Who is Buehler?

Buehler is a premier manufacturer of scientific

equipment

Metallographic preparation
• Sectioning
• Mounting
• Grinding & Polishing

Imaging and Analysis

• Imaging software
• Image analysis suite
• Nikon microscopes

Hardness Testing
• Hardness Testing Software
• Full range of hardness testing equipment

Buehler also provides expert applications and technical

support.
 Stainless Steels Preparation
• Relatively straightforward to prepare:
Solution annealed austenitic and fully ferritic stainless
steels are the most difficult to prepare.

• Prone to mechanical damage during sectioning and grinding.

• Properties are characterised by the form and quantity of

phases present

• Etchant selection critical – resistant to many chemicals

Microhardness indent performed on a surgical blade, HV10gf 747 @
26µm from blade tip.
• Sub-surface deformation from grinding and polishing can
interfere with etching
Select the correct blade for your material
For mixed hardness/material samples, match hardest material

Minimize contact area through blade selection and clamping

Clamp sample securely – the leading cause of blade breakage!

Use equipment functions to improve speed and quality - SmartCut,

Pulse, Orbital

Look after your coolant system

Minimize contact area by selecting thin blades!

Mounting Considerations
Deburr edges to ensure specimen sits flat (least grinding)

Clean/degrease specimen prior to mounting (prevent gaps)

Select mounting material that:

• Retains specimen edge = faster preparation and more accurate results
• Grinds at the same rate as your sample = best flatness
• Has low shrinkage = minimize contamination & easy etching
Cool mount fully and under pressure (hot mounting – prevent gaps)

Bevel specimen corners (can increase cloth life)

Hot mounting presses have a high initial outlay, but the “per specimen”
consumable cost is much lower
Grinding/Polishing Core Concepts
Minimize sectioning damage for faster, more efficient preparation
Use an appropriate initial grinding stage
Understand how your grinding surface works – and use appropriately
Get advice to optimise methodology
Flat, high removal rate surfaces for intermediate stages
Softer surface just for final finish, and limited times
Educate users to:
Maintain good housekeeping
Know, and use, the recommended processes
Recognise problems (such as cloth wear)
Establish a good system of work in the laboratory – and keep to it

A “right first time” approach is usually the most economical.....

 Preparation Methods for Stainless and Maraging Steels
Force
(Per Specimen – Platen Speed Head Speed Relative
Step No. Surface Abrasive Lubricant/ Extender 30mm) Time (min:sec) (rpm) (rpm) Rotation
120-320 grit
1 CarbiMet Water 6lb (27N) 0:40 250rpm 60rpm
(P120-P400)

2 UltraPad 9µm Metadi Supreme Metadi fluid 6lb (27N) 5:00 150rpm 60rpm

3 Trident 3µm Metadi Supreme Metadi fluid 6lb (27N) 3:00 150rpm 60rpm

Optional Trident 1µm Metadi Supreme Metadi fluid 6lb (27N) 3:00 150rpm 60rpm

MasterPrep Water
4 ChemoMet 6lb (27N) 2:00 100rpm 60rpm
Alumina (for last 20s)

Vibratory polishing can help!

Typically 20-60 minutes greatly improves etching

results for tough samples
George Vander Voort
Principal of Vander Voort Consulting LLC
Consultant to Buehler Ltd.
- Graduate of Drexel and Lehigh Universities.
- 29 years’ experience in the steel industry
- Past President of the International Metallographic Society
- Past Chairman of ASTM Committee E-4 on Metallography

• 447 publications, 6 patents, 457 lectures in 42 countries, a video

course, and 8 ASTM standards.
• He has taught 277 seminars and courses and has received 36
awards in metallography contests.
• He was a trustee for ASM International and is on the editorial
boards of 4 journals
• He is a Fellow of ASTM International, ASM International and the
International Federation of Heat Treatment and Surface
Engineers.
• He is a Fellow and Honorary Life Member of Alpha Sigma Mu
metallurgy and materials science honorary society and an
honorary member of the Polish Society for Stereology.

