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Materials Today: Proceedings 2 (2015) 2654 – 2665

4th International Conference on Materials Processing and Characterization

Tribological and Corrosion behavior of HVOF Sprayed WC-Co,

NiCrBSi and Cr3C2-NiCr Coatings and analysis using Design of
Experiments
Shabanaa*,M.M.M. Sarcar b, K.N.S.Sumanc,S Kamaluddind
a*
Assistant Professor, Department of Industrial Engineering, GIT, GITAM University, Visakhapatnam, Andhra Pradesh, India.
b
Professor , Department of Mechanical Engineering, Andhra University, Visakhapatnam, Andhra Pradesh, India..
c
Assistant Professor, Department of Mechanical Engineering, Andhra University, Visakhapatnam, Andhra Pradesh, India.
d
Professor, Department of Mechanical Engineering, GIT, GITAM University, Visakhapatnam, Andhra Pradesh, India.

Abstract

This paper contributes to the evaluation of wear and corrosion resistance of the three types thermally sprayed cermet
coatings deposited by High Velocity Oxygen Fuel (HVOF) spraying. In this paper, three different commercial powders
agglomerated and sintered WC-12%Co, Cr3C2-25%NiCr (80-20) and gas atomized NiCrBSi a self fluxing alloy were thermally
sprayed to deposit coatings onto mild steel substrates. The tribological tests concerned with the sliding wear behavior of the
coated samples were performed using Pin on Disk apparatus and were analysed by Response Surface Methodology (RSM). To
develop a wear model of coatings three factors temperature, load, sliding distance were used. ANOVA was carried out to
determine the significant factors and interactions..The wear resistance of these coatings at room temperature and at 350 0C were
compared. The corrosion test was performed for which the specimens were tested in 3.5%Nacl aqueous solution with P H adjusted
to 10 by adding potassium hydroxide and the polarization curves were obtained using the Potentiodynamic polarization system of
GILL AC units. The property of the coatings such as adhesion was measured with the pull-off test method according toASTMC-
633-01 standard, micro hardness. Deposition morphology and microstructure of coatings were studied using optical and electron
microscopy. These measured mechanical properties were discussed with the microstructures of the coatings using electron
microscopy, EDAX and X-ray diffraction. NiCrBSi is the best wear and corrosion resistant at room temperatures and WC-Co is
best at a temperature of 3500C.
© 2014Elsevier
© 2015 The Authors.
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Selectionand
Selection andpeer-review
peer-review under
under responsibility
responsibility of theofconference
the conference committee
committee members
members of the 4thofInternational
the 4th International
conferenceconference
on Materialson
Materials Processing
Processing and Characterization.
and Characterization.
Corresponding author. Tel.: 91-8895430160
E-mail address: shabana_farhat@yahoo.co.in

2214-7853 © 2015 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of the conference committee members of the 4th International conference on Materials Processing
and Characterization.
doi:10.1016/j.matpr.2015.07.227
 Shabana et al. / Materials Today: Proceedings 2 (2015) 2654 – 2665 2655

Keywords:Thermally sprayed coatings; HVOF; wear; friction; corrosion; SEM; WC-Co; NiCrBSi; Cr3C2-NiCr.

