowed to harden in air and then post-cured
by heating for 30 minutes at 250 F.

B a s e d b o t h on p e r f o r m a n c e a n d on e a s e of a p p l i c a t i o n, the
p o l y e s t e r resin sealant (Loctite 290) was selected for use on the
coated rods subjected later to functional testing. Visual observa —
tion of f i n i s h e d , impregnated surfaces indicated better penetration
af the coating , and static pressure tests confirmed these observa-
tions. Specifically, when pressurized with hydraulic oil in the
bench test apparatus shown in Figure 20, the phenolic-impregnated

74
 ~~~~~~~~~~ ~~

Coated Test Piece

Hydraulic Fluid

Piston

Compressed Air

sure

FIGURE 20. PRESSURE-TESTING AP PARA Ti~JS (9)

75

- - -
 __

— ~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~

~~~~~~~~~~~~~~~~~~~~~~~~

shafts permitted infiltration of oil through the coating at pres-

sures as low as 20 psi. On the other hand , polyester-resin im-
pregnated shafts did not leak when pressurized in this apparatus
to 100 psi. In later tests , all coated shafts were shown to with-
stand 2000 psi pressure when they were assembled into the hydraulic
wear-test apparatus and allowed to stand under pressure overnight.

Representative coated shafts were subsequently subjected

to even greater pressures. The bench—testing apparatus was modi-
fied to determine the effectiveness of sealed coatings against air
infiltration . Randomly selected shafts representing each of the
coating materials were assembled in the apparatus , pressurized
with air to 300 psi , and held at pressure for five minutes. The
c o a t e d s u r f a c e p r o t u d i n g above t h e p r e s s u r i z e d c y l i n d e r w a s d o u s e d
with SNOOP leak detection li quid [Mil Spec MIL—L-25567C (ASG)
Type 1] and observed . No air leakage was observed in any of the
coated rods tested . These shafts were then assembled in a standard
hydraulic cylinder and pressurized to 3500 psi with the hydraulic
fluid used in the functional wear tests. This pressure was main-
tained for 15 minutes , durina which time no infiltration of fluid
through the sealed coatings was observed .

T h e r m a l s p r a y e d c o a t i n g s u s u a l l y c o n t a i n some i s o l a t e d
p o r e s n o t c o n n e c t e d to each other or to the surface. Closed pores
c a n n o t be f i l l e d by i m p r e g n a t i o n a n d may be o p e n e d b y finish grind-
ing or machining operations. For some applications , it may be
desirable to treat spray-coated components with a sealer or filler
after machining. This was true for the hydraulic cylinder rods ,
and e p o x y r e s i n w o r k e d w e l l f o r t h e p u r ~~o s e . Epoxy r e s i n (Epon
828) w a s a p p l i e d to t h e s h a f t s a f t e r g r i n d i n g to f i n a l d i m e n s i o n s .
The p r o c e d u r e c o n s i s t e d of c o a t i n g t h e s u r f a c e , p l a c i n g t h e shaft
in a vacuum chamber , scrap ing the excess epoxy o f f w i t h a s h a f t
seal , and c u r i n g t h e r e s i n by r o t a t i n g t h e sh a f t in an oven a t
150 F for four hours . The presence of t h e f i l l e r i n s e c t i o n e d
pores provides some mechanical support to the coatinq and reduces
leakage along the surface. Some materials used for sealing and
filling pores or voids in plasma—sprayed coatinos are listed in
Table

6.2 Surface Finishing

The u n i que s t r u c t u r e of p l a s m a - s t r a y e d d e p o s i t s r e q u i r e s
that considerable care be taken in any machining or grinding
o p e r a t i o n s i n o r d e r to a v o i d d a m a g e to t h e c o a t i n u . Since a H

sprayed coating is composed of an aggregation of individual

particles , improper techniques during the finishing operation
could result in “pull—out ” of pa rti c l e s , singly or in clusters ,
thus producing a severely pitted surface. It is essential , there-
fore, that the sprayed particles be cleanly sheared and not pulled
from the surface. It is important to note that even an ideally
finished surface will probably not be shiny , but may have a matte
f i n i s h d u e to p o r o s i t y .

76

I
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‘0 ‘0 ‘0 ‘0 ‘0 ‘0 ‘0 ‘0
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77

-
-
~~~ -~~~~~~~~~~~~~~~~ -~ •~~~ --~~~~ —~~
r
_ _ _ _ _ _

~~~~~~~~~~~~~~~~

The selection of a finishing method depends on the type

of coating , its hardness , and its thickness. Consideration should
also be given to the properties (hardness , flexibility) of the sub-
strate material. Softer sprayed materials are often finished by
• machining, especially coatings applied to machine components. Such
applications usually involve plasma-sprayed refractory metals or
the softer cermets. A good finish can be obtained using high
speeds and carbide tools for most such applications. More often ,
howev er , plasma-sprayed coatings are finished by grinding.

The ph y s i c a l c h a r a c t e r i s t i c s of the c o a t i n g and t h e sub-

strate influence the selection of grindina equi pment and techniques.
When done properly, much less stress is impose i on the coating ,
substrate , and interface in grinding than in a machining operation.
Factors to be addressed in finishing by grinding include the type
of wheel to be used , as to abrasive medium , e.g., diamond or
silicon carbide , abrasive—grit size , wheel hardness and bonding
medium; and whether to dry-grind or wet-grind. Some general guide-
lines regarding these factors grovide a starting point , but optimum
m a t e r i a l r e m o v a l p a r a m e t e r s depend on the material being finished
and i t s intended use.

Generally, wet-grinding is recommended over (iry-grinding,

p r o v i d e d the proper wheel
is used. Sprayed materials , having a
different structure than the same materials in solid form , cannot
be ground with the same wheels , feeds , ~needs , etc. , recommended
for solid materials. Sprayed metals , in particular , are difficult
to grind because they tend to adhere to and “load” a grindin q
wheel. Consequently , wheels with coarse grain and tow bond
strength are used to grind metals to prevent loadin ci the wheels.

Guidelines set forth by the American W elding Society (AWS)

are help ful in determining a starting point for wheel selection. (10)
According to the AWS , if hi gh precision is not required , a 150—300
m i c r o i n c h p l a s m a— s p r a y e d s u r f a c e m a y e a s i l y be i m p r o v e d to 7 5 - 1 2 0
microinch using a soft rubber bonded 80-cirit silicon carbide abra-
sive or a vitrified bonded (H—L hardness) silicon carbide stick (80-
300 g r i t) or d i a m o n d s t i c k ( 8 0 — 3 0 0 g r i t) - D r y erindin q at speeds
slow enoug h to avoid overheatinq is considered approoriate.
For smoother finishes , the AWS states that the best
diamond grinding results have been obtained with resinoid-bonded
diamond wheels of 50—100 percent concentration , “L” or “ N ” hard-
n ess , with diamond grit sizes of 100 to 400 mesh. Grit sizes
80— 120 are used for roughinu , 150 to 240 for semi—finishing and
320— 500 for high finish.

Wheels with grit sizes appropriate for the surface fin-

ishes desired should be used. Results expected from diamond con-
cen trations of lOU are:

78

~~~~~~~~~~~~~~~~
~ -
- - ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

Gr ’t Size , S u r f a c e Rou gh ne ss ,
mesh microinch (AA )
100 24— 36
220 12—18
400 6—12

Flood cooling with a water—base fluid containing a rust inhibitor

is recommend ed. (10) Wheel speeds in the range from 1000 to 6000
feet/minute are considered satisfactory; a harder wheel is prefer-
able for lower speeds. Cross feeds of 0.04 to 0.08 in. and infeeds
of 0.0001 to 0.0005 in. are often used .

S m o o t h e r finishes than those just mentioned can be ob-

tained by lapping. The achievable surface roughness varies dir-
ectly with the size of the lapp ing particles; e.g ., lapping with
1-5 microinch diamofld grit is expected to produce a surface
roughness of 3 microinch (AA ) -

The coated and sealed rods, described in Paragraph 6.1 ,

required a very smooth surface finish for testing in hydraulic
piston wear tests. ( 9 ) In finishing the rods , the surface char-
acteristics of conventional steel cylinder rods supp lied by the
cylinder manufacturer were taken as the standard to be attained .
These standard cylinder rods were specified as having a finished
diameter of 1.000 +0.000 — 0.001 inch with a 5-10 microinch (AA ) sur-
face . “Talysurf ” surface roughness measurements indicated that an
even better surface finish of 2-3 microinch (AA ) could be attained .

To finish the coated rods , they were rc’:ated on centers

and ground using a combination of silicon carbide and diamond
grinding wheels. Particular attention to technique was required
in the case of the Al~ O - ~—TiO~ composite and Cr 2 O~ coatings, as the
nature of these ceramic materials is such that individual part icles
within the coating will tend to fracture , or pull out during grind-
ing, making it difficult to obtain a s m o o t h , d e f e c t — f r e e s u r f a c e .
S i m i l a r difficulties were posed by the molybdenum coatings. Of
the four coating materials evaluated , only the 8ONi—2O Cr coatinQ
y i e l d e d a s u r f a c e finish comparable to the conventional steel
cylinder rods.

In grinding the coatings , a No. 120 grit diamond grinding

wheel was used for rough grinding and gross stock removal. Finish
grinding was accomplished with a No. 180 grit silicon carbide
wheel. During finish grinding stock removal proceeded at a rate
of 0,0005 in./pass. The coating thicknesses of 0.022 and 0 .030
inch , as sprayed , on different rods were reduced to 0.015 inch
by grinding .

79

I
 - -~~~~~~~ -~~~~~-—---- - ~- -

80

. -~-~~~~~~~~ - -~~~• - -- —~~~~~ -— -

--- -
_ _ _
- - - --
 SECTION V II

7. HEALTH AND SAFETY

P lasma spray , l ike n umerous o th er i n d u s t r i a l processes

being used today , has its hazards , but those hazards can be elim-
inated or at least minimized , provided the proper safety precau-
tions a r e f ollowed . The poten ti al h a z a r d s to h e a l th a nd sa f e ty
of the operators and surrounding personnel can be grouped as
follows :
• Dust and Fumes
• Gases
• Arc R a d i a t i o n
• Noise
• E l e c t r i c a l Shock

These hazards are discussed individually in the following sections.

Information given here is intended to supplement and help identify
the need for the services of specialists in industrial hygiene and
safety .

7.1 DUST AND FUME S

In c o n t r a s t w i t h o t h e r t h e r m a l s p r a y ing and s u r f a c i n g
operations, the dust and fume s produced during plasma-arc spraying
originate primarily with the material being sprayed . Thus , poten-
tial dust and fumes hazards can be estimated by considering the
hazards associated with the coating material. The magnitude of
the hazard presented by dust and fumes depends on the composition
and concentrE ’tion of contaminant in the breathing zone . In cases
where control is not certain , air sampling should be accomplished
in the spray area to evaluate personnel exposure. The most common
method for air sampling is by use of lapel samplers , w h e r e the
operator carries a unit on his person and air is sampled continu-
o u s l y in the breathing zone . Analysis of samples permits calcu—
lation of the contaminant concentration in the operator ’ s
breathing air.

E x p o s u r e s determ ined by air sampling can be compared to

permissible exposure standards established for the contaminant(s)
in question. Some commonly used exposure standards and guidelines
are available as follows :

St a n da r d -
Source

Threshold Limit Values The Am erican Conference of

(TLV ’ s ) Gover n men tal Indus tri al Hyg ien-
i s t s (A C G I H ) , r e v i s e d a n n u a l l y ,
p u b l ished in p amphle t form .

81
 Standard Source

OSHA S t a n d a r d s The Occ upa tio n a l Saf et y a nd

H e a l t h A d m i n i s t r a t i o n, U.S.
D e p a r t m e n t of Labor , p u b l i s h e d
in Code of Federal R e g u l a t i o n s ,
T i t l e 29 , P a r t 1910 , S u b p a r t Z .

ANS I Standards The American National Standards

I n s t i t ute.

Hyg ienic Guide Series The Am erican Industrial Hygiene

Association.

Criteria Documents (Criteria The National Institute for Occu-

for proposed new OSHA pational Safety and Health , U.S.
Standards) Department of Health , Education ,
and Welfare.

Permissible exposure standards have been subject to frequent change

in recent years , as new information on toxic properties develops
rapidly. Care should be taken to see that the standards used are
up to date .

7.1.1 Ventilation

The p r i n c i pal control measure for airborne contaminants

is local ventilation . Existing guidelines for ventilation ade-
quacy are incomplete and their validity ir not well docu~ mented .
Exposure should be monitored by lapel samplers in cases where
contro l adequacy is in d o u b t .

A n e x h a u s t hood is c o n s i d e red nece ssary in a l l cases f o r

plasma—arc spray ing , general room ventilation being considered
i n a d e q u a t e . For t h e most innocuous spray materials (nuisance par-
t i c u l a t e s —- see the TLV pam ph l e t r e f e rred to a bove ), a f r e e l y
suspended hood of t h e t y pe commo n ly us ed f o r weld ing (a ttache d to
flexible hose ) may be adequate if spraying is carried out right
at the face of the hood and a face velocity (capture velocity) of
2 00 f e e t per - m inute is maintained . The spray velocity must be
d i r e c t e d i n t o the hoo d .

82

I
 - - - - - - — -----—-----—--—- — -— --• - -- •
-~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~ ~ ~~~~~~~~~~ • • ~~~~~~

For toxic * ma te ria ls a tota l l y e n c l o s ing hood is spec i f ied ,

with 200 feet per minute face velocity . The hood is to enclose
t h e e n t i r e operation , the opera tor rema ini n g in an upwind position .
It is stated further ** that an approved supplied—air respiratory
p r o t e c t i o n s h o u l d be provided when toxic materials aie used .

Ventilation design should not overlook adequate make—up

to replace air exhausted. Care must be taken to ensure that ex-
hausted air is suitably cleaned and/or exhausted at an appropri-
ate location and in such a manner that problems will not be created
and exhaust air will not be drawn into an air intake .

7.1.2 Resp iratory Protection

Respirators are occasionally recommended as a control

measure , but are in general much inferior to good ventilation
control. Where respirators are used , good work practice standards
must be followed to avoid losing the protection afforded by the
respirators. Chief among standards is the OSHA Respiratory Pro-
tection standard 1910.134 , which is supplemented by American
National Standard Practices for Respitatory Protection Z88.2. A
few pivotal requirements of these standards are:

• Approved *** respirators are to be used .

• Respirators are to he selected on the basis of
hazards to which the worker is exposed (even a
respirator approved for a given material will
be u n a c c e p t a b l e if the concentration of air
contaminant is too hi gh)
• Users are to be instructed and trained in proper
use and limitations of the respirators.
• Resp irators are to be properly cleaned , stored ,
maintained , and inspected on a routine basis.
• Appropriate continuing surveillance of the
respirator usage is to be maintained by respon-
sible qualified persons.

* Precisely what materials belong in this category has not been

defined clearly, but it has been suggested that all materials
with exposure limits lower than 10 milligrams per cubic meter
or 100 parts per million be included . At the present time C
cadmium , cobalt , lead , copper , z i n c , chromium , a nd n i c k e l would
be included in addition to highly toxic materials like beryllium.
** Industrial Venti lation A Manual of Recommended Practice , 13th
Edition , Print No. VS 415 , American Conference of Governmental
Industrial Hygienists.
~~~ Approval is by the National Institute for Occupational S af e t y
and H e a l t h (N I O S H ) ; Bureau of Mines approvals are b e ’~g phased
out.

03

I
 7.2 GASES

The p l a s m a - a r c s p r a y ing env ir o n m e n t is also cha rac ter ized

by the presence o f va ri ous gas es , som e of wh ich may presen t a
h a z a r d to t h e h e a l t h of e q u i p m e n t o p e r a t o r s . In addition to the
gases used to f o r m th e p l a s ma and pro pe l t h e ma te r ial b ein g sp rayed
(argon , hel ium , nitrogen , hydrogen , etc.), the following gases may
be present:

(1) Nitrogen Oxides. Various oxides of nitrogen may be

produced during spraying by reactions between atmos-
pheric nitrogen and oxygen. Nitrogen dioxide (NO 2 )
is of most concern.

(2) Ozone. Ozone may be produced by the reaction of

atmospheric oxygen and ultraviolet radiation from
the plasma arc.

For example,
O t h e r g a s e s may be p r e s e n t u n d e r c e r t a i n c o n d i t i o n s .
phosgene and dichloroacetyl chloride can be produced by reactions
in the presence of ultraviolet radiation of the chlorinated hydro-
carbons (e.g., trichloroethylene) used for degreasing metal sur-
faces. Such reactions may occur if spraying is done near a
degreasing facility or in an area where vapors from the degreasing
facility can be carried by natural or artificial air currents.
Both of these gases are classified as pulmonary irritants; also ,
in addition to being extremely toxic, phosgene can cause derma-
titis upon contact with the skin. The toxicity of dichloroacetyl
chloride is not well defined and the threshold limit value has not
yet been established for this gas.