In 2020, he was named a Distinguished Life Member of ASMI

Where did the Term “Stainless” Steel Come From?
Harry Brearley (left) of Sheffield, England
has been credited as the one who invented
“rustless” steel in 1912, although there
were several earlier attempts by others.
His first grade was a martensitic stainless
steel with 12.8% Cr. Also in 1912, Benno
Strauss and Eduard Mauer of Krupp in
Germany patented the first austenitic
stainless steel called Nirosta. Brearley’s
martensitic stainless steel was marketed
as “Staybrite”. The cutlery manager of
Mosley’s was the first to call it “stainless”
due to his tests using vinegar, which did
not cause staining.
Carl Zapffe, Author of 2nd Book on Stainless Steel

Carl Zapffe, author of “Stainless Steel – The

Miracle Metal”, published by the American
Society for Metals in 1960, wrote:

“Starting from rust, men have produced

something which looks like platinum and
resists chemical attack like gold, and yet a
square inch can support a quarter of a million
pounds….this is the crowning achievement of
metallurgy.”
 History of Development of Stainless Steel Types
● Martensitic stainless steels – Besides Harry Brearley in 1912, Elwood Haynes
applied for a US Patent in 1912 for a martensitic stainless steel.

● Austenitic stainless steels – On 17 October 1912, a German patent by Krupp

engineers Benno Strauss and Eduard Mauer was filed for Nirosta. Dr. W.H. Hatfield
was credited with the invention of 18/8 SS in 1924.

● Ferritic stainless steels were introduced in the US at that time by Christian

Dantsizen and Frederick Becket.

● PH stainless steels were developed after WW II.

● Duplex stainless steels were introduced starting in the 1970s.

● Development of stainless steels began in 1798!

316L Stainless Steel Cloud Gate Sculpture in Chicago!

The “bean” was designed and used 316L stainless

steel by Anish Kapoor (Feb 2004 to May 2006)
Commonly Used Etchants for Stainless Steels
15 mL HCl Glyceregia. Mix fresh; do not store. Good for about
10 mL glycerol 20 minutes. Use by swabbing. General purpose etch.
5 mL HNO3
15 mL HCl Acetic glyceregia, stronger than glyceregia. Mix
10 mL Acetic acid fresh; do not store. Good for about 20 minutes.
5 mL HNO3
1 - 2 drops glycerol
General purpose etch.
15 mL HCl Mixed acids, for the more corrosion-resistant grades;
10 mL Acetic acid e.g., Alloy 625. Mix fresh; do not store. Good for 30
10 mL HNO3
minutes. General purpose etch.
5 g CuCl2 Waterless Kalling’s reagent (Kalling’s # 2). This
100 mL HCl reagent can be made as a stock solution. Good grain
100 mL ethanol
boundary etch.

The first three etchants are commonly applied by swabbing with light pressure
using surgical-grade cotton balls; Kalling’s can be used by swabbing or by
immersion.
Beraha’s Color Etchants Based on HCl and K2S2O5
Ingredients B0 BI BII BIII BIV BV

HCl (%) in H2O 0.6 16.7 33.3 40 50 66.7

NH4FHF* 0 2 4 5 5 2-10

K2S2O5* 1 0.1-0.6 0.3-0.8 0.3-1.0 0.3-0.8 0.6-1.0

Na2S** 0 0 0.1-0.25 0.1-0.25 0 0

CuCl2** 0 0 0 1 1 1

FeCl3** 0 0 0 0 1-1.5 1-3

• *Amount per 100 mL ** Optional additions, amount per 100 mL

• BI through BIII work for Stainless Steels (low to high Cr)
 Beraha’s Sulfamic Acid Etchants
Reagent H2O K2S2O5 NH2SO3H NH4FHF
mL g g g

1 100 3 1 0

2 100 6 2 0

3 100 3 2 0

4 100 3 1 0.5 - 1

1 is basic solution for cast iron, carbon and alloy steels. 2 and 3 are faster acting. 4 is for martensitic
stainless steel, Mn steels, and tool steels.
 Ralph’s Reagent
50 mL Water
50 mL Ethanol
50 mL Methanol
50 mL HCl
1 g CuCl2
3.5 g FeCl3
2.5 mL Nitric Acid

Can mix and store a large bottle (keep out of the sun and keep at cool temperature (< 70 ºF)).