1. Introduction:

Wide range of thermal sprayed coatings applied in the basic industries with different combinations of coating
substrate material are used for applying protective coatings to material surfaces as no other technology of coating
deposition offers. HVOF is one of such technologies, which involves the deposition of molten or semi-molten
droplets of powder onto a substrate to form a coating [1]. It is found that this technique forms coatings with very
small porosity (<2 %) and high adhesion strength (> 80 MPa) [2, 3, 4]. Recently this coating technique is often
considered as a best alternate for the replacement of traditional electrolytic hard chrome (EHC) plating which
pollutes the environment and has serious environmental and health concerns causes lung cancer by toxic hexa-valent
Cr6+ [5]. The HVOF sprayed WC-based cermet hard coatings such as WC–Co, WC–Co–Cr have been investigated
for obtaining the coatings of high hardness, wear resistance, thermal stability and corrosion resistance [5, 6]. Ni–Cr
and other additives such as B, Si, W, Fe, and Mo can also be applied to protect steel articles [7]. The tribological
properties of part surfaces like wear, frictional force at the room and at higher temperatures is a serious problem
occurring in many of the machine components like aircraft, automobile and metallurgical industries. One of the most
serious problems of industries is corrosion which causes damage in billions of dollars each year. Materials are very
often exposed to environments wherein the metallurgical reaction between the environment and the materials that
are corrosive can affect the lifetime of the components and produce high maintenance costs [8,9].
Here, an attempt was made to find a coating by selecting the tungsten and chromium based cermets. The
mechanical properties like bond strength, hardness and the tribological properties like wear resistance and frictional
force at room temperature and at 3500C, were tested. And simultaneously the corrosion behaviour is also evaluated.
Coating characterization of the powders was also considered for discussion.
2.1 Substrate preparation:
Substrate selected for the application of the coatings was mild steel. Roughness of substrates prior to
HVOF deposition is required, as a means of improving the mechanical bonding of the coating, the substrate material
was cleaned with isopropyl alcohol followed by grit blasting with coarse Al2O3-24mesh.
2.2 Coatings Evaluated:
Tungsten carbide and chromium carbide-based coatings are frequently used in various industrial fields such
as the steel industry and aerospace industry for improving the resistance to wear and corrosion [10-16]. WC-Co
cermets are extensively used in wear resistance applications. These cermets provide a wide range of mechanical and
physical properties with the combination of hard and brittle WC phase and ductile cobalt phase in different
proportions. NiCrBSi a self fluxing alloy is applied extensively in numerous applications, both because of their
outstanding wear and corrosion resistance at high temperatures and is considerably available at relatively low cost
[17–19]. So, for the present work three commercially available powders WC-Co, NiCrBSi and Cr3C2-NiCr were
chosen for comparison at room temperature and at 3500C. The details of these thermally sprayed powders are as
presented in table 1.
Table 1 Powder Characteristics

Powder name Manufacturer Powder Thickness of the

size(μm) coating
WC-12%Co C&M Technologies -38/10 150 to 170 μm
NiCrBSi ISN Diffusion -53/15 150 to 170 μm
Cr3C2-25%NiCr H.C. Starck -45/10 150 to 170 μm
2656 Shabana et al. / Materials Today: Proceedings 2 (2015) 2654 – 2665

2.3 Coating Application:

These powders were sprayed onto the mild steel substrates selecting the spray parameters as tabulated in
table 2 using the gas fueled HVOF process. The powders were sprayed by using DJ2700 gun Metalizing Equipment
Corporation private limited (MEC), Jodhpur.
Table 2Process parameters
Gun DJ2700
Fuel LPG
Spray distance 6 to 8inches
Oxygen flow rate 200-300
Powder feed 25-38 gm/min
Deposition Efficiency 60-70%
Traverse rate (m/sec): 0.0028-0.0030 m/sec