As in the case of fumes , the hazards presented by gases

are a function of the type of gas and its concentration in the
breathing zone. The gases Used for plasma—arc spraying are not
toxic; however , a deficiency of oxygen can occur if they are leaked
into a confined area and the plasma gases displace oxygen in the
atmosphere . Hydrogen is , of course , a highly flammable gas and
must be handled accordingly. Nitrogen dioxide and ozone are very
toxic , and problems can be created if these gases are present. Gas
contaminant concentrations are expressed in part of gas per million
parts of air (ppm) ; the threshold limit values (TLV ’ s) f o r ozone
and nitrogen dioxide are 0.1 and 5 ppm , respectively. The nitrogen
d iox ide TL V i s a ceil i ng v a l u e wh i ch s h o u l d n o t b e exce ed ed even
f o r a por ti on of the work ing day .

Few problems with gases should be experienced if ventila-

tion is adequate in accordance with the guidelines discussed pre-
v io u s l y u n d e r Dust and Fumes . Sp r a y i ng f a c i l iti es sh o u l d no t be
l o c a t e d n e a r those used f o r d e g r e a s i n g or o t h e r o p e r a t i o n s u s i n g
c h l o r in ated s o l v e n ts.

84

_ _ _ _ _ _ _ _ _ _ _
J
7.3 ARC RADIATION

Ul trav iol et , visible , an d in f r a r e d rad ia ti on are produced

by plasma-arc spraying operations. As shown below , the spectrum
of the plasma arc can be divided according to wavelength:

Type of Radiation Wavelen gth , nm *

Extreme ultraviolet 4-200
Ultraviolet 200—400
Visible 400—750
Infrared 750—1300
Far infrared 1300—greater

Of course, the boundaries of these regions are not as well defined

as this table indicates. From the health and safety standpoint ,
radiation with wavelengths of 200 to 1300 nm is of most concern .
Also of concern is the radiation intensity , a parameter whose mag-
nitude is a function of (1) the spraying process , (2) the plasma
and propellant gases , (3) the substrate , (4) the operating vari-
ables , and (5) the distance from the plasma arc.

The problems associated with each type of radiation are

reviewed in the following sections.

7.3.1 Ultraviolet Radiation

The radiation of ultraviolet energy by the plasma arc can

have both a direct and an indirect effect on the health and safety
of equipment operators. Directly, exposure to ultraviolet can
cause temporary or permanent damage to the eyes , and it can affect
the sk in i n the same m ann e r as s o l a r rad ia tio n . U l t r a v io l e t is the
portion of sunlight believed responsible for excess skin cancer
among outdoor workers . Indirectly, toxic gases can be produced by
reactions between ultraviolet radiation and atmospheric oxygen ,
nitrogen , o r c h lor in ated hy dro ca rbon s . Sin c e such r e a c t ions h ave
already been reviewed , this discussion is concerned with the
direct effects of ultraviolet radiation .

As noted previously, ultraviolet radiation can produce

temporary or permanent eye damage . However , the mo st common ey e
ailment experienced by equipment operators is “arc-flash” or “arc—
eye ” . Both of these terms are misnorners for conjunctivitis , an
inflammation of the transparent membrane that covers the inner
surface of the eyelids and the white of the eye . This is a tern-
porary condition from which recovery is complete unless re-exposure
occurs. Conjunctivitis can be prevented by the use of proper fil-
ter lenses. It is recommended that at least a shade 12 should be
used for any close viewing of the plasma . Eye protection should
a l s o b e f u rn ish ed to nea rby w o r k e r s who may be exposed to arc
radiation .

* Wavelength is measured in nanometers (nm) or 0.000 ,000 ,001 meter.

85
 —

Ultraviolet radiation can also produce a skin burn that

is similar to sunburn and just as painful. Such burns can occur
on unprotected parts of the body that are exposed to arc radiation
d u r i n g spray ing . They can be prevented by wearing protective gar-
ments. Heavy work clothing is advisable for all but the mildest
exposure , a nd a l u m in i zed m a ter ial sh o u l d be use d f o r h eavy ex po s u r e .

It should be noted that eye damage and skin burns can

also be caused by ultraviolet radiation that is reflected by walls
and ceiling of spraying enclosures. Such surfaces can be coated
with paints that absorb rather than reflect radiation .

7.3.2 Visible Radiation

There is little evidence that visible radiation consti-

tutes a serious hazard in plasma-arc spraying. However , glare can
produce ey e d iscom f o rt , fati gue , and headache. The use of the cor-
rect filter lenses provides adequate protection against visible
radiation.

7.3.3 Infrared Radiation

Most of the radiation from the plasma ~ rc lies in the

infrared region. Excessive exposure to this type of radiatior can
produce retinal burns and cataracts , which can be prevented by the
use of filter lenses that absorb infrared radiation .

Infrared radiation also produces a sense of heat on the

skin. Heat produces physiological as well as psychological effects
on equipment operators; the physiological effects are most impor-
tant from the health and safety standpoint. Excessive heat can
produce d i s com f o r t , sweating, fatigue , and headache; in addition ,
performance is impaired . The psychological effects of heat are
more d i f f icul t to m eas ur e . However , there is little doubt that
efficiency is decreased.

The use of adequate protective clothing and standard types

of eye protection for ultraviolet will also serve to min imize ex-
posure to infrared radiation .

7 .4 NOISE

The noise associated with p lasma-arc operations may pre-

sent a hazard because of its intensity and frequency . Noise levels
in excess of 90 dB (A ) have been measured near p l asm a arcs . A l s o ,
t h e n o i s e produced by such arcs is distributed over a wide fre-
quency range , including the high frequet-icy range to which the ear
is more sensitive . The effect of noise on hearing is a function
of the sound intensity , pitch or frequency, and duration.

86
/
AD—A044 618 BATTELLE COLUMBUS LABS 04110 F/s 13/a
A PLASMA FLAME SPRAY HANDBOOK. tU)
MAR 77 T .1 ROSEBERRY. F W BOULGER NOO197 73 C leO3O
~
UNCLASSIFIED NAVSEA—MT—0143 NL

u
 Threshold limit noise-exposure val
Table XXIV . In Table XXIV , the sound lev e l
for decibels weighted according to a standa
dc-emphasizes low-f requency and very-high-f
are less important either because they are
ear (low frequencies) or less important in
high frequencies) . A-weighting is incorpor
sound level meters.

85
TABLE XX IV . THRESHOLD LIMIT VAL

Sound Leve l , Duratic

dB(A ) ho
80 1

90
95
100
105 1
110 1
115 1
No exposure to continuous or irt
in excess of 115 dB(A)

S The noise control eouipm ent that i

recommended by the equitnent supplier shoul
posures threaten to exceed the TLV ’ s, and t
be supplemented by ear muffs or ear plugs.
to sound levels approaching or exceeding th
initial and periodic hearing tests to help
lems and sensitive individuals.

7.5 ELECTRICAL SHOCK

Electrical shock hazards from plas

ment are similar to those presented by many
trical equipment. Only well-designed and w
should be used , and it must be properly ins
The open—circuit , operating, and supply cir
high enough to present a serious hazard .

Operators of the equi pment are pro

two control measures :

r
87
7.5.1 Grounding

To protec t aga inst the possib i lity of eq uip men t cabinets ,

housings , etc. being accidentally energ ized by short circuits ,
all such exposed metal parts should be connected together and to
electrical ground . The groundin g conductors used should be as
prescribed by the National Electr ical Code . The Code usually
requ ires that the grou n d in g path be carr i ed b ack to a p anel where
the circuit originates. Operators should be alert to the impor-
tance of main tainin g the gr oundin g sys tem and repor t in g imm edi at ely
any suspec ted damage to co ndui t or other gro unding conduc to r .

7.5 .2 Insula tion and Guard~~~

Cables , elec trodes , and other circuit parts which carry

a hazardous vol tage must be insulated or guarded to prevent opera-
tor conta c t . When ins talled accordi ng to the Na tional E lec trical
Code , all l ive p ar t s or equ ipmen t opera t ing a t 50 vol t s or more
will be guarded against accidental contact by persons or conduc-
ti ve objec t s. O pera tors sho u ld be a le rt to see tha t all gua rds ,
access panels, etc. are maintained in proper position . Insulated
parts should be inspected before each use and withdrawn from ser-
v ice if damaged .

Maintenance , repai rs , or modifications of equipment should

be done only by qual ified persons. Additional guidance with res-
pect to electrical hazards can be found in American National Stan-
dard Z49 .l-1973 , Safety in %~elding and Cutting , and in the American
Welding Society pamphlet , “Recommended Safe Practices for Plasma
Arc Cutting ” .

7.6 OSHA STANDARDS

The following OSHA Standards for general industry apply

to plasma-arc spraying and related activities , either as legally
binding regulations or as guidance in good health and safety
practice. OSHA General Industry Standards can ue found in the

8
U .S. Code of Federal Regula ti ons , Title 29, Chapter XVII , Part 1910.
Standard Title and/or Subject Covered
1910.95 Noise
1910.96 Radiation (Ionizing)
1910.101 Compressed Gases
1910.103 Hydrogen
1910.106 Flammable Liquids
1910.132 Personal Protective Equi pment
1910.133 Eye Protection
Standard Title and/or Subject Covered
1910.134 Respiratory Protection
1910.166 Compressed Gas Cylinders
1910 .242 Hand an d Por table Powered Tools
1910.252 Welding, Cutting, and Brazing
1910.308 Electrical
1910.309 National Electrical Code
1910.1000 A ir Contaminants

89
r ~~~~~~

90

_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _
_
_
_ _ _ _ _ _
-A
_
r

SECTION VIII

8. QUALITY ASSURANCE PROCEDURES

8.1 QUALIFICATION PROCEDURES

The success of plasma-arc coated components depends on the

skill of the operator , the condi t ion of the equipment , and the
selection of appropriate process variables. Therefore , it is logi-
cal that qualification tests be part of the quality assurance pro-
cedures for organizations required to produce components for severe
service. Although there seem to be no generally accepted indus-
tr ial standards for the purpose , the ma jor purchasers of plasma-
sorayed components for aircraft engines require potential suppliers
to demonstrate their capabilities before being approved as vendors.
The qualif ica tion procedures are in tended to establish that the
vendor has operators , equipment , and processes capable of thermal-
spray ing accep table coatings , of specif ic types , on appropr iate
substr ates. Somewhat sim i lar qualif ication procedures may be of
interes t , or poss ible usefulness , in Navy fac ilities.
So far as plasma-spray system operators are concerned ,
qualifica t ion p rocedures should be intended to demonstrate sk i ll
and knowledge , the ability to follow process instruc tions , and to
produce acceptable products. As in the widely used welding quali-
fication procedures , a combination of the following exercises would
seem to be appropriate.

• The operator should take and pass a short written test

covering questions pertinent to cleaning , surface pre-
pa ration and m asking procedures , and the general prin-
ciples of the plasma-spray ing equipmen t and procedures.

• The operator should demonstrate familiarity with appro-

priate equipment by connecting, setting up, and oper-
ating plasma-arc spraying equipment according to the
man uals supplied by the manufacturers.

• The operator should demonstrate capability by deposi t-

ing an acceptable coat in g to a spec i fied thickness on
an appropriate test specimen. The quality of the test
coating should be jud ged by suitable methods -- some
are described later in this section , such as bond
strength .

The qualif ication of equipment for plasma-arc spraying

requ ir ed by purchaser s of critical components is usually d i rected
toward two quali ty-contro l objectives. First, using a qualif ied
operator , the equipmen t must be shown to be capable of depositing
coatings meeting the acceptance quality agreed upon by the vendor

91
and purchaser. Secondly, all of the meteri ng and control devices
governing deposition variables must be shown to be properly cali-
bra ted and checked at regular intervals such as at least every
30 days.

The purchaser of high quality plasma-arc coated parts

usually requires that the deposition process proposed for produc-
tion be qualified by experiments. In the qualification tests , the
coa t ings of in terest are deposi ted on test st rips represen ti ng the
ma terial and surface charac teris ti cs of those to be used in the
sho p . The coa tings are deposited to spec i f ied thicknesses by
qua lif ied opera tors us ing wr i t ten process shee ts and qualified
equipment. Then the coatings are evaluated by test methods mutu-
ally agreed upon .

8.2 POWDER CHARACTERIZATION

Suppliers of sho t , grit , and powders of int eres t for

thermal spraying or substrate preparation ordinarily provide the
chem ical analys is and information on the particle size of the
m aterials they offer for sale. When chemical compositions are to
be checked , standard analytical methods are employed . Most metal
samples are analyzed by optical emission spectroscopy or wet tech-
niques. Gas contents of metal powders , coatings , or substrates
are de te rm ined by vacuum fus ion. Other mate rials are usually
analyzed by wet methods.

The particle sizes of powders can be determined by a vari-

ety of proce dur es and descr ibed by di f f e r e nt des i gna t ions . Fo r
particle sizes larger than 325 mesh (45 pm) , the range is charac-
te rized b y the m inim um and maximum cumula ti ve perce nt ages , by
weight , tha t w i
ll pass thro ugh or be re tained by scree ns (s ieves )
wi th different designation . That system is used for most particu-
late materials of interest in plasma spraying . Table XXV gives
the designations and openings of wire-cloth sieves used for test-
ing or classifying materials according to particle size. The
sieves to be u sed for that p urpose and the metho d s for conduct in g
the tests are described in ASTM Specifications Ell-70 and B214—66 ,
res pec tively. (25 ,26)

In genera l the ap p a ratus used for si eve anal yses cons ists
of a se t of s tandard s ieves assem bled in sui tab le order by nesting,
a mechani cal shaker , and an analytic al balance for we igh ing the
or igin al samp le and the sam p le of powder reta i ned on a particular
sieve . The balance should be able to weigh a 100-gram (0.2205 ib)
sample to a sensitivity of 0.01 gram (0.002205 lb) . The recommended
sample weigh ts for sieve analyses are 100 grams (0.2205 lb) and
50 grams (0.1102 lb) for materials having apparent densities , res-
pectively, above or below 1.5 grams/cm 3 (93.64 lb/ft 3 ).