Use by swabbing or by immersion.

Commonly Observed Minor Second-Phase Precipitates
 M23C6 Carbide – FCC, (Cr16Fe5Mo2)C6 or (Fe,Cr)23C6 (mainly in SS)

 M6C Carbide – FCC (not commonly observed)

 M7C3 Carbide – Hexagonal, Cr7C3, (mainly in Martensitic SS)

 MC – Cubic, TiC or NbC

 Sigma () – Tetragonal, FeCr, FeMo, Fe(Cr, Mo) – Hard, brittle intermetallic
phase that reduces corrosion resistance and markedly reduces toughness and
ductility. It precipitates more readily from ferrite than from austenite.

 Chi () – BCC, (Fe, Ni)36Cr18Mo4 – It precipitates in ferrite more readily than in
austenite. Usually seen only in grades with  3% Mo.
 Martensitic Stainless Steels
FED-14 (Casting Grade)
Fe – 2.21% C – 0.92% Mn – 0.54% Si – 12.65% Cr – 0.3% Ni – 0.7% Mo – 0.11% V

100 µm 20 µm

Tempered martensite and extensive alloy carbide

networks in FED-14, 670HV, Beraha’s sulfamic
acid reagent No. 4.
 Martensitic Stainless Steels
FED-25 (Casting Grade)
Fe – 2.84% C – 0.67% Mn – 0.48% Si – 25.92% Cr – 0.21% Ni – 0.14% Mo

100 µm 20 µm

Tempered martensite and extensive alloy carbide

networks in FED-25, 643HV, Beraha’s sulfamic acid
reagent No. 4.
 Martensitic Stainless Steels
Wrought AISI 403
Fe - <0.15% C – 12.25% Cr - <0.6% Ni

25 µm 100 µm

Annealed Quenched and Tempered

Annealed (ferrite and carbides) and quenched and
tempered (tempered martensite) microstructures of
AISI 403; Vilella’s reagent.
 Martensitic Stainless Steels
AISI 410, 1900 °F/1038 ºC, Oil AISI 420 in the Quenched and
Quench, 1200 °F/650 º C Temper Tempered Condition

20 µm

Tempered martensite in 410 revealed using Tempered martensitic matrix and prior-
modified Fry’s reagent. austenite grain boundaries with Vilella’s
reagent. Image at 1000X.
 Martensitic Stainless Steels
AISI 420, Fe – 0.30% C – 0.42% Mn – 0.79% Si – 13.8% Cr – 0.27% Ni

Vilella’s Reagent Beraha’s Sulfamic Acid Reagent No. 4

Carbide networks have been a problem in large

sections of hardened (1038 °C/1900 º F, AC,
177 °C/350 ºF) AISI 420.
 Martensitic Stainless Steels
AISI 422, Fe – 0.22% C – 12.5% Cr – 0.75% Ni – 1% Mo – 1% W – 0.23% V

25 µm 25 µm

1900 °F/1038 ºC, AC, 500 °F/260 º C, AC, 1900 °F, AC, 1200 °F/650 ºC, AC, Wrought EF-
Wrought P/M AOD/ESR
Tempered martensitic microstructure of wrought P/M (left) and EF-AOD-ESR (right) 422 stainless etched with
Ralph’s reagent.
 Martensitic Stainless Steels
Wrought Annealed AISI 440C, Fe – 1.05% C – 17% Cr – <0.75% Mo

10 µm 10 µm

Annealed microstructure, ferrite and carbides, in 440C martensitic stainless steel. Excessive cold reduction
(wire drawing) will crack the larger Cr7C3 carbides (right). Villela’s reagent.
 Martensitic Stainless Steels
Wrought AISI 440C, Fe – 1.05% C – 17% Cr – <0.75% Mo