2.4 Coating Characterization

2.4.1 Microhardness:
To determine the basic properties of coatings the micro hardness of the coated samples at their cross sections
were measured using a calibrated Vickers micro indentation hardness indenter, under a test load of 50 grams , dwell
time 15 s,indenter speed of 60μm/sec, and the angle between two faces is maintained as 136 0. The reported values
are averages of 5 measurements.
2.4.2 Adhesion:
Adhesion of coatings was evaluated by pull-off test according to ASTM C-633-01 Standard with the help
Universal Adapter for Attaching Bond Test Specimens to Tensile Test Equipment. The bond strength of the bonding
agent is defined each time this examination method is executed.
2.4.3 Microstructural Evaluation:
The coating characterization included optical microscopy of metallographically prepared cross-sections
where the porosity was measured. and the insight of the coating into the substrate was observed to be very secure
and as pictured in figure 1.
2.4.4 Sliding Wear Test:
The wear test on the coated samples (pins) was done using the Pin-on-Disc apparatus (DucomTribometer)
as per the ASTM G99 standard. A disc of EN-31with Ø160 mm x 12mm thickness was taken as a standard
counterpart. The coated samples of pins of size Ø10mm is tested at a load of 20N and 30 N, run at a velocity of 1000
RPM, for a distance of 15Km were tested at room temperature and at 3500C.
2.4.5 Design of Experiment (DOE):
In literature mostly the wear analysis has been done by varying a single factor. In the present work an
approach that takes the interaction effects of the all factors that influence the wear into consideration are evaluated.
Design of Experiments and Response surface Methodology has been used to find the interaction effects of factors on
sliding wear of the three coatings.
As discussed in reference (20) the most significant factors that affect wear are grain size, hardness, sliding distance,
temperature, spray parameters and spray systems (21) etc. The factors considered in the present work are Sliding
Distance, Temperature and Load. The parameter distance is taken as continuous variable, temperature and load as
discrete variables. The experimental design matrix for different runs is shown in table 3. A user defined quadratic
model is designed using DOE and RSM is chosen to find the relationship between the response function and
variables using the statistical software package Design Expert Software 9 (Stat Ease, Inc., and Minneapolis, USA).
 Shabana et al. / Materials Today: Proceedings 2 (2015) 2654 – 2665 2657

The interaction between the variables and the ANNOVA has been studied using RSM. The quality of the fit of this
model is expressed with the coefficient of determination R2.

Table 3: The design table along with response for coatings WC-Co, NiCrBSi, Cr3C2-NiCr

Std Run Sling Distance(A) Load(B) Temperature(C) Response( Wear )

0
m N C μm
WC-Co NiCrBSi Cr3C2-NiCr
12 1 5[-1] 20[-1] 350[1] 2.28 205.83 18.18
3 2 5[-1] 20[-1] 40[-1] 28.74 9.63 0.08
4 3 5[-1] 30[1] 350[1] 68.49 58.72 17.15
7 4 5[-1] 30[1] 40[-1] 26.19 5.98 28.65
15 5 3753.75[-0.33] 20[-1] 350[1] 60 1051.98 11.52
19 6 3753.75[-0.33] 20[-1] 40[-1] 51.23 19.25 13.73
8 7 3753.75[-0.33] 30[1] 350[1] 220.8 295.62 414.2
1 8 3753.75[-0.33] 30[1] 40[-1] 60.3 16.45 51.47
9 9 7502.5[0] 20[-1] 350[1] 340 1057.29 57.67
13 10 7502.5[0] 20[-1] 40[-1] 56.59 19.61 21.84
16 11 7502.5[0] 30[1] 40[-1] 61.32 18.57 54.9
10 12 7502.5[0] 30[1] 350[1] 358.94 930.6 543.83
14 13 11251.25[0.33] 20[-1] 350[1] 340 1113.57 61.32
17 14 11251.25[0.33] 20[-1] 40[-1] 57.33 20.15 38.16
5 15 11251.25[0.33] 30[1] 350[1] 358.94 1193.99 816.62
11 16 11251.25[0.33] 30[1] 40[-1] 61.5 19.78 56.11
2 17 15000[1] 20[-1] 40[-1] 57.77 21.46 58.42
20 18 15000[1] 20[-1] 350[1] 500.68 1152.9 41.63
18 19 15000[1] 30[1] 350[1] 549.68 1192.22 1307.26
6 20 15000[1] 30[1] 40[-1] 61.38 20.54 58

The factors and their levels considered under this study are tabulated in table 4
Table 4: Various factors and their levels used in Sliding wear behavior study.
Factor Name Units Type Subtype Lower Upper Std. Dev.
Level Level
A Distance m Numeric Continuous 5(-1) 15000(1) 5346.273
Traversed
B Load N Numeric Discrete 2(-1) 3(1) 0.504219
0
C Temp C Numeric Discrete 40(-1) 350(1) 156.308