.
92

~~~~~~~~~~~~~~~~~~~~~ . . . . . .
 TABLE XXV . NOMINAL DIMENSIONS FOR STANDARD TEST SIEVES
(U .S.A. Standard Series) (25)

Nonstandard
U .S . Standard Nominal Tyler Sieves and
and ISO (a) Opening , Designation ,
ASTM Sieve Designation inch um (b)
No. 8 2.36 mm 0.0937
No. 10 2.00 0.0787
No. 12 1.70 0.0661
No. 14 1.40 0.0555
No. 16 1.18 0.0469
No. 18 1.00 0.0394
No. 20 850 pm 0.0331
No. 25 71 0 0 .0278
No. 30 600 0.0234
No. 35 500 0.0197
No. 40 425 0.0165
No. 45 355 0.0139
No. 50 300 0. 0117
No. 60 250 0.0098
No. 70 212 0.0083
No. 80 180 0.0070 175 (80 mesh)
No. 100 150 0.0059 149 (100 mesh)
No. 120 125 0.0049
No. 140 106 0.0041 104 (150 mesh)
No. 170 90 0.0035
No. 200 75 0.0029 74 (200 mesh)
No. 23G 63 0.0025
No. 2 70 53 0.0 021
No. 3 25 45 0 . 0 017 44 (325 mesh)
No. 400 38 0.0015

(a) ISO (International Standards Organization) designations in

mill ionths of a meter .
(b) pm = millionth of a meter = 0.000040 inch.

Data obta ined from a sieve analysis of a powder should

identify the specific weight fractions passing a particular size
opening and retained on screens with smaller openings. (2 6) The
classification should be in size steps small enough to be useful
for characterizing the mate rial. It is customary to use successive
sieves covering the size range of interest , or every second sieve .
For instance , the sieve analysis of a powder for plasma spray ing
might be recorded in the following form (exemplary , not actual data ).

93

11
 Wei ght , percen t
Ma terial A Material B
Retained Passing Cumu- Cumu
on Sieve Sieve _ _ _ _ _ _
lative _ _ _ _ _ _
la t ive
30 0 0
35 30 3 3 21 21
40 35 7 10 21 42
45 40 11 21 21 63
50 45 16 37 16 79
60 50 21 58 11 90
70 60 21 79 7 97
80 70 21 100 3 100
80

For the assumed di stribut ions indicated , the median p a rti cle si ze
is smaller for m aterial A and the pro p ort ions of particles larger
than sieve size No. 50 are 37 percent for Material A and 79 per-
cen t for Mater ial B . The example indicates that char ac ter i z ing a
powder as being -30 + 80 mesh is a rather gross description . It
may mea n compa ra tively lit tle for con trol purposes unless the
ma ter ial in question is known to have been produced by the same
supplier by consistent procedure s and to have performed satisfac-
torily in previous plasma-spraying applications.

Particle sizes smaller than 325 mesh (0.0017 in.) are

used when very smooth finishes must be produced by plasma-arc
spraying . When it is necessary to determine their size and size
dis tribu t ion , the elutriation methods described in ASTM Specif I-
cation B293-60 are applicable. (27 ) Those metho d s , based on the
velocity of particles fall ing in a countercurrent of ai r or gas ,
are not stric tly accurate for porous or nonporous powders , but
give reproducible results even on thos e types of particles. The
method is appropriate for particles ranging in size from -5 to
over 40 pm (—0 .0002/+0 .0016 inch) .

For scien tific investigations , par ticle size distr ibutions

and informat ion on par t icle sha p e ca n be ob ta in ed by two more
elaborate procedures. The equipment used is known as the Coulter
Counter and the MSA (M ine Safe ty Ap p l ia nce ) appara tus. The Coulter
Counter measures the change in electrical resis tivi ty across an
orifice as par ticles , suspended in an electrolyte , are passed
through the orifice. This change in resistivity is related to the
volume of the particle passing through the orifice . This instru-
ment has an effec tive range of 1.0 to 500 microns. The MSA is a
centrifugal-sedimentation type equipment. It makes use of cen tri-
fugal force in speeding the settling time of very fine par ticles
and extends the practical range of sedimen tation techniques to
the submicron ran ge. The M SA has an effective particle size range
of 0.1 to 80 microns.

94

_ _
 Par ticle shape can be obtained by use of microscopic
techniques. A minimum of 500 particles should be measured. The
d iameter max imum an d diame ter minimum ratio is obt ai ned and , usi ng
the techniques describe d by Irani and Coll i s , the shape can be
calcula ted. (2 8)
For prac ti cal purposes , the “ true ” density of mos t powder
part icles can be measured by dividing the weight of a sample by
the amoun t of water i t displaces. (29) If the powder is represen-
ta tive of the material in the coating a f t e r spray ing, the densi ty
de term inat ion is useful in compu t ing the porosity of the sprayed
coating by some techn iques. The density measurement of powders
requires an analytical balance and a clean 50—ml graduate. The
procedure is as follows :

1. Fill the graduate approximately half full of water. Use a

funnel to avo id we tti ng the inside wall of the g rad uate
above the water level. Reco rd the volume of wa ter in the
graduate.

2. Weigh a sample of dry powder , either new or sprayed mate-

rial , and record the we ig h t .

3. Drop the powder sam p le i n the wa ter and recor d the wa ter
volume af ter the s ample se tt les , reading at the bottom of
the m eniscus.

4. Divide the weight of the powder sample by the apparent in-

crease in water volum e to obtain the density; e.g.,
4 5 . 1 g/ lO m l = 4 . 5 1 = dens ity .

Useful information on flow rates and apparent densities

of powders can be obtained with the Hall Flow Funnel. These data
gi ve informatio n as to the ease of handling of the powder dur i ng
p rocess ing , and the density to expect when powder is placed in
the powder feeding device .

Precise information about the true density of powders ca n

be obtained with the Micromeritics Helium-Air Pycnometer Model 1302.

8.3 MECHANICAL PROPERTIES

8.3.1 Bond Strength

The strength of the bond between a plasma-sprayed coating

and the substrate is of vital importance for most applications.
Conseque nt ly , tensile testing i s the most commonly used me thod for
evalua ting the mechan ical properties of coatings. Approved pro-
cedures for d et erm inin g bond i ng or adhesive st re ngth of a coat ing
to a subs t rate , and of the coa ting it self , are descr ibed in the
national standard designated as ASTM C633-69. (30) That method is
lim ited tc flame—sprayed coatings with thicknesses exceeding

95
 0.015 in. (0.38 mm ). The tests are usually conductLd at or near
room tempera ture because of the propert ies o f the adhesives appl ied
to the specimens. The method is recommended for qualification ,
qual ity control , and compone n t or process accep tance tes t in g. It
is also useful for comparing the adhesive or cohesive strengths of
differe nt coatings or diffe rent methods of sub stra~~ preparat i on .
Because of complicating f a c t o r s , however , the strength data a re
not suitable for desi gn purposes.

The standard bond-strength test consists of thermal-spray

coa ting one face of a substra te fix ture , bonding the coating to
the fla t face of a loadin g fixture w it h an ad he si ve , and then ap-
ply ing a tens i le loa d normal to the coa t in g. The A STM pu b l icat i on
sho uld be consulted , but m any of the recommenda tions follow in
s ummary fo rm .

The tension testing machi i1e used for determining bond and
coa ting s trengths should be cap able of dete rmining loads w ithin a
variation of 1 percent. It is desirable to increase the load at
a constant rate of cross head travel between 0.030 and 0.050 in./
mm (0.013 and 0.021 min/s). It is essential that the load be
applied perpendicular to the coating . If the self-aligning devices
on the testing machine do not prevent eccentric loading and bending
of the specimen , apparatus of the type shown in Figure 21 should be
used . That figure also shows a method of connecting the self-
ali gning fixture to a test specimen .

A test specimen consists of a substrate fixture , to which

the sprayed coating is applied , and a loading fixture. Both
fix tu res sho u ld be round soli d cyli nders n o t substa n ti ally shor ter
than their diameters. Figure 22 shows the dimensions of fixtures ,
for e ither load ing o r s ubs t r a te coa ting , considered suitable for
tensile testing . One end of each fixture should be capable of
attaching to the self-aligning shackles of the testing machine .
Both ends of each fi x ture sh a ll have faci ng s pa rallel to each
other and norma l to the loading axis. Facing diameters of 0.9 in.
(23 mm ) to 1.0 in. (25 mm) are appropriate and should be the same ,
w ithin 5 perc ent , for bo th f ix tures.

The subs tra te f ixture should be co n s truc ted of metal ,

preferably the s ame metal tha t w il l be used for the pro du c ti on
substra tes ,. If no t o therwi se spe ci f i e d , the fixture can be made
from 1018 or 1020 steel. After use , substrate rixtures can be
ground , given suitable surface preparation treatments , and reused .

Some organ izations use nonstandard tensile specimens

patterned after the ASTM confi guration for measuring bond strengths.
A convenient variation employs a test button or disk , 0.200 to
0.250 in. (5.08 to 6.35 mm) thick. The button is ordinarily
sim i lar i n comp osition and hardness to the p roduc tio n par t and

96
given the same surface preparation . Only one face is coated by
thermal spr ayin g . The tes t d i sk i s cemen ted to t he two lo ad i n g
fixtures by an adhes ive .

_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _
 PULL APPLIED
AT THIS END

_ _

—F H’H

4
HOL E
±

~~~~~~~~~~~~~~~~~~~~~
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_ASSEMBLY TEST SAMP L E
VI EW T U D . TO F I T
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LOADING F I X T U I E

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END TEST MACHINE FIXTUR E

M,fyk
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64 9 ~c 4 17 18 64

FIGURE 21. FIXTURE S FOR ALIGNING SPECIMENS FOR

BOND STRENGTH TENSILE TESTS (3O)

97
 _ .~~~. - - _
~~~~~~
.
_

TOLERANCE

F R A C T I O N S — ) ~4 T I.R. - .OO3 ~
MACHINED SURFA CES ./ S U G G E S T E D TH ’ D. S I Z E
__ (MIN.) Y2
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
— 2 O U N F - - 2 1 T H D~
U N F - 2 S TH ’ D.
(MA X.) 3/4— 1 6 U N E - 2 S THD.

A A

1.000 DIA
M USE BE S Q U A R E

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WITH C( N I UL I N E

S E CTION A —A

MATERIAL I DIA • 1~~LG — PER SPECIFICATION 24~ 1 0

( lifE1 in , Ifl ., Ill In Si fl

MeI ri~ ((0$ mm (I ( $ m m ( 2 I mm (2 mm I~ V mm

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~~mm ‘4mm ~

FIGURE 22. TEST SPECIMENS FOR ADHESION AND COHESION

STRENGTH TESTS ON THERMAL-SPRAYED COATINGS (30)

98

, . ,
.
. -. .
- ~~~~~~~ ~~~~~~~~~ - . - —
 - —-
~~

The ma terial used for adhesive bonding the coating to the

loading fixture must have a tensile strength at least as high as
the adhesive and cohesive strengths of the coating . The adhesive
bonding agent shall be sufficiently viscous not to penetrate
through the coating. Several commercial resins that cure and har-
den at room temperature are suitable. M~ong those known to have
given satisfaction are the following mate rials:

Conapoxy AD- l222 resin with Conacure EA-03 catalyst (Conap, Inc. ,
184 East Union Street , Allegheny , New York 1470 6)
Epon 911F (Shell Chemica l Co., Adhesives Department , P.O . Box 831 ,
Pittsburg, Cal i fornia 945 65 )

Bondmaster M 777 (Pittsburgh Plate Glass Co., Adhes ives Depar tmen t ,
225 Belleville Avenue , Bloomf ield , New Je rsey 07 00 3) .

Brochures provided by the manufac turers explain how to apply and

cure their adhesives. The strength of the adhesive bonding agent
shall be determ ined each time the bond or coating strength is
determined . This should be done by using the bonding agent to
at tach two loadin g fix tures and testin g, in order to detec t
deteriora tion or improper mixing of the adhesive. Depending on
the bonding agent , the strength is of the order of 4000 to 8000 psi.

The ASTM testing specification requires coating thick-

nesses over 0 .015 in. (0 .3 8 mm ) and uniform in thickness to wi thin
0.001 in. (0.025 mm ). Larger variations in thickness should be
corrected by machining or grinding before testing . The number of
specimens tested depends on the purpose to which the data will be
put . For acceptance tests , data from at least five specimens are
desirable.

The bonding strength or the cohesive strength of the coat-

ing is take n to be :
Strength = Maximum Load/Cross-Sectional Area

The strength value represents the weakest part of the system . If

the fa ilure occurs entirely at the coating-substrate , the value is
reported as adhesion strength. If the failure occurs entirely in
the coating , the strength is considered to be the cohesive strength
of the coating. The location of the failure is often determined
by a low-power microscope at a magnification up to b OX. Failure
in the adhesive bonding agent can be considered a satisfactory
resul t i f the strength value exceeds req u irements for quali ty
assurance or qualifica tion tests.

Ot her me thods of de term in i n g the tensile strengths of

thermal-spray coatings have been described in brochures .(29)

99

—s- - .
- - - ------ ~~~~
8.3.2 Shear Strength

Methods for jud ging the shear strength of p lasma-sprayed

coat in gs have been developed by sup p l i e rs of equ ipm en t and po w d e r s .
A test that is used quite frequently consists of coating a half—
inch band of a solid round cylinder and then applying axial pres-
sure to shea r the co a t i n g from the cy l i nd er . The s u p p l ie r ’ s
instructions on testing procedures follow . (29)

1. Make two sleeves to fit a 1-inch r o u n d specimen as i n d i c a t e d

in Figure 23. Drill and tap each sleeve to take one set
screw . The equipment avoids the necessity for machining or
grinding the coating .

2. Assemble the cylinder and sleeves and abrasive blast both

the bare area of the cylinder and the tapered ends of the
sleeves.

3. Remove the sleeves and remove any loose abrasive .

4. Reassemble the sleeves on the specimen , tighten the set

screws and preheat as for production spraying .

5. Apply the coating on the specimen and sleeve as shown in

Figure 23. Friable or porous coatings should be given a
top coat of stainless steel (Metco 420) or Ni-Cr alloy
(Metco 43C) to improve the distribution of the shear stress
over the test section.

6. Loosen both set screws and measure the shear strength , using
a laboratory machine capable of measuring the load accurately.

MOUND
SPE CIMEN -
SL EE VE
_ _ _ _ _ _ _ _ _ _

FIG RF. 23. ROUND SPECIMEN USED TO DETERMINE THE

SHEAR STRENGTH OF A SPRAYED COATING (29)

The te’~ description mentions that shrinkage stresses in the coat-

ings w i l l Iffect th t m easured shear shrength , ve ry l i k e l y to a
cons 1di r.~h l i i extent.

100

_ _ _ _ _ _ _
 - ~
8.3.3 H a r d n e s s Tests

Hardness values are often men tioned when comparing coat-

ings and effects of spray variables. It is usually a misuse of
hardness data to consider them as measures of coating strength.
The measurements may be of more value for quality contro l and
for evaluating process variables. Because most coatings are
thin, porous , and charac terized by relatively low cohesive
s t r e n g t h s, m a c r o h ar d n e s s t e s t s are not applicable. Although
m icrohardness data are mo re useful , they require careful deter-
mina tions and interpretations. Rockwell Superficial Hardness
tests ar e simp ler to conduct an d a re considered useful for quali ty
con trol and processing studies .

Spec ime n s fo r microhar dn ess test s should be pol i shed to

a metallographic-quality f ini sh because t h e d ime nsions of t h e
hardness impressions are measured with a microscope . The measur-
ing microscope shall be graduated in 0.5-pm (0.00002—in.) divi-
sions or smaller. The standard methods for de termining the micro-
hardness of materials are described in ASTM standard E384-73 . (31)
That publication gives the procedures for determining microhard-
ness numbe r s u sin g bo th K noop an d Vicker s (or Diamo n d Pyram id )
inden tors . I n both sys tem s , the hardness number is th3 pressure
exerted on the specimen by the diamond indentor used to produce
the impression. The indentors used for Knoop and Vickers deter-
minations are of different shapes and the pressures are calcu-
la ted for di ffe rent are as. On the K noop scale , the p r e s s u r e is
the load in kgf (2.2 lb-force) divided by the projected area of
the impr e s s ion i n mm 2 . The p ressu re or h ar d n ess numb er on the
Vi.ckers scale is calculated from the contact area of the indenta-
tion by assuming that it is the imprint of an undeformed indentor.
In p r i ncip l e , both systems of measur in g microhard n ess are less
affec ted by porosi ty than one based on meas u r i ng the indentor
trave l caused by a specific increase in load . Microhardness tests
are usually made transverse to the coating surface , even though
serv ice loads are usually norma l to the surface and hardness may
vary because of micros tructural anisotropy . It is often convenient
to make microh ardness measurements on specimens prepared for metal-
log raphi c stud ies of coa t in g an d subs t ra te m icrostruc tures and
coating porosity.

Procedures for Rockwell Sup erficial Hard n ess tests are

described in ASTM standard E-18-74. (32 ) They are far better
sui ted to evaluating sprayed coatings than standard Rockwell tests
because they employ smaller loads. The superficial hardness in-
strument measures the difference in the depths of indentation
caused by the minor load (3 kgf or 6.72 lb-force) applied first
and t h e m a j o r load w h i c h m ay be 15 , 30 , or 45 k g f. One un it on
the superficial hardness scale represents a penetrator movement of
0.001 mm (0.00004 in. ) between minor and major loads. Of the five
types of indentors used for Rockwell superficial hardness deter-
minations, the most commonly used are the diamond penetrator
(N scale) and the 1/16-inch (1.588 m m ) ball (T scale). In reporting

101
r
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

Rockwell hardness numbers , the penetra tor , load , and dial used
should always be indicated . For example , a value of “8 1 HR 3 0 N”
indicates a superficial hardnes s number of 81 on the 30 N (30 kg
load , diamond penetrator) scale. There is no reliable genera l
method of converting hardness numbers from one Rockwell scale tu
another , or to tensile strengths.
The choice of an appropriate scale to use for measuring
superficial hard n ess depends on the hardness and thickness of the
coating . Table XXVI provides some information for guiding such
jud gments. When the substrate has a hardness somewhat similar to
that of the coatin g, and the coating is th ick enough , h e a v i e r t e s t
loads give more reliable and consistent readings.

Several precautions should be taken in conducting super-

ficial hardness tests on plasma-sprayed coatings. The surface
should be clean and free of gross imperfections. The impressions
should be spaced at least three impression-diameters from each
other and from a free edge. A t least five de termina t ions are
u s u a l ly necessary to obtain rel iable results. A surface finish
of 30 microinch is recommended for using the 15 N scale ; slightly
rougher surface finishes are adequate for the other scales. Fla t
surfaces are preferable for hardness tests ; measuremen ts on curved
surfaces give erroneous values. The factors listed in Table XXVI I
should be used to correct hardness values determined on round
specimens. The correct ions vary with the curvature , type of pene-
trator , and the hardness value.

8.4 METALLOGRAPHIC EXAMINATIONS

Metallography is one of the prime tools u sed by mater ials

people to evaluate the quality of flame-sprayed coatings. Since
approval of a coating for a given application depends on the re-
s u l t s of m e t all o g r a p h ic study , it is impera tive that the specimen
studied be represen tati ve of the coating, and tha t i t b e properly
prepared .

The metalb ographic procedures are similar to those used

for prepar ing most wrought materials. However, specimens of flame-
sprayed LDa.tings require some special techniques. The structure
of the coa ti ngs i s nonhomogeneous , c~~ aisting of particles mechan i-
cally and metallurgically bonded to each other. The coatings con-
tain oxides and metallic phases not normally found in wrought
materials. Care must be taken in the 3ectioning and polishing to
avoid pull ing them out , thus avo idirg false evaluations. Proper
preparation is v ital to preserve the integrity of the microconsti-
tuents. Ultrasonic cleaning should be avoided , and vibratory
polishing used rarely.