10 µm 10 µm 50 µm

1150 °C/2102 ºF, Oil Quench 1204 °C/2200 ºF, Oil Quench 1260 °C/2300 ºF, Oil Quench

Influence of excessive austenitizing temperature on the microstructure of 440C martensitic

stainless steel (Beraha’s sulfamic etch No. 4, polarized light plus sensitive tint).
 Ferritic Stainless Steels
AISI 409, Fe – <0.08% C – 11.2% Cr – 0.5% Ni + Ti

50 µm

Ferritic microstructure of 409 stainless steel Microstructure of ferritic P/M 409 stainless
sheet revealed using Vilella’s reagent steel that was not fully compacted. Note the
voids and oxides at grain boundaries and
within grains; Vilella’s reagent.
 Ferritic Stainless Steels
Monit®, Fe - <0.025% C – 25% Cr – 4% Ni – 4% Mo - <0.035N + Nb/Ta
Sea-Cure®, Fe - <0.025% C – 27.5% Cr – 1.2% Ni – 2.5% Mo - <0.025% N – 0.5% Ti

50 µm
20 µm

Ferritic grain structures of Monit and Sea-Cure revealed

by electrolytic etching, 60% HNO3 in water, 1 V dc, 60 s.
 Ferritic Stainless Steels
E-Brite® (26Cr-1Mo), Fe - <0.015% C – 26.25% Cr – 1.2% Mo - <0.015% N
29-4-2 FSS, Fe - <0.010% C – 29% Cr – 2.25% Ni – 3.7% Mo - <0.020% N

100 µm 100 µm

Left: Bi-modal grain-size distribution (longitudinal plane) in 26Cr-1Mo ferritic stainless steel. Right: uni-modal
distribution in 29-4-2 FSS. Both etched with 60% nitric acid in water, 1 V dc, 20 s.
 Austenitic Stainless Steels
Custom Flo 302-HQ, Fe - <0.08% C - <2% Mn – 18% Cr – 9% Ni – 3.5% Cu

200 µm 200 µm

302-HQ stainless steel tint etched with Beraha’s BII Solution annealed grain structure revealed
reagent, viewed with polarized light + sensitive tint. with waterless Kalling’s reagent, BF.
 Austenitic Stainless Steels
AISI 304, Fe - <0.08% C - <2% Mn - <1% Si – 19% Cr – 9.25% Ni

100 µm

Solution annealed 304 etched with Kalling’s Solution annealed (1038 °C/1900 ºF – 1 h, water quench)
No. 2 reagent (“waterless” Kalling’s),100X. and aged at 650 °C/1200 ºF for 2 h to sensitize the
specimen. Carbides were darkened by etching with
aqueous 10% ammonium persulfate, 6 V dc, 10 s.
 Austenitic Stainless Steels
316L Solution Annealed at 1750 °F/954 ºC, Fe - <0.03% C – 17% Cr – 12% Ni – 2.5% Mo

50 µm 50 µm

Kalling’s No. 2 Aqueous 60% HNO3, 1.5 V dc, 120 s Beraha’s BI tint etch

Austenitic grain size in solution annealed (1750 ºF/954 ºC) 316L using three different etchants. Waterless
Kalling’s did the poorest revelation while electrolytic 60% Nitric acid revealed nearly all of the grain
boundaries, but none of the twin boundaries. Beraha’s tint etch revealed the grain structure well – note the
delta ferrite stringer (red arrow).
 Austenitic Stainless Steels
316L Solution Annealed at 1750 °F/954 ºC

Aqueous 20% NaOH, 3 V dc, 10 s Concentrated NH4OH, 5 V dc, 10 s

Delta ferrite (left) and carbides (right) found along the centerline of this 316L stainless steel bar.
 Austenitic Stainless Steels
AISI 316 – As Cast, Fe - <0.08% C – 17% Cr – 12% Ni – 2.5% Mo