102

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) (0 WZ WZ QJ Z 0) E-i 0) 0 ) E -~ .~~ .0 4-)~~
~ 0 C C C C C E-I C 4)C 100)
~~
H 0 IOC
‘0 Lf l ‘ 00 ‘0 L f l ‘0 U) ‘0 o ‘0 L n E. 0
I-i ’-I I I, - 4 C C )1 U .,.4
~~~m I-i~~~ ~~ ~~~~
0 (0 (0 (0 (0 (0 (’ ) (0 0) C) )~~ 4J
~~~~ - ~~~~ - ~~~~ - ~~~~ - ~~ ~~~~ - > 10
‘-4100 )
0 0
0” 0” I- i C
4)) ØJ
0” 4)) 0” WC
0”
0 ) 0”
C b” W U) Q
H 4J~~
.,.4 .$J~~
.,-4 .i~~•,-4 4J ’,-4 4) .,.4 4 .,.4 CW Q~’0
1 0’ 0 (0’ 0 (0 ’0 (0’0 (11 .4 C (0~ -4
E1 0 E(0 E1 0 E1 0 E(0 E(0 C) ’0
.,.4Ø) •Q ) •4Q ) ... •,. .,4 4)) I.i ’H I-i 0)0
~~~~~~ ~~~~
~~~ X~~ O . C (0 .C .C
0 0 0 0 0 0 ~~~4 ) .C E-I U)
)—i ,
-I I.-4 .-4 I—I .--4 I-I~~-4 I4 4 i.I ’-l
~ ~~~
0~ (0 0~~10 Qi0
1 0~~10 —
Q~•H ~~~ 4 Q -4
~ OeH Q~.,.4 Q~’H 10 .0
~~~~ 4c~ ~~~
-

103

_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ —. nn
 TABLE XXVII . CORRECTIONS TO BE ADDED TO ROCKWELL SUPERFICIAL
VALUES OBTAINED ON CYLINDRICAL SPECIMENS (a) OF
VARIOUS DIAMETERS (32)

Diameters of Cylindrical Specimens

Dial
1/8 in. 1/4 in. 3/8 in. 1/2 in. 3/4 in. 1 in.
Readin g
(3.2 mitt) (6.4 mm ) (10 mm) (13 mm ) (19 mm ) (25 mm)
Corrections to be Added to Rockwell Superficial
15 N , 30 N , and 45 N valu e s (b )
20 6.0 3.0 2.0 1.5 1.5 1.5
25 5.5 3.0 2.0 1.5 1.5 1.0
30 5.5 3.0 2.0 1.5 1.0 1.0
35 5.0 2.5 2.0 1.5 1.0 1.0
40 4.5 2.5 1.5 1.5 1.0 1.0
45 4.0 2.0 1.5 1.0 1.0 1.0
50 3.5 2.0 1.5 1.0 1.0 0.5
55 3.5 2.0 1.5 1.0 0.5 0.5
60 3.0 1.5 1.0 1.0 0.5 0.5
65 2.5 1.5 1.0 0.5 0.5 0.5
70 2.0 1.0 1.0 0.5 0.5 0.5
75 1.5 1.0 0.5 0.5 0.5 0
80 1.0 0.5 0.5 0.5 0 0
85 0.5 0.5 0.5 0.5 0 0
90 0 0 0 0 0 0

C o r r e c t i o n s to be Added to Rockwell S up e r f i c i a l
15 T , 30 T , and 45 T v a l ue s (b )
20 13.0 9.0 6.0 4.5 3.0 2.0
30 11.5 7.5 5.0 3.5 2.5 2.0
40 10.0 6.5 4.5 3.5 2.5 2.0
50 8.5 5.5 4.0 3.0 2.0 1.5
60 6.5 4.5 3.0 2.5 1.5 1.5
70 5.0 3.5 2.5 2.0 1.0 1.0
80 3.0 2.0 1.5 1.5 1.0 0.5
90 1.5 1.0 1.0 0.5 0.5 0.5

(a) When testi ng cylindrical spec imens , the accuracy of the test
will be .seriously affected by alignment of elevating screw ,
V-anvil , penetrators , surface fi n ish , and the str a i g h tness of
the cylinder.

(b) These corrections are approximate only and represent the

averages , to the nearest 0.5 Rockwell superficial number , of
numerous actual observations.

104

_ _ _ _ _ _ _ _ _ _ _ _

- .- .-
~~~~~~~~~~~~
. .- .-
~~~ -fl-- ~~ — - -.- -~~
 -.
~~ -

8.4.1 Sectioning and Mounting

After careful selection , samples can be sectioned on any

type of a metallurgical cut-off machine . Allison C-l20 SiC cut-
off wheels are satisfactory for most materials. A continuous—rim
diamond cut-off wheel, 0.040 inch , is used for sectioning coupons
with ceramic coating. Coolant , usually tap water or water and
cutting oil in a recirculating system , is used in all cutting
operations. To avoid chipping the unsupported coating , it is
sometimes advisable to mount the samples in epoxy resin before
s e c t i o n i n g.

Sampies may be mounted in Shell Epon Resin 815 , using

vacuum impregna tion procedures to fill the pores. This is a liquid
c a s t i n g p l a s t i c which is easy to h a n d l e , has good adherence , hard-
ness , and dimens ional stability. Thermosetting powders such as
Bakelite can be used , but mount size is limited , and Bakelite does
not fill the pores as well as Epon. Two specimens are mounted to-
gether , positioning the coatings front to back , in the case of very
hard specimens , or coating-to-coating , if the coating is soft or
medium hard . The coatings themselves ~ nd the substrate material
serve as backup to protect the coating .

8.4.2 Grinding

Samples are ground on a 10-inch disc grinder using 120-

gri t SiC grinding d iscs , to level the mount , usin g water as a
coolant. Wet gr inding continues on an 8-inch disc grinder , using
successively finer Si C disc s 18 0, 240 , 400 , and 600 grit. With
each grit the mount is turned 90 degrees and the sample is ground
until all scratches left by the preceding grit have been removed .
After each step the mount is thoroughly washed with running water.
Ultrasonic cleaning is never used for cleaning specimens of flame—
sprayed coatings. Diamond laps 240 , 400 , and 600 grit are used
instead of SiC discs to grind very hard ma terials such as ceramics.

8.4.3 Polishing

Preliminary polishing of soft metallic samples is done by

hand on a low-speed (100 to 300 rpm ) wheel using a medium-nap cloth
charged with 3-micron diamond paste. Kerosene or lapping oil is
used as a lubr icant and polishing proceeds until all grinding
scratches have been removed . Then the sample will be hand polished
using 1-micron diamond on a medium—nap cloth . If better flatness
and edge reten t ion are desired , vibra tory polishing can be used
with 1-1/2-micron diamond on a silk cloth . Tungsten carbide coat-
ings should not be polished on a vibratory polisher.

Diamond polish ing causes excessive porosity in ceramics ,

cerme ts , and carbides. Overpolishing of tungsten carbide and hard—
metal coatings on diamond create relief of the harder constituents

105

I
p .

and pull—out of any loosely bonded constituents. Therefore , an

alternative preliminary polishing technique is used for pol ishing
some semihard to very hard materials. Grind ing scratches are re-
moved on a fast wheel (1750 rpm ) covered with a low-nap cloth
(nylon , silk , or lintless) and a slurry of 20 0 cc water , 4 grams
chromium trioxide and 25 grams of “Linde A ” polishing abrasive .
If chromium trioxide preferentially attacks some phases , it can
be reduced or eliminated from the slurry .
Final polish is obtained on a low-speed (100 to 300 rpm)
wheel covered with a fine-nap cloth (Buehler microcloth or Gamal)
with a slurry of 200 cc water , 4 grams chromium tr ioxide , and 2 0
grams ferric oxide . As in the preliminary polishing , chromium
trioxide can be reduced or eliminated from the slurry to obtain
the most satisfactory results. For some materials , 0.05 Gamma
Alumina on a fine-nap cloth is used . Care should be taken not to
polish too long , so as to avoid excessive relief of carbide and
solid solution phases. When there are problems with galvanic at-
tack due to the difference of potentials between brass or copper
wheels , the subs tra te and the microconstituents in the coa ting ,
it can be el im in ated by plac ing Saran W rap be twee n the wheel and
the cloth.

8.4.4 Etching

Specimens are not etched before examining the coating for

porosity or oxide contents. When othe r attributes are being ex-
amined , the coa ting is etched . The comp o s i t ion of the coating
determines which etchin g technique is used : chemical , electro—
chemical , or vacuum cathodic etching .

Etchin g reveals the coating components by preferential

attack or by staining the various phases. It is sometimes neces-
sary to mask the substrate with tape before etching to eliminate
galvanic attack between substrate and coating . Chemical etching
is done by swabbing or by immersing the mount. Some coatings re-
quire electrolytic etching to reveal the structure . Some chemical
etchants found useful for plasma-sprayed coatings are listed in
Table XXV III.

Structures of some coatings are revealed by the proper

use of the chrom ium trioxide etch polish. Another method is to
heat tint the surface. The color of the oxides formed on the
polished surface relates to the composition of the carbide phases
present.

Cathodic vacuum etching enjoys several advantages as com-

pared with chemical etching techni ques. It produces a surface
free of stain and results in excellent relief delineation of the
phases , which is desirable for studies with the electron microscope .
Due to the time and expense , cathod ic etching is used only for
special evaluations.

106

I
 _ _ _ _ _ _

TABLE XXVIII . SOME ETCHANTS FOUND USEFUL FOR METALLOGRAPHIC

EXAMINATIONS OF PLASMA-SPRAYED COATINGS

Coating Major Constituent Etchants

Metco 450 Ni-4.5A1 50 cc lactic acid
Metco 404 Ni-20A1 10 cc HNO 3
Metco 405 Ni-Al 50 drops HF
Carapella ’ s Etchant
~
1
~~~ 5 g FeCl 3
2 c c HCl
98 cc ethyl alcohol
Swab or immerse
Metco 43 9 Tungsten c~ rbide Murakami ’s Reagent
Metco 438 WC + NiA1 10 g K 3 F e ( C N ~ )
Metco 72F WC-12 cobalt 10 g KOH
Metco 430 CrC + NiAl 100 cc H 2 O
Metco 501 Ni- 3OMo Mod i fied Murakami ’s
2.5 g NaOH
11.0 g K 3F e (CN ~~)
500 cc H 2 O
Swab or immerse
Metco 54 Aluminum silicon Keller ’s Reagent
95 cc H 2 O
2.5 cc HNO 3
1.5 cc HC1
1.0 cc HF
60 cc gl ycerin
20 cc HNO 3
3 cc HF
100 cc H 20
1 cc HF
50 cc HF
50 àc }jNO 3
50 cc H 2 0
Metco 43F N ickel-chromium 100 cc H 2 0
Metco 44 100 cc HC 1
Metco 4lC 20 g CuSO ,,
Metco 42C 90 cc HC1
Metco 43C 30 cc H 2 O 2
Metco 44C Swab or immerse
Metco 45C
10% oxalic acid
6v DC electrolytic
Metco 91 Carbon steel 96 cc ethyl alcohol
Metco Sprasreel 4 cc HNO 3
96 cc ethyl alcohol
4 g picric acid
Immerse

107

—. ——
 TABLE X X V I I I . SOME ETCHANTS FOUND USE FUL FOR METALLOG RAPHIC
EXAM INATIONS OF PLASMA-SPRAYED COATINGS (Cont inued )

Coating Major Constituent Etcha n ts

M etco 43 9 Tungste n carbide Murakami ’ s
Metco 438 -
KOH-5% electrolytic
Metco 7 2F

8 .4.5 Metallographic Evalua tion

In te r p r e t a t i o n of m i c r o s tr uc t u r e and c o r r e l ation of th a t
in forma tion w i th the overall propert ies of the sprayed coati ng i s
a p rob lem . In many pre l imi n a r y meta ll o g r a p h i c inves tig a tions ,
q u a l ita tive in forma tion is all t h a t is ne c e s s a r y .

On a p roduc tion basis , t h e best m e tho d f o r determ in ing

whe ther a sprayed coating is acceptable is to compare its appear-
ance wit h t h a t of a sta n d a r d ma t e r i a l k nown to pe r f o r m adeq uate l y
in service.

For final evaluation of flame-sprayed coatings , quantita-

tive information is almost always required. It is desirable to
de term ine perce nt ages of porosity , oxides , and other phases pres-
ent in the flame-sprayed coating. Grid area point-count method
and the Quantimet are the methods used for these determinations.
Mic r o h a rdness da ta ca n prov ide con s ide ra b l e in f o r mation about the
nature of a flame-sprayed coating . Difference in hardness is a
v a l u a b l e method f o r d is tin g u i s h i ng be tween and iden ti f y in g phases
of a flame-sprayed coating . The type of hardness testing , whe ther
Superf ic i a l Rockwell , V ickers , or Knoop, should be chosen according
to the application. Microprobe and/or X-ray diffraction can be
used to iden ti f y phases in flame-spr ayed coatings during the
resea rch developm ent stag e of coa t in g, but are not needed for pro-
duc t ion applica tions .

8.5 COATING POROSITY

M~ tallographic methods are widely used fo r judg i ng the

poros ity of plasma-sprayed coatings. The quantitative approaches
are based on the quantitative relationships between measurements
on the two-dimensional plane of polish and the magnitudes of the
m icrostructural features in three-dimensional materials. The ap-
plications and limitat ions of quanti ta ti ve m etallography have been
described in detail by Underwood .(3 3) The underly ing theories are
well establ i shed . The principal sources of errors in estimat ing
pore volumes are inadequately prepared metallographic specimens
and taking too small a number of measuremen ts. At the risk of
oversimplification , the technique s used to determine the volume of
voids , or discre te p hases , in a microstruc ture can be briefly
summarized .

108

I
— -I
~~~~~~~~~~~~~~~~~~~~~~~~ ~- — -— --. - - .--.- - - - .
. .- — -.- - —lu~~

The volume fraction occupied by a microstructural feature ,

such as a void or pore , is equal to the areal , linear , or point
ratio of the selected feature as seen on random sections through
the microstructure. Television-scanning equipment , such as the
Quan timetTM instrument, is used for applications where the number
of specimens examined makes automation justified . Linear ratios
are commonly measured in a semiautomated fashion utiliz ing a
Hurlbut Counter. The point-counting method is efficient and re-
quires very little special equipment. The test poin ts to be counted
are those fallin g within the images of the microstructural feature
(e.g., voids ) being measured . The number of those points counted
d ivided by t h e t o t a l n umber of a v a i l ab l e tes t p o i n t s gives the
volume fraction of the specimen occupied by voids. Ordinarily the
a r r a y of a v a i l a b l e test p o i n t s is provided by the i n t e r s e c t i ons of
a grid in serted in the eyep iece of a micro scope . Alternatively, a
clear plastic grid can be placed over micrographs and used for
point countin g . In either case , the gr id spacin g should be close
to the spacing of the microstructural feature of interest (e.g.,
pores). Grid points fall ing on the boundary of a pore should be
counted as one—half. Care must be taken in counting phases or voids
not to overlook any or to count some twice .

Because po in t c o u n t i n g is tedious and special instruments

for quanti tative metallograph y are ex pensive , some organizations
judge porosity by comparing the microstructures with standard
pho tom ic r o g r a p h s . Tha t me thod is simpler , q u i c k e r , and sui table
for control and acceptance purposes. One large purchaser of plasma-
sprayed componen ts provides its vendors with micrographs illustrat-
ing its requirements for densities of coatings and for contents of
oxides , inclusions , and unmelted particles. Depending on their
purpose , comparisons are based on m icrographs taken at magnifica-
tions rang ing from 50 to 500X.

Although the two metallographic approaches just mentioned

are recommended , some product ion sho ps use d irect methods f o r
measuring the porosity of plasma-sprayed coatings. The method
suggested by a supplier several years ago consists , in general , of
the follow ing steps (2 9)
1. Prepare a solid cylindrical bar approximately 5-in, long X
7/8-in, in diameter; measure and record the diameter to 0.001 in.

2. Using the surface preparation methods and pla sma-spray vari-

ables of interest and masks , apply a coating about 0.110-in.
thick to the bar for a length of about 2.5 in.

3. Using the center holes , mount the coated bar in a lathe.

Mach ine or grind the coated section to a thickness of 0.100 in.,
or 0.050 in. for self-fluxing coatings . Measure and record
the diameter to 0.001 inch.

109

p
~
- — ~~ - -

4. Cut specimens approxima tely 1.1-in, long f r o m the coated

and uncoated reg ions of the bar.
5. Grind both ends of both specimens flat and perpendicular
to the c e n t r a l ax is.

6. Weigh the specimens using an analytical balance to 0.001

grams (0.0000022 lb) and record the weight.

7. Calculate the volumes by the following equation:

Volume = length X (diameters)2 X (0.7854)

I f tha t cal cu la tion is made i n inches , divide the value

by 0.081025 to obtain the volume in cm 3 .

8. Determine the density of the coating :

Wt. of coated sample (g) - Wt. of uncoated sample (g)

V o l . of coated samp le (cm 3 ) Vol. of uncoated sample (cm 3)
-
—

Tha t “measured” density value can be divided by the “ true ” d e n s it y

of the coa ti ng m ater i al , de term ined as su gge s t e d by Sec tion 8. 2 ,
page 95 , or by anoth er method , to express the density as a fraction
of the “ true ” val ue.

The volume fractio n of porosity can be obtained from

“ measured” and “ true ” d e n s i t y v a l u e s in the f o l l o w ing f a s h i o n :

Void Volume Fr ac t ion = (“ true ” density - “measured” density)

(true density)

8.6 SHOT PEENING TESTS

The eff icacy of a shot peening operation depends on con-

troll ing the ope r ation of the blas ti ng ope ra t ions and on the ir
relationsh ips to the work being peened . The effects of the peen-
ing o p e r a t i o n can be m e a s u r e d , and t h u s c o n t r o l l e d by a d j u s t i n g
the b l a s t i n g v a r i a b l e s , by tests on flat test strips. The evalua-
tions are based on the fact that a thi n metal strip b las ted with
shot while olamped to a solid block will be curved after removal
from the fixture . The peened side of the curved strip will be
convex ; the degree of curvature is a measure of the residual stress
developed in the strip and the severity of peening. The properties
of the blast are the velocity , size , shape, densi ty and hardness of
the shot. The impingement angle , le ngth of t i m e of b l a s ting , and
sho t f l o w r a t e a r e a l s o impor tan t .

When peened substrates are to be plasma-arc sprayed , the

just-men tioned variables should be controlled to give the appro-
pria te peen ing intensi ty. The Soc i e ty of A ut omo t ive Engineers has

110
F
-. -- . . -. - - - -.
- . -- - --

~~~~~~ ~~~~~~~~~ ~~ ~~~~ ~~~~

adopted recommended prac t ices for measur i ng the e ffec t s of sho t

p e e n i n g tha t can be u sed f o r qu al it y cont r o l . (34 ,35) The peening
studies are made on SAE 10 70 cold rolled s teel t es t st r ips , un i-
formly harden ed to Rockwell C 44 to 50 and flat to 0 .OOl inch .