100 µm 20 µm

As-cast microstructure of 316 stainless contains more delta ferrite than seen after hot working due to
segregation during solidification. Glyceregia etch.
 Austenitic Stainless Steels
AISI 316 - Wrought

100 µm 100 µm

Acetic Glyceregia Marble’s Reagent

Two common etchants used to reveal the austenitic grain structure of 316 stainless steel.
 Austenitic Stainless Steels
AISI 316

100 µm
100 µm

HCl – HNO3 – H2O 10% Oxalic Acid, 6 V dc, 10 s

Two more common etchants used to reveal the austenitic grain structure of 316 stainless steel.
 Austenitic Stainless Steels
AISI 316

100 µm

Kalling’s No. 2 reagent (“waterless” Kalling’s) 60% HNO3 in H2O, 0.6 V dc, 90 s
These 6 etchants reveal the challenge in fully revealing the grain structure of austenitic stainless steels. Only
60% Nitric acid fully reveals all grain boundaries, but no twins!
 Austenitic Stainless Steels
AISI 316

100 µm

Tint etched with Beraha’s solution (15 mL Sensitized by aging at 1200 ºF/650 ºC for 2 h to
HCl – 85 mL water – 1 g K2S2O5). precipitate Cr23C6 carbide on the grain boundaries.
Etched with equal parts of HNO3, HCl and water.
Two different etchants/approaches to reveal the grain
structure in austenitic stainless steels.
 Austenitic Stainless Steels
AISI 321, Fe - <0.08% C – 18% Cr – 10.5% Ni + Ti

Bright Field Nomarski DIC

Delta ferrite stringers in an austenitic matrix (longitudinal plane) in solution annealed 321 stainless steel
(swab etched with 15 mL HCl – 10 mL acetic acid – 10 mL HNO3).
 Austenitic Stainless Steels
AISI 347, Fe - <0.08% C – 18% Cr – 11% Ni + Nb

100 µm 100 µm

5% Cold Reduction 10% Cold Reduction

Effect of % cold reduction of the bar diameter on the austenitic grain structure and slip deformation revealed
using 60% HNO3 at 4 V dc.
 Austenitic Stainless Steels
AISI 347, Fe - <0.08% C – 18% Cr – 11% Ni + Nb

100 µm 100 µm

15% Cold Reduction 30% Cold Reduction

Effect of cold reduction of the bar diameter on the austenitic grain structure and slip deformation revealed
using aqueous 60% HNO3 at 4 V dc.
 Austenitic Stainless Steels
22-13-5 (Nitronic 50), Fe - <0.06% C – 5% Mn – 22% Cr – 12.5% Ni – 2.25% Mo –
0.2% Nb – 0.2% V – 0.3% N

100 µm

Duplex grain size distribution in solution annealed 22-13-5 austenitic stainless steel etched with “waterless”
Kalling’s reagent.
 Austenitic Stainless Steels
SCF-19, Fe – 0.03% C – 5% Mn – 20% Cr – 18% Ni – 5% Mo – 0.35% N

100 µm

Necklace-type duplex grain size distribution in SCF-19 austenitic stainless steel that was cold reduced 10% in
thickness and solution annealed at a low temperature (900 °C – 1 h, water quench). Etched with aqueous 60%
HNO3, 1 V dc, 60 s.
1180 °C/2155 ºF is the recommended solution
annealing temperature.
 Austenitic Stainless Steels
18-18 Plus, Fe - <0.15%C – 18% Mn – 18% Cr – 1% Mo – 1% Cu – 0.5% N

100 µm 50 µm

Austenitic grain structure of 18-18 Plus, nitrogen-strengthened austenitic stainless steel etched with
Beraha’s BI reagent and viewed with polarized light and sensitive tint.
 Precipitation Hardenable Stainless Steels
AM 350, Fe – 0.09% C – 0.85% Mn – 16.5% Cr – 4.5% Ni – 2.85% Mo – 0.1% N