St a n d a rd s t r ip hol de r s and ga ges , of the types shown in

Figures 24 an d 25 , are used for the tests. During peening the
test s t r i p is mo u n t e d on t h e h o l d e r ; a f t e r p e e n i n g i t is placed
on t h e gage with the indicator stem bearing on the unpeened sur-
face. The curva t ure of the st r ip is determined by measuring the
height of the combined longitudinal and transverse arcs across
standar d cho rds . Tha t arc hei ght is obt ai n ed by meas urin g the
displacement of a central point on the unpeened surface , to one—
thousandth of an inch , from the four balls forming corners of a
particular rectangle.

As indicated in Table XX IX , one of three different thick-

nesses of test strips is used for the evaluations. Strip A is
recommended for peening test intensities that produce arc heights
ranging from 0.006 to 0.024 inch. The relationships among arc
heights for test stri ps A , C, and N after identical peening treat-
ments are indicated in Table XXIX. Peening intensities are desig-
na ted by th e a r c he ig h t i n in ches and the ty pe of tes t str ip
employed , ror example 0.004 A , 0,001 C , or 0.012 N.

TABLE X X I X . CORRE LATION OF ALMEN PEENING I N T E N S I T I E S AS

INDICATED BY ARC HEIGHTS OF STANDARD TEST
STRIPS PEENED UNDER IDENTICAL BLASTING AND
EXPOSURE CONDITIONS (34 )
Alinen Intensities for Test Stri ps Indicated , 0.001 inch (a)
A Stri p C Strip N Strip
2 — 6
4 — 12
6 1.8 18
8 2.4 24
10 3 .0 —

15 4.5 —

20 6.0 —

25 7.5 —

30 9.0 —

(a) Test Strip Dimensions , inch :

A 3.000 +0 .015 x 0.745 to 0.750 x 0.051 -0 .00l
N 3 .000 ‘0.015 x 0.745 to 0.750 x 0.031 ~ O .O0l
C 3.000 ‘0 .015 x 0.745 to 0.750 x 0.094 ÷0 .001

111
._
‘_‘_•~~~ -
.
-
~
-
~~

,— NOLOeR i— rEsT - ~imP

0.040

/
~
(SEcT IONW ) ~~~~~
HOLE CV4TERS

HOLE CENTERS

-l
X 4 HOLES

L
~~
FOUR NO 10 3200 NO $0 54 ROUND-HEAD
SCREWS W I TH HEX . NUTS

FIGURE 24. ASSEMBLED TEST STRIP AND HOLDER (34)

DIAL IM)ICA TOR . ,.IAA VA LU E

/ 0) 7 3

—
OF GRADUAT IO N 0 O0I 0 377
/ CO UNT EPC LO C ” WISE ~
, eA C K ADJUSTA BL E B AC IcE1 ,
I Os ~ FRI CYI O N J EW E L~~
ED
BEA R IG,S EOUIPPE0 W IT . , ~~~~~
~
‘-Il L.
1iuI
~-~
EXTENS ION POINT

i’
‘S
“
‘~ — .( —
~~~~ ,~ “
TJT CONTACT SURFACE
L4, J OF ALL BA LLS TO
____________ BE IN ONE PLANE
*0.002

~~~~UIN
J
g
______
~

f
t haAx -.j I-: 1 ..-
~ ~~~ UAX

~ 3O7S ~ -
Q4~~
0830

- P0vQ
4 I4A RDCNED STEE L~~~~~ 3

~~~~~~~~~~~

FIGUR E 25. ALMEN GAGE N O .

~~~

112

J
 - -‘ - ‘

The procedures for using the standard shot peening test

strips , desc r ibed in SAE J443 , are br iefly as follows (35 ):

1. Fasten the test strip tightly and centrally in the holder

(Figure 24).

2. Expose the surface , X in Figure 24 , to the peening conditions

to be evaluated . Record the time used for blasting .

3. Remove the test strip from the holder and measure the arc
height with the gage (Figure 25 ). The zero position of the
gage mu s t be checked f r e q u e n t l y and , if necessary , ad justed .

The degree of coverage of shot peening can be estimated

by the following procedure :
1. Polishing the strip to obtain a reflective surface.

2. Fastening the specimen to the test stri p holder and peening

under conditions identical to those to be used in production
and for determining the Almen gage reading.

3. Removing the strip from the holder and placing it in the

field of a metallurgical camera .

4. Using a piece of transparen t paper as a ground glass and a

magn i fica tion of 50X , trace the indented areas with ~ sharp
penc il. The indented areas can be identified by the con-
trast with the polished surface .

5. Measure the area of the indentations within a known area

using a plan imeter. The ratio of the indented area to the
total area is the percentage of coverage .

113

1•

-~~~“ -
- --
 114

-~~~~~~ -~~~~ ~~ - = ~~~~~~ --‘-~~~~~~~~

. _ _

-- -
_
- - -- - - -- -
-
- --
--‘ - -- ~~~~
 SECTION IX

9. GLOSSARY

Abrasive: Material used for cleaning a n d/or surface roughening ,

usually sand , crushed c h i l l e d cast iron , crushed steel grit ,
aluminum ox ide , silicon carbide , f l i n t , g a r n e t , or crushed slag .
Abrasive Blasting or Grit Blasting : The forceful direction of
a b r a s i v e p a r t i c l e s a g a i n s t the s u r f a c e of workpieces or p r o d u c t s
to re m ove con tam inants o r to condi tion surfaces fo r subsequent
operations.

Air Coole r: Work Piece Cooler , which see.

Anode: The electrode maintained at a positive electrical potential.
In most plasma-torch designs this is the front electrode , construc-
ted as a hollow no z z l e and f a b r i c a ted from copper.

Apparent Density or Density Ratio: The ratio of the measured den-

si ty of a n ob ject to the absolu te density of a perfec t ly solid
ma te r i a l of the same com pos ition , usually expressed as a percen tage.

Arc: A l u m i n o u s d i s c h a rge of e l e c t r i c a l cu rr e n t cross ing the gap

be twee n two e l e c t r o d e s .

Arc Chamber: The conf ined space e n c l o s i ng the anode and cathode
in which the arc is struck.

Arc Gas: The gas i n t r o d u c e d i n t o t h e a r c chamber and i o n i z e d by

the ar c to f o r m a p l a s m a .

Base Metal: Substrate , wh ich see.

Base Material: Substrate , which see.

Berry Formation: A detrimental build-up of spray material on the

gun nozzle and/or air cap during the spraying operation .

B l a s t i n g: A method of c l e a n i n g a n d/ o r s u r f a c e r o u g h e n i n g by a
f o r c i b l y p r o j e c t e d s t r e a m of s h a r p a n g u l a r a b r a s i v e .

Bond: ( 1) To j o i n s e c u r e l y . (2 ) A u n i t i n g force . (3) In t h e r m a l

spraying , the junction between the material deposited and the sub-
s t r a t e , or its strength.

Bond Cap : The term commonly used to describe a test specimen on

w h i c h c o a t i n g is a p p l i e d f o r the purpose of t e s ti n g bond s t r e n g t h .

115

-
 - - ---- -- - --- ‘ - “ - _
--‘ -‘
~~~~~ ~~~~~ ~~~~~~~~~~~~~~ ‘ ~~~ ~~~~~~~~~~~~~~~~~ ~~~~~~~~~~ ‘

Bond Coating or Bonding Coat: A thin , intermediate plasma-sprayed

layer of a material (e.g., molybdenum) applied on the substrate to
enh ance the adhe rence of a su bs e q u e n t l y spr ay ed coa ti ng .

Bond Strength: The force required to pull a coating free of a

substrate.

Carrier Gas: In thermal spray ing , the gas used to carry the powdered
materials from the powder feeder or hopper to the gun .

Cathode: The electrode maintained at a negative electrical poten-

tial. Ysually the rear electrode , conically shaped and fabricated
f rom tungst~ n or thoriated tun gsten.

Coating Density : The ratio of the determined density of the coat-

ing to the th~~~retica1 density of the material used in the coating
process. Usually expressed as percent of theoretical density.

Coating Stren gth: A measur of the cohesive bond within a coating,

as opposed to codting-to-substrate bond ; the tensile strength of
a coatin ~~.

Coating Stress: The stresses in a coating resulting from rap id

quenching of molten or semimolten harticles as they impact the
subs tra ~e.

Coefficient of Thermal Expansion: The ratio of the change in

length per degree of temperature to the length at 0 C or 0 F.

Composite Coating : A coating consisting of two or more layers

of different spray m aterials.

Control Console: The instrumented unit from which the plasma

torch is operated and operating parameters are monitored . Func-
tions controlled and monitored are power level , stabilizing gas
pressure and flow , powder-feed Tas pressure and flow , and cooling
water flow .

Controlled Atmosphere Chamber: An enclosure or cabinet filled

with an inert gas in which plasma spray ing or welding can be per-
formed to minimize (or prevent) oxidation of the coating or sub-
strate. The enclosure is usually fitted with viewing ports , glove
ports to permit manipulations , an d a sma l l separa te a ir l o c k f o r
introducing or removing components without loss of atmosphere .

Density : The mass per unit volume of a material , u su al l y ex pressed

as grams/cubic centimet~’r or pounds/cubic inch .

Density Ratio: Apparent Density, which see.

116

- -
‘ ~~- ~~~~ - _ _ _ _
Deposit: Spray Deposit, which see .

Deposit Efficiency : The ratio , by w e i g h t , of material deposited

to m a t e r i a l fed i n t o t h e gun , measured by s p r a y i n g on a l a r g e sur-
face away from edges.

Depos ition Rate: The speed with which material is deposited on a

substra te , usually expressed in grams/minute or pounds/hour.
D w e l l _ Time : The l e n g t h of time the particles spend in the plasma
stream .

Edge Effect: Loosening of the bond between the sprayed material

and t h e base m a t e r i a l a t the edges , due to s t r e s s e s set up in
cooling.

Edge Loss: Material lost as overspray resulting from spraying near

the edge of an object.

E l a s t ic M o d u l u s : The r a t i o of s t r e s s , wi thi n the proportional

l i m i t , to t~ e corresponding strain. Young ’s Modulus is measured
in tension or compression; the modulus of rigidity is measured by
shear or torsion tests.

Elec trode: A n el ectr ical con d uctor for leading c u rrent in to or

out of a medium . In arc and plasma s p r a y i n g , the c u r r e n t - c a r r y i n g
componen ts wh ic h support the arc .
Enclosur e: For me tal spray ing , a chamber used for minimizing con-
tamination. See Con troll ed A tmosphere Chamber.
Exhaust Booth: A mechanically ventilated , semi-enclosed area in
which an air flow across the work area is used to remove fumes,
gases , and overspray material during therma l spraying operations.

Feed Rate or Spray Rate: The q u a n t i t y of m a t er i a l passed through

the gun in a unit of time .

Fines: Those p a r t i c l e s at the lower end of the s p e c i f i e d mesh s i z e .

Flame Spraying : A process in which materials are melted or softened

in a heating zone and propelled in a molten or heat-softened
(plastic) condition onto a target to form a coating . The term
“f lame ” s p r a y i n g is u s u a l l y used when r e f e r r i n g to a combustion—
spraying process , as differentiated from “ plasma ” spraying or
“plasma-f lame ” spraying .

Flow Meter: Device for indicating the rate of gas flow in a system .

117

- -.. .
~~~~~~ -~ -~~~~‘-- ~-- =-:~~-~~- --- -
-
 _

Fretting : Surface damaqe re sulting fron ~ relative motion between

surfaces in contact under pressur e , especially likely in a corro-
sive environment.

Fusion Spray : The process in which the coating is completely fused

to the base metal , resulting in a meta l lur q ica lly bonded , essen—
t i a l l y void-free coating .

Galvard o Corrosion: Corrosion caused by the current between two

d i s s i m i l a r cor h~ctcr s in an electrolyte , or two similar conductors
in d i s s i m i l a r e l e c t r o l y t e s . If th~ two dissimilar metals are in
contact , the rc~iction is referred to as “ couple action ” .

Gradated or Gradient Coating : A deposit which changes continuously

but almost imperceptibly in composition from one surface to another ,
e.g., from 100 percent A at substrate to 100 percent B at top of
the coatioc .

Graded Coatir.~ ’ : A coath ~q consisting of several successive layers

of d if ferent materials; e .q . , starting with 100 percent metal ,
followed by one or more layers of m eta l-ceramic mixtures , and
finishing with 100 percent ceramic.

Grit: Ah ras~ vc , which see.

G r i t Blasting : Ab r a sive 31as~~inq , which see .

Gun : A term used t o ~d ent i f a therma l sprayinci device , especially

the types used for deposit inc coatings ho the olasma-arc or detona—
tion—s r ray processes.

Inert Gas: A ~aS , s u c h a s h e~~iun , ar ~en , or neon , wh ~ch is stable

and ~Joes not form reaction orod~ cts w i t h other mat er ials.

Interface: A surface formi n g a common boundary between adjacent

l a y e r s , usually the surface between the spray deposit and the
substrate.

Ion : An atom or group of atoms (molecule) that carries a positive

or negative charge as a result of having lost or gained one or
more electrons.

lask: A device for protecting a surface from the effects of blast-

ing and/or coating. Masks are cenerally of two types: reusable
or disposable.

118

—~ — - -----—--
Masking : The method of pro tecting the areas adjacen t to the areas
to be thermal sprayed or blasted to prevent adherence of a coating
or surface roughening .

Matrix: The p r i ncipal phase or aggregate , u s u a l l y c o n t i n u o u s , in

which other constituents (such as oxides or carbides) are embedded .

Mechanical Bond: Adherence of a coating to a base material , accom-

plished mainly through mecha n ical inte r lock ing wi th roughened
surfaces.

M e t al l i z i n g: Forming a m e t a l l i c c o a t i n g by spray ing w i th molten

metal or by vacuum deposition .

M e t a l l u r g i c a l Bond: Adherence of a c o a t i n g to t h e base m a t e r i a l

c h a r a c t e r i z e d by d i f f u s i o n , a l l o y i n g , or intermolecular or inter-
g r a n u l a r a t t r a c t i o n at t h e i n t e r f a c e between t h e sprayed p a r t i c l e s
and the base mat er ia l; usually stron ger than a m echanical bond .
Modulus of Ruptu re: N om inal stress at f ractu re in a bend test or
a t o r s i o n test .

Open Circuit Voltage: The potential difference applied between

the ano d e and ca thode pr ior to in it ia ti ng the a rc.

O v e r s p r a y: The excess s p r a y m a t e r i a l t h a t is not d e p o s i t e d on t h e

par t bein g sprayed .

Pa ram e ter: A m easu r able cons tant or variable tha t is rela ted to
and a f f e c t s o ther char ac te ri s ti cs or var iables describin g a system
or pro du c t .
Particle-Size Range: Classification of spray powders defined by
an uppe r an d lower size limi t; e . g . , -200 + 325 m e s h : a q u a n t i t y
of powder , the l a r gest pa rticles of w h i c h w i l l pass t h r o u g h a 200
mesh sieve and t h e s m a l l e s t of w h i c h w i l l not pass t h r o u g h a 325
m esh s ieve .

Pass: A s ing le progress ion of the thermal s p r a y device across the

s u r f a c e of t h e s u b s t r a t e.

P lasma: An elec trically neu tral , highly ionized gas com posed of
ions , e l e c t r o n s , and n e u t r a l p a r t ic l e s .
Plasma Flame: The zone of intense heat and il ght emanating from
the o r i f i c e of the arc chamber resulting from energy liberated as
the charged gas particles (ions) recombine .

119
 ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
_ _ _ _ _ _ _ _ _ _

Plasma—Forming Gas: The gas , in the plasm a g un , which is heated

to t h e h i g h tempera tur e pl asm a sta te by the el ectr ic a r c .

Plasma Gases: Plasma Fo rm ing Gas , wh ich see.

Plasma Gun: A device wherein a plasma is generated to provid e a

heat source for therma l spraying operations.

Plasma Sp r a y ing : Producing a coating by passing a material in

particulate or powder form through a plasma flame and depositing
the subsequently heat-softened particles onto a base material or
substrate.

Plasma Torch or Plasma Gun: A device for producing a plasma flame ,

consisting of an arc chamber , an anode and a cathode , and equipped
with cooling water , stabilizing gas , and powder-feed inlets and
external power leads .

Powder Feeder: A mechanical device designed to introduce a

metered and controlled flow of powder into the plasma-spray torch.

Powder-Feed Rate: The quantity of powder introduced into the arc

per unit time ; expressed in pounds/hour or grams/minute.

Powder-Feed Gas: The gas used to transport the powder from the
feeder into the arc; usually an inert gas and most often argon.

j~~~: Parts per million ; 1 ppm is equal to 0.0001 percent.

Preheat: Heat applied to the base material prior to initiating

the spray operation so as to avoid the presence of condensate on
the substrate surface as the first particles are deposited or to
minimize residual stresses.

Primary Gas: In therma l spray ing , the gas constituting the major
constituent of the arc gas fed to the gun to produce the plasma .

Quench Rate: The speed with which a sprayed particle cools upon
striking the surface of the base material.

Ro tary Roughening : A method of surface roughening wherein a revolv-

ing roughening tool is pressed against the surface being prepared ,
while either the work , or the too l , or both , move .

Relative Density : Apparent Density , which see.

Resid ual Stress: Stre ss presen t in a body th at is f r e e of ex ter nal

forces or thermal gradients.

120

- -
r
- ‘ - . .- -- - - - - -

~~~~ ~~~~~~~~~

Rough Threading : A method of surface roughening which consists of

cutting threads w ith the sides and tops of the threads jagged and
torn .

Seal Coat: M a t e r i a l a p p l i e d to i n f i l t r a t e the pores of a thermal

s p ray depos it .
Secondary Gas: In thermal spraying , the gas constituting the minor
constituent of the arc gas fed to the gun to produce the plasma .

Self- Bonding Materials: Those materials that exhibit the charac-

t e r i stics of f o r m i n g a me ta l l ur gical bond with the substrate in
the as-sprayed condition.

Self-Fluxing Alloys: Certain materials that “wet ” the s u b s t r a t e

and coalesce when hea ted to t h e ir mel ti n g poin t , without the addi-
tion of a flux ing agent.

sf m : Surface feet per minu te ; linear pa ss veloc ity in surface

speed per m i n u t e .

Shadow Mask: Method of partially shielding an area during the

s p r a y i n g operat ion , t h u s p e r m i t ting some ove rsp r a y to produce a
f e a t h e r i n g at the coa ting ed ge .

S h i e l d i n g Gas: A s t r e a m of i n e r t gas d i r e c t e d at the s u b s t r a t e

d u r i n g s p r a y i n g so as to envelop the p l a sma f l a m e and s u b s t r a t e;
int ended to prov ide a barrier to the a tmosphere in order to
minimize oxidation.

Sieve A nalys i s:
A me thod of de te rm i nin g part i cle s i ze distribution ,
usually expressed as the weight percentage retained upon each of
a series of standard screens of decreasing mesh size.

Spall ing : Flaking or separation from the substrate of a sprayed

coating.

Spray: A moving mass of dispersed liquid droplets or heat-softened

particles .

Spray A n g l e : The a n g l e of p a r t i c l e impingement , measured from the

s u r f a c e of the s u b s t r a t e and the a x i s oi the spray nozzle.

Spray Deposit: A coating applied by any of the therma l spray

methods .

Spray Distance: The distance maintained between the plasma—torch

nozzle and the surface of the base material dur ing spraying .

Spray Rate: Feed Rate , w h i c h see .

121

_ _ _ _ _ _ _ ______ _ _ _ _ _ _ _
~p r ay i n g Sequence: The o r d e r in wh i ch d i fferent passes of similar
or differen t mater ia ls are appl ied in a pla n ned relationship, such
as overlapping, s upe ri mposed , or at certain angles.

S tabilizing Gas: The a r c gas , w h i c h is i o n i z e d to f o r m the plasma .

Introduced into the arc chamber tangentially, the re 1 a ti v e ly cold
gas chills the outer surface of the arc s t ream t en d ing to co n s t r ic t
t h e arc , r a i s e i t s t e m p e r a t u r e , and f o r c e i t out of t h e f r o n t anode
n o z z l e in a steady , rela ti vely unfluc tua ti ng s tream .

Subs trate: The ma te r i a l , workpiece , or sub stanc e on wh ich the

coating is deposited .

Substrate Preparation: The set of operations , in c l u d in g clea n in g ,

degreasing , and roughening , applied to the base material prior to
applying a coating; intended to insure an adequate bond to the
coat in g .

Substrate Temperature: The temperature attained by the base mate-

rial as the coating is applied . Proper control of the substrate
temperature by phased s p r a y i n g or by the a pp l ic at ion of ex te r n a l
cooling will minimize stresses caused by therma l expansion
differences.

Surface Preparation: The operations necessary to prepare a surface

for therma l spraying.

Surface Roughening : A group of procedures for producing irregu-

larities on the surface to be therma l sprayed . See Blasting,
Rotary Roughening , Rough Threading , and Threading and Knurling.

Thermal Spray : Any coating process in which particles are heated

to a molten or plastic state and propelled onto a substrate to
form a coating ; includes flame and plasma spraying using wire or
powder processes.

Thermo Spray : A trade name for a particular flame—spray process.

(Metco , Inc . powder flame-spray process.)

T h r e a d i n g and K n u r l i n g : A method of surface roughening wherein

sp i r a l t h r e a d s are made and t h e tops of t h e t hr e a d s a r e spread
w ith a k n u rl in g t o o l .

Torch: U s u a l l y , a gas burner with feed lines for fuel and oxygen
used to braze, cut , wel d , or to heat material to be sprayed .

T r a n s f e r r e d Arc: A p l a s m a- s p r a y process in w h i c h the w o r k p i e c e is

the an ode for the plasma arc.
T r a v e r s e Speed: The l i n e a l v e l o c i t y at w h i c h t h e torch is passed
across the subs t ra te du r i ng the s p rayi ng o peration.

122

I
Undercoat: A depos ited coat of material which acts as a substrate
for a subsequent thermal sprayed deposit. See Bond Coat.

Undercut ting : A step in surface preparation involving remova l of

substrate material.

Water Wash: The forcing of exhaust air and fumes from a spray
booth throug h wa ter so that the vented a ir is free of thermal
sprayed particles or fumes.

Wire Flame Spraying : Flame spraying metallic material fed to the

torch or gun in w i r e or rod f o r m .

Wire Flame Spray Gun: A flame spraying device utilizing an oxy-

ace ty l e ne gas f l ame to provide the h e a t , and the metallic material
to be s p rayed in wire or rod form.

Wire Speed: The length of wire sprayed in a unit of time .

W i r e St r a igh tener: A f ix ture f or taking the cas t out of coiled

wire t o en abl e i t to be eas i ly fed i nto the gun .
Work Piece Cooler: A device used to direct an air blast onto a
par t being sprayed to prevent overheating of the part .

123

I
__ _ _
_-; - -- -- - - ------ -- -
-
-- — ---- - - - - ----
—‘U’
~~~ ~~~~~~~~~~~ ~~~~~~~ ~

124

~~~— — - —~~~~- - - - - —~~ -~~~~~~~~~~ - - =-

 SECTION X

10. REFERENCES

1. Ano nymous , “A New Use for the P lasma G un ” , Busi ness Week ,
( S e p t . 27 , 197 6) , p 7 2 x .

2. Poorman , R . M . , S a r g e n t , H . B . , and Lamprey , H . , “Method and

Appara tus Ut i l i zing Deton at i o n Waves for Sp r a y ing and O t h e r
Purposes ” , U.S . Patent No. 2 ,714 ,563 (1955).

3. Doyle , A.G., and Lambert , J . W . , “The Flame P l a t i n g Process ” ,

B r i t i s h W e l d i n g J o u r n a l , vol 10 (1963) p 450.

4. Most , C . R . , “S ur face Coa ti ng s Available to Indus try Today ” ,

p r e s e n t e d a t Society of Automotive Eng i n e e r s Mid-Year M e e t i n g ,
Chicago , IL (1969)

5. Tucker , R.C., J r . , “Str u c t u re Proper ty Rel at i o n s h ips in Depo-

si ts Produced by P lasma Spr ay and Detonatio n Gun Techniques ” ,
J. Vacuum Sc ience , vol 11 , no 4 ( July/August , 1974) pp 725—734.
6. Mash , D . R . , and Brown , I . M . , “Str u c tu r e a nd Pr o p e r t i e s of
Plasma—Cast Materials ” , M e t a l s En gr g . Qu a r t e r l y , vol 4 , no 1
(Feb. 1 9 6 4) pp 1 8 — 2 6 .

7. Kuijpers , T.W., an d Zaa t , J .H., “ Influence of Oxygen and Cool-

inq Rate on the Microstructure and Microhardness of Plasma-
Sprayed Molybdenum ” , M e t a l s Technology , vol 1, no 3
(March 1974) pp 142—150.

8. Metals Handbook, 8th Edition , Volume 1, American Society for

Me t a l s , Me tals Park , OH (1961)

9. Roseberry , T.J., Onesto , E .J. , and D u f r a n e , K.F., “F i n a l

Repor t o n Test ing of Plasma Sprayed Coa tings ” , Contract
N — 0 0 l 9 7 - 7 5 — C - 0 0 6 0 , B a t t e l l e , Columbus L a b o r a t o r i e s, Columbus ,
OH (Feb. 1 9 7 6) .

10. AWS Committee on Thermal Spraying, “ P lasma Spraying” , Publi-

cation AWS C2.1 3— 70 , American Welding Society, Inc., New York ,
NY (1970) 18 pp.

11. Van Wyk , J.W., “ Ceramic A irframe Be arings ” , Report no D180—

19181—1 , Boeing Aerospace Co., S e a t t l e , WA (Nov . 1, 1975) .

12. Truskov , P.F ., Kovalchuk , Yu.M., et al., “AK—4 Antifriction

Plasma Coat ings ” , Report no FTD—HT-23—l067-72 , Foreign Tech-
nolo gy D i v i s ion , WPA FB (Nov . 17 , 1972).

125

- - .
~~~~~~~~~ -
 - — -

13. Levy , M., a n d Moross i , J .L., “ E r o s i o n and Fa ti gue Behav ior of

Coated T i t a n i u m A l l o y s f o r Gas T u r b i n e E n g i n e Compressor
A p p l i c a t i o n s” , Report no AMMRC— TR-76-4 , Army Materials and
M e c h a n i c s Re s e a r c h C e n t e r , Water tow n , MA (F e b . 1 9 7 6) .

14. Preece , C.M. , Herma n H . , et al ., “T he Respons e of Coa ted

Steels to C av i ta ti on in Corrosive Env i ro nm en ts ” , Repor t TR— l ,
Dept . of Materials Sciences , State University of New York at
Stony Brook (May 1976).

15. C a l a b r e s e , S., and Coda , H.T., “Substrate Corrosion of Plasma-

Coated Surfaces ” , Technical Report NT1 71TR7 , Mechanical
T e c h n o l o g y , Inc . (Feb . 1971)

16 . Handbook of Chemi stry and Physics, 34th Edition , Chemical

Rubber P u b l i s h i n g C o . , C l e v e l a n d , OH ( 1 9 5 3) .

17. “Specialized Blast Cleaning Equipment , A Selection Guide ” ,

M a n u f a c t u r e r ’ s B r o c h u r e 0 7 1- 0 4 7 5 , Clemco I n d u s t r i e s, San
Fr a n c isco , CA (July 1975).

18. Gole go , M.L., and Panamarchuk , V.G., “Effect of Roughness of

Titanium—Based Material on the Strength of Plasma Nickel—
Coating Adhesion ” , Soviet Materials Science , vol 10 , no 6
1974) pp 630— 632.
19. Grisaffe , S.J., “Analysis cf Shear Bond S t r e n g t h of Plasma—
Sprayed Alumina ” , NASA TN D-31l3 (1965) 11 pp.

20. Bethke , J.J. , “The E f f e c t of Plasma Sprayed Metco 4 0 4 and 439

Coatings on the Fatigue Life of 4340 Steel” , Phase Report
AIRTASK no WR-5l-5l78W , Work Unit no GA 802 , Report no NADC-
7 4 5 2 — 3 0 , AD B001662 (7 Jan . 1975)

21. “Shot Peening ” , in ASM Metals Handbook, Volume 2 , American

Soc ie ty f o r Me ta ls , Metals Park , OH ~l964) pp 398—405.

22. F i s h e r , l.A., “Variables Influencing the C h a r a c t e r i s t i c s of

P l a s m a — S p r a y e d C o a t i n g s ” , I n t e r n a t i o n a l ~ e t al l ur g i c al Reviews ,
vol 17 (1972) pp 117—129.

23. Palermo , J . R . , and P o t t e r , C . C . , “ P l a s m a S p r a y i n g Present -

and F u t u r e ” , Thermal Dynamics Corporation , Lebanon , NH ,

u n d a t e d p a m p h l e t , 19 pp.

24. Nimvitskaya , T . A . , and Fi shm an , S.L., “Deposition of Refrac-

tory Coa ti ng s Wi th the Use of P lasma ” , Report FTD-HT-23-176-
69 , Foreign Technology Division , Ai r Force Sys tems Command ,
AD no 694400 (13 May 1969)

126

-
--
-- A
-- ~~~~ --- _ - - ---~~~~~ -- — -- - -~~ ~~ - - - -
~~~~~~
- -
25. “Standard Specification for Wire-Cloth Sieves for Testing
Purposes ” , ASTM Designation Ell-70. American National Standard
A2 3.l-l973 approved Feb. 15 , 197 3 by A m e r i c a n N a t i o n a l
Standards In s t itute (ANS I)
26. “ S t a n d a r d Test Method f o r Sieve A n a l y s i s of Granular Metal
Powders ” , ASTM Designation B2l4-66 (Reapproved 1970). Ameri-
can National Standard H9 3-1973 approved Jan. 18 , 1973 by ANSI.

27. “Standard Method for Subsieve Analysis of Granular Metal Pow-

ders by A i r C l a s s i f i c a t i o n” , ASTM Designation B293-60 (Reap-
proved 1970) American National Standard H9 9-1973 (R 1969) ,
.

approv ed Ja n . 18, 1973 by ANSI.

2 8. I r a n i , R . R . , an d Co ll i s , C.F ., Particle Size Measurement ,
I n t e r p r e t a t i o n and A p p l i c a t i o n, John Wiley and Sons , Inc.,
New York (1963) 166 pp.

29. “ E v a l u a t i o n Methods and Equi pment f o r F l a m e- S p r a ye d C o a t i n g s ” ,

Metco Inc . (1963) 15 pp.

30. “ Standard Test Method for Adhesion or Cohesive Strength of

Flame-Sprayed Coatings ” , ASTM Designation C633-69 (Reapproved
1974). American National Standard Z167.22—l973 , a p proved
June 8, 197 3 by ANS I .
31. “St a n d a r d Tes t Method f o r M i c r o h a r d n e s s of M a t e r i a l s ” , A STM
Designation E384—73. American National Standard Z30.l2-l973 ,
approved Nov . 27 , 1973 by A N S I .

32. “Standard Test Methods for Rockwell Hardness and Rockwell

S u perfi ci al Hard ness of M e tallic M a terials ” , ASTM Designation
El8—74. American N a t i o n a l Standard Z l l S . 6 , ANSI.

33 . Underwood , E .E., “ Ap p licat ions of Quan t itat ive M e tallography ” ,

in ASM Metals Handbook, Volume 8, American Society f o r M e t a l s ,
M e t a l s P a r k , OH 4 4 0 7 4 ( 1 9 7 3 ) pp 3 7 — 4 7 .

34. “Test Strip, Holder a nd Ga g e for Sho t Peen ing ” , SAE S tandard
J 4 4 2 , SAE Handbook, Part I , SAE Inc., Warrendale , PA (1977)
pp 9.05—9.06.

35. “ P r o c e d u r e s f o r Us ing Standard Shot Peer u ing Tes t S tr ip ” , SAE

Recommended Prac t ice J 44 3 , ibid. pp 9.07-9.08.

127
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-

128

1
,

- ~~~~ --— -~~ ~~~~

_ _ _ _ _ _ _ _ _ _
---- - -
-
______________________ -

SECTION X I

11. BIBLIOGRAPHY

Criteria for Recommended Standard, Occupational Exposure to:

Ultraviolet Radiation, Publication No. HSM 73—11009 , Cat. No.
HE 20.28ll :Ul 8, U.S. Government Printing Office (1972).

Handbook of Laboratory Safet1, Ed. by Norman V. Steere, The Chemi-

cal Rubber Co., Clevela nd , OH ( 1967 )

Industrial Ventilation: A Manual of Recommended Practice, 13th

Edition , Committee on Industrial Ventilation , American Conference
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Chevela , O . B . , and Orlova , L . M . , “ S t r u c t u r a l C h a r a c t e r i s t i c s of t h e

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 Hagopian , John H . , and B a s t r e s s , E. K a r l , Recommended I ndu s t r i a l
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M a l i k , M.P., “A pp l ica tions of Plasma Me tal Spr a y ing in Salvaging

A i r c r a f t and E n g i n e Components ” , p r e s e n t e d at 6 t h I n t e r n a t i o n a l
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.
 _ _ _ _ _ _ _

Ph i lp o t t , T . , “ Hot-Spray Coatinq Offers Production Advantages ” ,

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132

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.
~l4
_ V V

SE CTION XII

12. COATING DATA SHEETS

12.1 BOND STRENGTHS

The a v e r a g e bond s t r e n g t h s for seven types of plasma-
sprayed coa t ing s deposited on five types of substrates are listed
in Table X XX. The c o a t i n g s were 0 .0 1 5 to 0.022 inch (0.38 to
0 . 5 5 mm ) thick. The oxide coatings were ground to 0.015 inch be-
f o r e test in g , to insure flatness. The coatings were sprayed , in
air , on bond-cap spec imens. The strengths were determined by pro-
cedures conformin g to the ASTM specifications for measuring ad-
hes i ve and cohesive strengths. (3u) The values are averages for
six determin atio n s on coatings deposited us ing controlled spray ing
p a r a m e t e r s and s u r f a c e p r e p a r a t i o n p r a c t i c e s . E x p e r i e n c e from
these t e s t s and o t h e r s i m i l a r s t u d i e s i n d i c a t e s t h a t the repro-
ducibi i l ty of values , from bond—s trength tests considered reliable ,
is about ±5 percent of the average value for six tests.