10 µm

AM350 in the solution annealed condition revealing delta Delta ferrite grains in a martensitic matrix
ferrite stringers (hot working axis is horizontal). Etched with observed on a transverse plane in AM 350;
aqueous 20% NaOH at 3 V dc, 5 sec. to color the delta ferrite modified Fry’s reagent.
(martensitic matrix).
 Precipitation Hardenable Stainless Steels
AM 350, Fe – 0.09% C – 0.85% Mn – 16.5% Cr – 4.5% Ni – 2.85% Mo – 0.1% N

50 µm 20 µm

Delta ferrite stringers in a martensitic matrix in AM 350 revealed using modified Fry’s reagent.
Longitudinal Plane
 Precipitation Hardenable Stainless Steels
17-4 PH, Fe - <0.07% C – 16.5% Cr – 4% Ni – 4% Cu – 0.3% Nb+Ta

20 µm 20 µm

Modified Fry’s Reagent Marble’s Reagent

Revealing the martensitic matrix and delta ferrite in 17-4PH stainless steel with two different
etchants.
 Precipitation Hardenable Stainless Steels
17-4 PH, Fe - <0.07% C – 16.5% Cr – 4% Ni – 4% Cu – 0.3% Nb+Ta

20 µm

Aqueous 20% NaOH, 20 V dc, 20 s Aqueous 10 N KOH, 2.5 V dc, 10 s

Selective etching of delta ferrite in 17-4PH stainless steel by electrolytic etching.
 Precipitation Hardenable Stainless Steels
17-4 PH, Fe - <0.07% C – 16.5% Cr – 4% Ni – 4% Cu – 0.3% Nb+Ta

Superpicral Murakami’s Reagent at 100 °C/212 ºF (200X)

Superpicral revealed the martensite, prior-austenite grain boundaries and delta ferrite while Murakami’s
reagent selectively darkens the delta ferrite.
 Precipitation Hardenable Stainless Steels
17-4 PH, Fe - <0.07% C – 16.5% Cr – 4% Ni – 4% Cu – 0.3% Nb+Ta

50 µm
100 µm 100 µm

Solution Annealed: 1900 °F and oil quenched Solution Anneal + 900 °F Age
Martensitic matrix of 17-4PH (left) solution annealed at 1900 °F and oil quenched, and (right) solution
annealed at 1900 °F/1038 ºC and aged at 900 °F/482 ºC. Etched with modified Fry’s reagent.
 Precipitation Hardenable Stainless Steels
PH13-8 Mo, Fe - <0.05% C – 12.75% Cr – 8% Ni – 2.25% Mo – 1.15% Al - <0.01% N

20 µm

Fracture toughness test specimen (96.8 ksi Tint etched with Beraha’s reagent (20 mL HCl
in plane-strain fracture toughness) etched – 80 mL water – 2 g NH4FHF – 1 g K2S2O5).
with modified Fry’s reagent. Original at 1000X.

Solution annealed and aged martensite in both.

 Precipitation Hardenable Stainless Steels
Custom 450, Fe - <0.05% C – 15% Cr – 6% Ni – 0.75% Mo – 1.5% Cu + Nb/Ta

10 µm 10 µm
25 µm

H850 Aging (400X) H1050 – 4 h Aging (1000X) H1150 Aging (1000X)

Ralph’s reagent Modified Fry’s Reagent Waterless Kalling’s Reagent

Tempered Martensite in Custom 450 PH Stainless Steel

(Hardness Decreases with Increasing Aging Temperature)
 Precipitation Hardenable Stainless Steels
Custom 455, Fe - <0.05% C – 11.75% Cr – 8.5% Ni – 1.2% – Ti 2% Cu – 0.3% Nb+Ta

10 µm 25 µm
50 µm

H850 Aging, 1000X 1525 °F – WQ, 950 °F – 4 h, AC, 200X 1525 °F – AC, 1100 °F – 4 h, AC,
Modified Fry’s reagent H950 Aging, Ralph’s Reagent 400X, H1100 Aging, Ralph’s Reagent