A l l of the s u b s t r a t e s were d egreased , gr i t b l a s ted ,

cleaned w i t h u l t r a s o n i c a g i t a t i o n in t r i c h l o r e t h y l e n e, and washed
in 200-proo f alcohol. They were spray-coated within 1/2 hour of
cleaning . The g r it blasting was co nducted a t an air pressure of
60 psi with a nozzle-workpiece distance of 4 to 6 inches. The
p article s i ze of the alumina gr i t was described as being
-60 + 40 mesh. As indicated in the table , those g rit blasting
conditions resulted in slightly different roughness values on sub-
s t r a t e s of d i f f e r e nt compositions .

The bond s treng th da ta in Table XXX were ob tained on

specimens spray coated u s i n g one p a r t i c u l a r type of p l a s m a — g u n
equ ipment. However , many bond- strength tests were also made on
coatings depos ited with two other types of commercially available
p l a s m a - s p r a y equipment . Those bond s t r e n g t h s agreed w i t h the
v a l u e s l i s t e d in the t a b l e , with in appro~c i m a t ely 5 percent , when
deposi ted under cond it io n s descr ibed i n Plasma Data Sheets.

12.2 PLASMA SPRAY VARIABLES

Parameters recommended for depositing seven types of

coatings are described in the attached data sheets. The conditions
are those found to be suitable by experiments with the three types
of plasma-gun equipment mentioned in the sheets . The quality of
the coatings was evaluated , using bond-strength tests , described
above , microhardness tests , and metallographic examinations for
porosity and for voids at the bond-substrate interface . It is be-
lieved that the conditions described in the sheets are suitable
for producing high quality plasma-sprayed coatings . The plasma-
spray ing parameters are not apprec iably affected by the substrate
material.

133

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_ _ _

TABLE XXX . BOND STRENGTHS OF PLASMA-SPRAYED COATINGS

DEPOSITED ON DIFFERENT SUBSTRATE MATERIAL S (a)

Bond S trength , f o r S u b s t r a te
Ma te r i a l I nd ic a t e d , psi
Low 316
A l u m i n u m Carbon Stainless
Coating Material Aluminum Bronze Steel Steel K-Monel (b)
87TiO 2 — 13A1 2 O 3 38 95 4175 41 05 41 65 415 0
Cr 2 03, 99% 5965 6220 6485 6450 6345
95 .5Ni—4.5A1 4430 4725 4880 4885 4800
8ONi— 2OCr 4310 4350 4455 4485 4541
Molybdenum , 99% 5075 5730 5920 5810 5745
Aluminum, 99.0+% 3965 4465 4405 4285 4270
Aluminum bronze 4 085 4555 4 67 0 47 55 471 5
Surface Roughness of Subst ra te , microinch AA
300 260 250 220 250

(a ) Values a r e averages for six d e t e r m i n a t i o n s . The plasma spray

parameters are descr ibed in Data Sheets 1 through 7. Plasma
sprayed c o a t i n g s deposited a c c o r d i n g to methods described in
Data Sheets 8 through 16 exhibited comparable bond strengths.

(b) The most recent designation for the material formerly known
as K-Monel is K-5 00.

In all of the exper iments s ummar i zed by da ta sheets 1

through 16 , the following practices were held constant:
Subs trate Surface Flat
Spray An g le 90 °
Preheating Temperature 150 F (65 C)
Coating Depth/Pass . . 0.002 inch (0.05 mm)
Coating Thickness lip to 0.030 i~zch ‘0.75 mm )
Coating Speed , lineal , fpm 12.5
Powder-Carrier Gas . . Argon
Carrier Gas Pressure . 5 0 psi
Substrates 1-in. D x 2.5 in.
Substrate Cooling Method Blast of dry air

If less-massive substrates than those used in these studies are to

be plasma-arc coated , better substrate cooling techniques are de-
sirable. Commercial devices marketed for that purpose are reputed
to work satisfactorily.

134

I
 Data sheets 17 through 25 describe spraying conditions
used for apply ing plasma-arc coatings on the cylindrical rods men-
tioned in Section 2 . 1 . 1 . 2 . The s p e c i f i c a t i o n s of the powders used
in that investigation are listed in Table XXI. In those studies
the round s u b s t r a t e s were r o t a t e d at 350 rpm , which resulted in a
lineal traverse speed of 91 fpm . The conditions described in data
sheets 17 through 21 were used to deposit coatings 0.030 inch
(0.75 mm) thick in approximately 15 passes.

Data shee ts 22 t h r o u g h 25 id e n t i f y the plasma-spraying

parame ters used at N a v a l O r d n a n c e S t a t i o n , L o u i s v i l l e, to deposit
coatings 0.022 inch (0.055 mm ) thick on specimen cy linder rods .
Ni trogen was used as the primary arc gas and as the powder-carrier
gas in those p r o c e s s i n g o p e r a t i o n s . The c o a t i n g s were considered
comparable in q u a l i t y to those produced us ing ar gon f o r arc and
carr ier gas and the c o n d i t ions d e s c r i b ed in da ta sheets 17
though 21.

The data sheets identify the nozzles used for the plasma—
arc d e p o s i t i o n o p e r a t i o n s by ma n ufac turer ’ s component numbers.
The f o l l o w ing com pa r a t i v e i n fo rma tion may be i n forma tive :

Data (Anode) Orifice Open-Circuit

Sheets Nozzle ID , inch Vol tage
8—12 901065 0.313 80
13—16 S 1—3—F 0.312 80
1—7 GH 0.250 160
17—21 GH 0.250 160
22— 25 G 0.249 160

FWB :ebk

135

_ _
V . _~~ _ _ _ - __ -~ -~~
~ - . _-
- -

PLASMA SPRAY DATA SHEET-- 1

Spray Material Alurnina—Titania

Compos ition Ti02 13% , A 1 2 O 3 87%
S i z e r a n g e , m i c r o n s -53 + 15

Spray Gun
Type Me tco 3MB
Nozzl e GH
Powder por t # 2
Gun- to-work distance , i nches 4
Gas
Pr imary A rgon
Secondary Hydro gen
Flow , cfh
Primary 80
Se c o n d a r y 25
Power
Amps 500
Volts 75
Kilowatt 37.5
Powder Feeder
Type Me tco 3MP
Gear se t No t appl ic a b l e
M e ter wheel S
Feed Screw N o t ap p licable
Vi bra ti on amplitude No t appl i cable
RPM 24
Powder gas flow , c f h 37
Coat ~~ng Data
Spray rate , lb/hr 5

136

-- .
_ _ _ _- -- _ -
P..
—
_— -
_ -— !UII
~~~~~~~~~~~~~~~~~~~~ ~~~~ ~~

PLASMA SPRAY DATA SHEET--2

Spray Material Chromium Oxide

Composition Cr 2 0 3 9 9 . 0 %
S ize range , microns -74 + 10

Spray Gun
Type M e tco 3MB
Nozzle GH
Powder por t #2
Gun-to-work distance , inches 3
Gas
Primary A rgon
Seconda r y Hydroge n
Flow , c f h
Primary 80
Secondary 15
Powe r
Amps 500
Volts 65
Kilowatt 32 . 5
Powder Feeder
Type Metco 3MP
Gear set Not appl ic a b l e
M e t e r wheel S
Feed Screw No t ap pil cable
Vibration amplitude N ot a pp licable
RPM 25
Powder gas flow , cfh 37
C o a t i n g D ata
Spray rate , lb/hr 7

137

—_
- _ ~~~~ _ -- - - _ -
V_ _ -VV_~~ V V V _
~~~~~~~~~~~~~~~~~~~~~~ u — V----- -- V

PLASMA SPRAY DATA SHEET--3

Spray Material Nickel-Aluminum

Composition Nickel 95.5%, Aluminum 4.5%
S i ze ra nge, microns -88 + 44

Spray Gun
Type ?4etco 3MB
Nozzle GH
Powder port # 2
Gun-to-work distance , inches 5
Gas
Primary Argon
Secondary Hydrogen
Flow , c f h
Prima ry 80
Seco n dary 15
Power
Amps 500
V olts 65
Kilowatt 32.5
Powder Feeder
Type Metco 3MP
Gear set No t a p p l i c able
Meter wheel S
Feed Screw N ot applicable
Vibration amplitude Not applicable
RPM 20
Powder gas flow , cfh 37
Coating Data
Spray rate , lb/hr 9

138

.j
VV
 PLASMA SPRAY DATA SHEET-- 4

Spray Ma terial N ickel Chrom ium

Compos it ion N i c k e l 8 0% , Chromium 20 %
S ize r a nge , microns -105 + 44

Sp r a y Gun
Type Metco 3MB
Nozzle GH
Powder port #2
Gun—to-work dis’tance , inches 5
Gas
Primary Argon
Secondary Hydrogen
Flow , c f h
Pri mary 100
Secondary 5
Power
Amps 4 00
Volts 60
Kilowatt 24
Powder Feeder
Type Metco 3MP
Gea r set No t ap p l icable
Meter wheel S
Feed Screw No t app l icable
Vibration amplitude Not a pp l i c a b l e
RPM 40
Powder gas flow , cfh 37
C o a t i n g D ata
Spray ra te , lb/hr 19

139
 - - ~~~~~ --~~~~~~~~~~ - --- -
- - - -—--

PLASMA SPRAY DATA SHEET-- 5

Spray Material M oly b denum

Composition 99.0+%
Size range , m i c r o n s 74 + 44

Spray Gun
V
Type Metco 3MB
Nozzle GH
Powder port #2
Gun—to—work distance, inches 4
Gas
Primary Argon
Secondary Hydrogen
Flow , c f h
Primary 80
Secondary 15
Power
Amps 500
Volts 65
Kilowatt 32.5
Powder Feeder
Type Met co 3MP
Gear set Not applicable
Mete r wh eel S
Feed Sc rew Not appl ica b le
V i b r a t i o n am p l i tude No t a ppl ic a b l e
RPM 15
Powder gas flow , cfh 37
Coating Data
Spray ra te , lb/hr 9

140

1’

.
-- —--- -_ - V -- - _ -
__ _
— --..- - V ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
 PLASMA SPRAY DATA SHEET-- 6

Spray Material Aluminum

Composition 99. 0+%
Size range , microns -5 3 + 44

Spray Gun
Type Metco 3MB
Nozzle GH
Powder port #2
Gun—to—work distance , inches 5
Gas
Primary Argon
Second ary Hyd ro gen
Flow , cfh
Pr i m a r y 150
Secondary S
Power
Amp s 500
Volts 65
Kilowatt 32 . 5
Powde r Feeder
Type Metco 3MP
Gear set Not a pp l i c ab le
Meter wheel S
Feed Screw Not appl icable
Vibration amplitude Not applicable
RPM 32
Powder gas flow , c f h 37
C o a t i n g D ata
Spray rate , lb/hr 6

141

1
 -V --V — __ ~V_ V_ _ V __
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~ ~~~~~~~~~ VV ~ ~-V _ _ _ -~ V ~~~~~~~~~~~ _—

PLASMA SPRAY DATA SHEET-- 7

Spray Material Aluminum Bronze

Composition Aluminum 9.5% , Iron 1.0% , Copper 89.5%
Size range , microns -105 +44

Spray Gun
Type Metco 3MB
Nozzle GH
Powder port #2
Gun-to-work distance , inches
~
Gas
Primary Argon
Secondary Hydro gen
Flow , cfh
Primary 15 0
Seco n dary 5
Power
Amps 50 0
Volts 65
Kilowatt 32.5
Powder Feeder
Type Me tco 3M P
Gear set N o t app licable
Meter wheel S
Feed Screw No t a p plicable
Vibration ampl i tude Not applicable
RPM 27
Pdwder gas flow , c f h 37
Coating Data
Spray rate , lb/hr 1 4

142

1
- -
~~~~~~~~~~~~~~~~~ . .
 V -_ V _ -=-V: ~_- V=
_ _ _ _ _ .~~~~ V V V . . Z ~ V.V ~ V. ~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~

VV
PLASMA SPRAY DATA SHEET-- 8

Spray Material Alumina-Titania

Composition Ti O 2 13% , A1 2 O 3 97%
S ize ra nge , microns -53 + 15

Spray Gun
Type AVCO PG-l00
Nozzle 90l06~
Powder po rt No t appl ic a b l e
Gun-to-work distance , inches 3
Gas
Primary Argon
Secondary No t ap p l icable
Flow , cfh
Primary 70
Seconda ry Not applicable
Power
Amps 600
Volts 33
Kilowatt 19.8
Powder Feeder
Type AVCO PF 200
Gear set Not a pp l icable
M et e r w h e e l No t ap pl i c a b l e
Feed Screw 8 pitch
V i b r a t i o n a m p l i tude 50
RPM 300
Powder gas flow , c f h 7
Coating Data
Spray ra te , l b/ h r
~

143

V
V ~V
~V -~~ V
-- V
 - - V~~~~~~~~~ — - V ~~~~~~~ - -_V ~~~~~~~~~~~~~~~~~~~~~ --_ ~~~~- V - -V ~~~ V~~~ V - V V~~~~~~~ -V _- -~~~~~~

PLASMA SPRAY DATA SHEET-- 9

Spray Ma terial Chrom ium Ox i de

Composition C r2 03 9 9 . 0 %
Size range , microns - 74 + 10

Spray Gun
Type AVCO PG-lOO
Nozzle 901065
Powde r port Not ap p l i c a b l e
Gun-to-work distance , inches 3
Gas
Primary Ar go n
Secondary Not a p p l i c a b l e
Flow , c f h
Primary 70
Secondary Not applicable
Power
Amps 600
Volts 33
K ilowat t 19.8
Powder Feeder
Type AVCO PF-200
Gear set Not ap pl i c a b l e
Me ter wh eel No t ap p licable
Feed Screw 8 p it ch
V i b r a t i on a m p l i tud e 50
RPM 300
~Powder gas f l o w , c f h 7
C o a t i ng Da ta
Spray rate , lb/hr ~

144

_ _ _ _ _ _ _
V
_ _ _ _ _
r ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

PL SMA SPRAY DATA SHEET-- 10

Spray Material Nickel-Aluminum

Composition Aluminum 4.5% , Nickel 95.5%
Size range , microns —88 + 44

Spray Gun
Type AVCO PG-lOO
Nozzle 901065
Powder p o r t Not a p p l i c a b l e
Gun-to—work distance , inches 4
Gas
Primary Argon
Secondary Not a p p l i c a b l e
Flow , cfh
Primary 70
Second a ry Not applicable
Power
AmpS 500
Volts 28
Kilowatt 14
Powder Feeder
Type AVCO P F - 2 0 0
Gear set No t appl ic a b l e
M e t e r wheel Not a p p l i c a b l e
Feed Screw 8 pitch
Vibration amplitude 35
RPM 250
Powder gas f l o w , c f h 6
C o a t i n g D ata
Spray rate , lb/hr 6

145

-~t_t ~ t= -~~~ ’t-r-— - :,

— ~~
_dll1
~~~
~ --
--V-V-
-~~~~~~~~~ - -V - V - - V V -
~~~ V - _ V V -
- - - ~~~~~~

PLASMA SPRAY DATA SHEET-- 11

Spray Material Nickel Chromium

Composition N i c k e l 80% , Chromium 20%
Size r a n g e , m i c r o n s - 105 + 44

Spray Gun
Type AVCO PG-lOO
Nozzle 9010 6 5
Powder port Not a p p l i c a b l e
Gun-to-work distance , inches 4
Gas
Primary Argon
Secondary No t appl icable
Flow , c f h
Primary 70
Secondary Not a p p l i c a b l e
Power
Amps 5 00
Volts 28
Kilowat t 14
Powder Feeder
Type AVCO PF-200
Gear set Not appl icable
Meter wheel N o t ap p li ca b le
Feed Screw 8 pitch
Vibration amplitude 35
RPM 250
Powder gas flow , c f h 7
Coating Data
Spray rate , lb/hr 7

146

V -V

- _-
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~-~~~~~~ - - V _ V
 V
- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

PLASMA SPRAY DATA SHEET-- 12

Spray Material Molybdenum

Composition 99 . 0%
Size range , microns -74 + 44

Spray Gun
Type AVCO PG-lOU
Nozzle 901065
Powder por t No t applicable
Gun-to-work dista nce , inches 4
Gas A rgon
Primary Ar gon
Secondary Not a pp l i c a b l e
Flow , cfh
Primary 70
Secondary Not appl icable
Power
Amps 500
Volts 28
Kilowatt 14
Powder Feeder
Type AVCO PF-200
Gear set Not appl icable
Meter wheel Not appl ic a b l e
Feed Screw 8 pi t c h
Vibr at i o n a m p l i t u d e 35
RPM 250
Powde r gas flow , c f h 7
Coatin g Data
Spray rate , lb/hr 9

147

_ _ _ _ _ _ _ _ _ _ _ _ _
-- ---A
 __ ~~~~~
- ~~~~~~~~~~~~~~~ V
V -V
~~~~ V ~~-V

PLASMA SPRAY DATA SHEET--l3

Spray Material Alumina -Titania

Composi tion ‘riO 13% , A1 2 O 3 87%
Size range, microns -53 + 15

Spray Gun
Type Pl a s m a d y ne SB lB
Nozzle Sl— 3—F
Powder p o r t Not a p p l i c a bl e
Gun-to-work distance , inches 3
Gas
Primary Argon
Second ar y No t ap p l ica b le
Flow , c f h
Primary 65
Secondary Not applicable
Powe r
Amps 600
Volts 34
Kilowatt 20 .4
Powder Feeder
Type Plasmadyne Roto-Feed 1000
Gear set A
Meter wheel N o t applicable
Feed Screw N o t appl i cable
Vibration amplit ude N o t app licable
RPM 8 0
Powder gas flow , cfh 12
Coa t ing Data
Spray rate , lb/hr ~

14 8

I
 - - - ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ - - — -V ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

r
-

PLASMA SPRAY DATA SHEET--l4

Spray Material Chromium Oxide

Composition Cr2 03 99.0%
Size range , microns —74 + 10

Spray Gun
Type Plasmadyne SG lB
Nozzle Sl— 3— F
Powder port Not a p p l i c a b l e
Gun—to-work distance , inches 3
Gas
Primary Argon
Secondary Not appl icable
Flow , cfh
Primary 65
Secondary Not a p p l i c a b l e
Power
Amps 6 00
Volts 35
Kilowatt 21
Powder Feeder
Type Plasmadyne Roto-Feed 1000
Gear set A
Meter wheel Not applicable
Feed Screw Not a p p l i c a b l e
Vibration amplitude N ot applicable
RPM 80
Powder gas flow , cfh 12
Coating Data
Spray rate , lb/hr 6

149

I
—

- - V .
-
- V -
~~~~~~~
- — --- V - V - V -
 _-V _ __ V V-VV_VV V VVV
~ ~ ~~~~~ ~_ V — — - — —- — .. V -—
~~~~ ~_ . V ~~~~~ _ V _ . . . r .

PLASMA SPRAY DATA SHEET-- 15

Spray Ma terial Nickel—Aluminum

Composi ti o n Aluminum 4 . 5 % , Nickel 95.5%
Size range , microns -88 + 44

Spray Gun V

Type Plas m adyne SG lB

Nozzle Sl— 3-F
Powder por t Not a pp l i c a b l e
Gun-to-work distance , inches 4
Gas
Primary A rgon
Seconda ry Not applicable
Flow , cfh
Primary 60
Secondary Not a pp l i c a b l e
Power
Amps 500
Volts 30
Kilowa tt 15
Powder Feeder
Type Plasmadyne Roto-Feed 1000
Gear set A
Meter wheel Not appl icable
Feed Screw Not applicable
Vibration am plitude N ot applicable
RPM 55
Powder gas flow , cfh 13
Coating Data
Spray rate , lb/hr 6

150

V .
— -
 ~~~~~V~~~~~~~~ V
_ _ _ _

~~~ V~~~~~~V V~~~~~

_ _

V
V
PLASMA SPRAY DATA SHEET-- 16

Spray Material N ickel Chromium

Composition N i c k e l 80 % , Chromium 20 %
Size range , micro ns —105 +44

Spray Gun
Type Plasmadyne SG lB
Nozzle S1—3—F
Powde r port No t appl icable
Gun-to-work distance , inches 4
Gas
Primary Argo n
Secondary No t applicable
Flow , cfh
Primary 60
Secondary Not a pp l i c a b l e
Power
Amp s 450
Volts 30
Kilowatt 13.5
Powder Feeder
Type Plasmadyne Roto-Feed 1000
Gear set A
Meter wheel Not applicable
Feed Screw Not appl i cable
Vibration amplitude Not applicable
RPM 50
Powder gas flow , cfh 13
C o a t i n g Data
Spray rate , lb/hr 7

151

- ~~~~~~~~~~~~~~~~~ V~
- -
r ~~~~~~~~~~~~~~~~~~~~~~~~~~~ — -- - -- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ -~~~~~~ - - ——------ —-—

PLASMA SPRAY DATA SHEET-- 17

Spray Material Aluxnina-Titania

Composition A 12 O 3 87% , Ti0 2 13%
Size range, microns -53 + 15

Spray Gun
Type Metco 3B
Nozzle GH
Powder port # 2
Gun- to—work distance , inches 5
Gas
Primary Argon
Secondary Hydro gen
Flow , cfh
Primary 80
Secondary 25
Power
Amps 500
Volts 74
Kilowa tt 37
Powder Feeder
Type 3MP H

Gear set Not applicable

Meter wheel S
Feed Screw No t a p pl icable
Vibration amp litude Not applicable
RPM 45
Powder gas flow , c f h 37
Coating Data
Spray rate , lb/hr 3

152
 __ V_V
- ~V V
~~~~ V_ V V
~~ V-V -- —

PLASMA SPRAY DATA SHEET-- 18

Spray Material Chromium Oxide

Composi t ion Cr 2 03 99.0%
Size ra nge , mic rons -140 + 10

Spray Gun
Type Metco 3MB
Nozzle GH
Powder port #2
Gun-to-work distance , inches 4
Gas
Primary Argon
Secondary Hydro gen
Flow , c f h
Primary 80
Secondary 15
Power
Amps 500
Volts 65
Kilowatt 32.5
Powder Feeder
Type 3MP
Gear set Not appl icable
Mete r wheel S
Feed Screw Not ap p l i c a b l e
Vibration amplitude Not a p p l i c a b l e
RPM 30
Powder gas flow , cfh 37
Coating Data
Spray rate , lb/hr 3

153

V ~~~~~~~~~~~~~~~~~~~ - V
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
 V
VV
V — ~~~~~~~~~~~~~~~~~~~~~~ -V V
- -—- - VV V
~~~~~~~~~~~~~~~~ ~~~~~~~~~
V V

PLASMA SPRAY DATA SHEET-- 19

Spray Material Nickel-Alum inum

Composition Nickel 95.5% , Aluminum 4 . 5 %
Size range , microns -90 + 40

Spray Gun
Type Me tco 3MB
Nozzle GH
Powder port #2
Gun-to—work distance , inches 5
Gas
Primary Ar gor.
Secondary Hydro g en
Flow , c f h
Primary 80
Secondary 15
Powe r
Amps 500
Volts 65
Kilowa tt 32 . 5
Powder Feeder
Type 3MP
Gear set Not applicable
Meter wheel S
Feed Screw N o t appl icable
Vibration ampil tude Not appl icable
RPM 40
-Powder gas flow , cfh 37
Coat ing Data
Spray rate , lb/hr 3

154

V ~~~ T V
V ~~~~~~~~~~~~~~~~~~~~~~~~~~~ - —- - - - -
V
______ ~~~~~~~~~~~~~~ V - V --

VV
PLASMA SPRAY DATA SHEET-- 20

Spray Material N ickel Chromium

Composition N i c k e l 80% , Chromium 2 0%
Size rang e , microns -105 + 45

Spray Gu n
Type Metco 3MB
N ozzle GH
Powder port #2
Gun—to—work distance , i n c h e s 5
Gas
Pr i m a r y Argo n
Secondary Hydrogen
Flow , cfh
Primary 100
Secondary 5
Power
Amps 400
Volts 60
Kilowatt 24
Powder Feede r
Type 3MP
Gear set Not applicable
Meter wheel S
Feed Screw No t a pp l i c a b l e
Vibration amplitude Not app l i c a b l e
RPM 40
Powde r ga s flow , c f h 37
Coating Data
Spray rate , lb/hr 4

155

- -V
V
- - V V
- - V _ V V V VV
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ _V _ _ V _-V -V-V

PLASMA SPRAY DATA SHEET-- 21

Spray Material Molybdenum

Composition 99.0%
Size r ange , microns —7 0 + 30

Spray Gun
Type Metco 3MB
Nozzle GH
Powder port #2
Gun-to-work distance , inches 5
Gas
Primary A rgon
Secondary Hydro gen
Flow , cfh
Primary 80
Secondary 15
Power
Amps 500
Volts 65
Kilowatt 32.5
Powder Feeder
Type 3MP
Gear set Not appl icable
Meter wheel S
Feed Screw Not applicable
Vibration amplitude Not applicable
RPM 45
Powder gas flow , cfh 37
Coating Data
Spray rate , lb/hr 3-1/2

156

- -~~~~~ -‘ . - - -~~~~~~ ~~~~~~~~~~~~~~

 PLASMA SPRAY DATA SHEET-- 22

Spray Material Alumina-Titania

Composition A 12 O 3 87% , TiO 2 13%
Size range , microns —5 3 V
-r 15

Spray Gun
Type Metco 38
Nozzle G
Powder p o r t #2
Gun-to-work distance , inches 5
Gas
Primary Nitrogen
Secondary Hydrogen
Flow , c f h
Primary 75
Secondary 15
Power
Amps 5 00
Volts 76
Kilowatt 38
Powder Feeder
Type 3M P
Gear set Not applicable
Meter wheel S
Feed Screw Not a p p l i c a b l e
Vibration amplitude No t applicable
RPM 24
Powder gas flow , cfh 37
Coating Data
Spray rate , lb/hr 3

157

-
~~~~~~ ~~~~~~~~~~~~~~ —~~~~~~~~~ -— — -~~~~~~
V
V
~~~~~~~~~~~~~~~~~~~~~~~~~
 V - V V ----VV- -— --—

PLASMA SPRAY DATA SHEET-- 23

Spray Material Chromium Oxide

Composition Cr 2 03 99.0%
Size range , microns -74 + 10

Spray Gun
Type Metco 3MB
Nozzle G
Powder port #2
Gun-to-work distance , inches 4
Gas
Primary Ni trogen
Secondary Hydrogen
Flow , c f h
Primary 75
Secondary 15
Power
Amps 500
Volts 76
Kilowatt 38
Powder Feeder
Type 3MP
Gear set Not a p p li c a b l e
Meter wheel S
Feed Screw Not applicable
Vibration amplitude Not applicable
RPM 45
Powder gas flow , cfh 37
Coating Data
Spray rate , lb/hr 5

158

—— ~~~~~~~~~~~~~~~ _~~~~_ ~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~ -

- -
r -V ~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~

PLASMA SPRAY DATA SHEET-- 24

Spray Material N ickel Aluminum

Composition Aluminum 4.5% , Nickel 9 5 . 5 %
S i z e r a n ge , microns -88 + 44

Spray Gun
Type Metco 3MB
Nozzle G
Powder port #2
Gun-to-work distance , inches
~
Gas
Primary N it r o g e n
Second a r y Hydrogen
Flow , c f h
Primary 80
Secondary 15
Powe r
Amps 5 00
Volts 65
Kilowatt 32 .5
Powder Feeder
Type 3MP
Gear set Not applicable
M e t e r wheel S
Feed Screw Not applicable
Vibration amplitude Not applicable
RPM 15
Powder gas flow , cfh 37
Coating Data
Spray rate , lb/hr 5

159

V
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ _ _ _ _
-
 ~~~~~~-V~~~ - V V V V~~~~~~~~~~~~~~~V V~~~~~~~~V

V
V
PLASMA SPRAY DATA SHEET--2’

Spray Material N ickel Chromium

Composition N i c k e l 80 % , Chromium 20 %
Size ra ng e , m icrons -105 + 45

Spray Gun
Type Metco 3MB
Nozzle G
Powder port # 1
Gun-to-work distance , inches 6
Gas
Primary Nit rogen
V
Secondary Hydrogen
Flow , c f h
P r i m a ry ioo
Secondary 15
Powe r
Amps 400
Volts 74
Kilowatt 29.6
Powder Feeder
Type 3MP
Gear set No t appl icable
Meter wheel S
Feed Screw No t a ppl i cable
Vibration amplitude Not applicable
RPM 45
Powder gas flow , cfh 37
Coating Data
Spray ra te , lb/hr 5

I
160

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UNCLASSIFIED
‘ ECU fII TY C L A S S I F I C A T I O N OF THIS PAGE (m,.n Dat. Enhir.d) ____________________________________

DEDt DT F I I I uEk V F A T I f l K I DA ( E READ INSTRU CTIONS

,
~“ “,~~~- “ “ ‘~~“ ‘ “~ BEFORE COMPLETING FORM
L V R P VQR.T MUMB ER 2. GOVT ACCESSION NO 3. RECIPIENT S C A T A L O G NUMB ER

I) MT-O43l~ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _

4 T(T L-E ( . , d S U b f f l. lT_ _ _ V _ _ V

- — --
j -
. i. tVWioc RIPOI~T e~~~~~~ob ;ov ~~~to
/ 7
,

A PLASMA FLAME SPRAY HANDBOOK’ Final ~ eport .

/
-
6 TPI Ma OAG. REPORT NV1IIPER
~
~~~ N-00197-73-C-4630 J -‘- -

- V _V ~~~~~ V
— ‘f ’ I CQ~I~ I.AGT * *~~~1
-
I “ T. J .7Roseberry ~_t1 F. W .1,~ ou1ger WR—3-5961
— V~~~~~~~ VV V
(Battelle Memorial Institute)

B- P ER F O R M I N G O R G A N I Z A T I O N NAM E AND ADD R ESS ~O. PROG RAM ELEM ENT. PROJECT , TA l K
A R I A S WO RK UNIT N U M B E R S
Battelle Columbus Laboratories \
505 King Avenue
Columbus , Ohio 43201 _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _

II. C O N T R O L L I NG O F F I C E NAME AND ADDRESS -

Naval Sea Systems Command Mareh 1977

Department of the Navy . Manufacturing Tech- 1
~~~ NUME ~~W~~~~ PAGES
V

nology B r . (SEA-0354) , Washington , D . C . 20382 164

14 . MONITORING AGENCY NAME & A D O R E S S (i t dtU.rwt from Co,itro iling OUlca) IS. S E C URI T Y CLASS. (of hi. r.porf)

Naval Ordnance Station (CC 8~~~~

- Unclassified
Southside Drive / -/ V “-
/
/

- -
_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _

Louisville , Ky. 40214 _ I[ IS. . ~~~~~~~~~~~~~~ I IC A TI O N/ O OW NG RA D I N O

/
1 5. D I S T R I B U T I O N S T A T E M E N T (of thu R.por l)

Approved for Public Release - Distribution Unlimited

17. i ift.rwt frao, R.port)

D I S T R I B U T I O N S T A T E M E N T (of Ih. ab.Iract .nt. r.d in Block 20 , i ~

IS SUPPLEMENTARY NOTES

IS. K E Y WORDS (Continua , Vn ror. ,.. aid. hlnac•awv arid id.nhufy by block nuai b.r)

Plasma , Metal Spraying , Flame Spraying, Thermal Spraying , Handbook ,

Powder Spraying , Spraying , Buildup , Repairing , Overhaul

20. AB S T RA C T (ConlI ni~. on r.~ •ra• aid. If n.c...aiv id i d.ntify by blocb nimib.,)

The Plasma Spraying process is a versatile fabrication technique used to

apply a wide range of coatings on various workpiece materials. Coatings are
applied to restore or attai n desired dimensions • to provide el ectrical or thermal
shielding (or conduction) , or to improve the resistance to abrasion , corrosion ,
or high temperatures . Success in meeting intended goals by Plasma Spraying
depends on selecting an appropriate coating material and using cleaning and
(Continued on reverse)

DD 2
~~ ~~~~
I 1473 EDITION OF I NOV El IS OBSOLETE UNCLASSIFIE D
S/N 0102.LF.014.6601
183 SECURITY CLAU I?I CATION OF YNIS. III(
PAGE D~~.
,

_ ~~~~ ‘
~~~
V/

II

- ~~~~~~~~~ — -V
-- ~~~ V - V . - -~~~~~~~~~ . -- —---- -~~~~~ - -—--- - - -
 UN C LASSIF IED
SECU R ITy C L A S S I F I C A T I O N F .
i
!
~ IS P A G E (Wh ai Data EnI•r.d)

spraying techniques suitable for the materials involved . Thi s report provides
usefu l , up-to -date info rmation about Plasma Spraying both metallic and non-
metallic coatings on steel and bronze . It discusses the principles and details
the procedures suitable for producing high-quality coatings destined for severe
service applications of interest to the U. S. Navy .

This handbook should be considered a guide , not a bible , for planners ,

designers , and production personnel responsible for choosing , applying , and
evaluating plasma-arc sprayed coatings . Limitations on space and reliable
information , and the variety of types and applications of coatings , prevented
covering some aspects of plasma spraying in detail . For such reasons ,
differences in the types of p lasma-spray system s used successfully , limiting
coatin g thickness , and effects of specific part geometries are not covered
comprehensively . Most of the information in the handbook is directed to
engineers overseeing and developing expertise in plasma-arc spraying .

The handbook is based on experience , published information • and experi-

mental data generated on this program . The experimental work was conducted
with seven typ es of coatings deposited on the following types of work piece
materials:

Aluminum Low-carbon steel

Alumi n um bronze 316 stainless steel .
K-Monel

UNCLASSIFIED
SECURITY CLASSIFICATION Or’T HIS PAOE(W ~ .n Data int .,a4~
164

_ _ _ _ _ _ _ _ _ _ _
- - • -V -- V --V