Tempered Martensite in Custom 455 PH Stainless Steel

(Hardness Decreases with Increasing Aging Temperature)
 18Ni250 Maraging Steel
Fe - <0.03% C – 18.5% Ni – 7.5% Co – 4.85% Mo – 0.4% Ti – 0.1% Al

50 µm 20 µm

Solution annealed and aged martensite in 18Ni250 etched with Fry’s reagent.
 18Ni300 Maraging Steel
Fe - <0.03% C – 18.50% Ni – 4.9% Mo – 8.75% Co – 0.65% Ti – 0.1% Al

Original at 500X Original at 1000X

Microstructure of 18Ni300 maraging steel in the solution annealed and aged condition, after etching with
modified Fry’s reagent, to reveal the substitutional martensite matrix.
 Duplex Stainless Steels
7-Mo PLUS, Fe - <0.03% C – 27.5% Cr – 4.5% Ni – 1.5% Mo – 0.25% N

50 µm 50 µm

Phase Boundaries Etched 15% HCl in Ethanol Ferrite Colored by Aqueous 20% NaOH, 3 V dc, 10 s
Ferrite-austenite grain structure of hot-rolled and annealed 7-Mo PLUS duplex stainless steel revealed
using two different etchants with different results. The NaOH etch darkens the ferrite which is much
better than the HCl etch where you cannot identify the phases.
 Duplex Stainless Steels
7-Mo PLUS, Fe - <0.03% C – 27.5% Cr – 4.5% Ni – 1.5% Mo – 0.25% N

Microstructure of 7-Mo PLUS duplex stainless steel etched with Beraha’s reagent (15 mL HCl – 85 mL water
– 1 g K2S2O5). Original at 200X. Ferrite is colored, while the austenite is unaffected.
 Duplex Stainless Steels – ASTM A890-4A
SAF Alloy 2205, Fe - <0.03% C - <0.8% Mn – 22% Cr – 5.25% Ni – 3% Mo – 0.15% N

50 µm

Solution annealed condition, etched with Solution annealed at 1200 ºC/2192 ºF, ferrite
aqueous 20% NaOH, 3 V dc, 12 sec to color colored using 20% NaOH, 3 V dc, 10 s.
the ferrite (austenite is white).
Duplex Stainless Steels - As-Cast ASTM A 890-5A
Fe – <0.03% C - <1.5% Mn - <1% Si – 25% Cr – 7% Ni – 4.5% Mo – 0.2% N

Etched with aqueous 20% NaOH (3 V dc, 10 Etched with LB1 (100 mL water – 20 g NH4FHF – 0.5g
sec). Original at 100X. Ferrite is colored K2S2O5). Original at 100X. Austenite is colored brown
brown and austenite is unaffected. and ferrite is unaffected. Because it is as-cast, the
are no annealing twins in the austenite.
Also know as SAF Alloy 2507
 Duplex Stainless Steels, As-Cast ASTM A 890-5A
Fe – <0.03% C - <1.5% Mn - <1% Si – 25% Cr – 7% Ni – 4.5% Mo – 0.2% N

200 µm 200 µm 200 µm

100 mL H2O – 10g NaOH – 10g 100 mL H2O – 20g NaOH – 20g 100 mL H2O – 30g NaOH – 30g
K3Fe(CN)6 – 90s K3Fe(CN)6 – 50s K3Fe(CN)6 – 10s

Influence of etch composition on etch time at 100 °C with standard Murakami’s (left) and two modified
versions of Murakami’s (center and right) to reveal the ferrite phase. Note the increased intensity of the
coloring of the ferrite (50X) (Also called SAF Alloy 2507).
Duplex Stainless Steels, As-Cast ASTM A 890-4A
Fe – <0.03% C - <1.5% Mn - <1% Si – 22.25% Cr – 5.5% Ni – 3% Mo - <1.0% Cu – 0.2% N

100 µm 100 µm

20% NaOH, 3 V dc, 10s Standard Murakami’s, near boiling

Ferrite colored in ASTM A 890-4A using (left) 20% NaOH, 3 V dc, 10 s and (right) with Murakami’s,
90-100 °C, 120 s (also called SAF Alloy 2205).
 Duplex Stainless Steels
As-Cast CD7MCuN, ASTM A890-1B, Fe ≤ 0.04% C ≤ 1.0% Mn ≤ 1.0% Si - 25.5% Cr –
5.65% Ni – 2.0% Mo – 3.0% Cu – 0.10 – 0.25% N

200 µm

Ferrite colored by modified (30-30-100) Murakami’s – 10 s at 90-100 C

Also known as Ferralium 255
 Formation of Undesirable Phases in Stainless Steels

20 µm

Sigma phase formed in a type 312 stainless steel weld (from the delta ferrite phase) by aging at 816 °C/1500 ºF
for 160 h. Sigma was colored orange by etching with Murakami’s reagent (10 g sodium hydroxide, 10 g
potassium ferricyanide, 100 mL water) for 60 s at 80 °C.
 Formation of Undesirable Phases in Stainless Steels

7-Mo was an unsuccessful

forerunner of 7-Mo Plus
developed by Carpenter
Technology Corporation. Its
composition was Fe < 0.1% C –
27.5% Cr – 4.5% Ni – 1.5% Mo.

10 µm

Microstructure of wrought 7-Mo duplex stainless steel solution annealed and aged 48 h at 816 °C/1500 ºF to
form sigma. Electrolytic etching with aqueous 20% NaOH (3 V dc, 10 s) revealed the ferrite as tan, the sigma
orange, while the austenite was not colored. The arrows point to new austenite produced as ferrite is
consumed forming sigma.
 Formation of Undesirable Phases in Stainless Steels
UNS 32760, Fe - ≤0.03% C - ≤1.0% Mn - ≤1.0% Si – 25% Cr – 7% Ni – 3.5% Mo – 0.75% Cu – 0.75% W – 0.25% N

20 µm 20 µm

Bright Field Nomarski DIC

“Sigmatized” Super Duplex Stainless Steel etched with 10% Oxalic Acid, 6 V dc, 10 s.
Formation of Undesirable Phases in Stainless Steels
SCF-23, Fe ≤ 0.02% C ≤ 4.25% Mn ≤ 0.45% Si – 22.75% Cr – 17.75% Ni – 5.5% Mo – 0.40% N

20 µm 10 µm

Chi phase formed in solution annealed SCF-23 aged at 1800 ºF/982 ºC for 24 h; etched in 15 mL
HCl – 10 mL HNO3 – 10 mL acetic acid.
 Formation of Undesirable Phases in Stainless Steels
SCF-23, Fe ≤ 0.02% C ≤ 4.25% Mn ≤ 0.45% Si – 22.75% Cr – 17.75% Ni – 5.5% Mo – 0.40% N

20 µm

Microstructure of SCF-23 stainless steel in the solution annealed condition after aging 48 h at 927 °C/1700 ºF
forming chi phase in the grain boundaries and within the grains. The chi particles were colored using
Murakami’s reagent (10 g sodium hydroxide, 10 g potassium ferricyanide, 100 mL water at 80 °C for 30 s).
 Formation of Undesirable Phases in Stainless Steels
As-Cast CD3MN, Fe - <0.03% C – 22.25% Cr – 5.5% Ni – 3% Mo – 0.2% N

As-cast CD3MN duplex stainless steel aged 30 days at 800 °C/1472 ºF after etching with Murakami’s reagent
for 40 s at 90 °C to color the ferrite tan. Austenite is white. The intermetallic phases are sigma and chi phases.
 Conclusions
● Stainless Steels are highly corrosion resistant alloys with 5 basic types.

● They are: Martensitic, Austenitic, Ferritic, Precipitation Hardened, Duplex.

● Grades are used as-cast, wrought or cold rolled. Close to 100 different grades
have been created.

● Many etchants have been created to reveal the general microstructures or

specific phases.

● When properly produced they can be used in service for many years, unless
thermal conditions change and they become embrittled.
 May Webinar
Etching and Microstructure Series:
Tool Steels

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