2.4.6 Response Surface Methodology:

2658 Shabana et al. / Materials Today: Proceedings 2 (2015) 2654 – 2665

Response Surface Methodology (RSM) with three levels of each factor was used in the present study. The
factors were designated as A (distance traversed, m), B (load, N) and C (temperature, 0C) respectively. The coded
values of upper, middle, and lower levels of each factor are designated by +1, 0, and -1 respectively. The coded
values of various factors and response wear for 3 coatings under consideration used in the present study are shown
in Table 3.
3. Corrosion behaviour of the coated specimens:
Metal corrosion occurs via electrochemical reactions at the interface between the metal and an electrolyte
solution. Here the pitting corrosion test was done by using GILL AC unit.
3.1 Potentiodynamic polarization tests:
A software based PAR weld electrochemical system of the GILL AC unit was used to conduct the
potentiodynamic polarization tests for studying the pitting corrosion behaviour of coated steel surfaces. A saturated
calomel electrode (SCE) and carbon electrode were used as reference and auxiliary electrodes respectively. All
experiments were conducted in aerated 3.5% NaCl solution with PH adjusted to 10 by adding potassium hydroxide.
The potential scan was carried out at 0.166 mVs-1with the initial potential of –0.25 V (OC) SCE to the final pitting
potential. The exposure area for these experiments was 1 cm2. The potential at which anodic and cathodic current is
equal was considered to be the corrosion E corr. The specimens exhibiting relatively more positive potential (or less
negative potentials) were seen to have better pitting corrosion resistance.
4. Results and discussion:
From the above experimentation the mechanical properties of the three coatings are tabulated in table 5. It
is observed that all these properties like adhesive strength, microhardness and porosity exhibited by WC- Co are
superior.

Table 5 Mechanical properties

Coating Bond strength (N/mm2) Porosity Hardness (HV 50)

WC-12%Co 79.22 0.855 1293

NiCrBSi 58.15 0.922 997

Cr2C3-25%NiCr 78.90 1.4946 1081

The microstructures in the fig.1 showed that there is very good penetration of the coating into the substrate.
For all the 3 coatings the porosity was less than 2%, which are generally acceptable.

Fig.1. Micro structure of (a) WC-Co (b) NiCrBSi (c) Cr3C2-NiCr

 Shabana et al. / Materials Today: Proceedings 2 (2015) 2654 – 2665 2659

Cross sectional images of SEM exhibit that the coatings are compact and without defects and
cracks. The concentration and distributions of elements in the interface between the coating and substrate were
analyzed by energy dispersed X-ray analysis (EDAX) provided in figures 2 & 3.As seen in figure 2 (a) the SEM
image shows the white flakes represent the tungsten flakes showing the hexagonal crystallographic structure which
increases the hardness of the coating. But in the case of NiCrBSi in figure 2 (b)as the hardness was low, the grain
size is very big and the particle size varied in several hundreds of micrometers very slight initiation of the cracks is
observed. The Cr3C2-NiCr flakes are relatively bigger in size and darker well distributed in the matrix of Ni and Cr
as in figure 2 (c).

Fig.2 SEM (a) WC-Co (b) NiCrBSi (c) Cr3C2-NiCr

Fig. 3 EDAX (a) WC-Co (b) NiCrBSi (c) Cr3C2-NiCr

In WC-Co it is observed that the structure was more uniform without any appreciable appearance of
porosity/oxides/ decomposition/decarburization and also the cohesion is superior due to interlocking of carbides in
the cobalt matrix. The adhesion is better because of good surface preparation of the substrate.
The various compounds formed in the powders are tested with X-ray Diffraction (XRD).
2660 Shabana et al. / Materials Today: Proceedings 2 (2015) 2654 – 2665

Fig. 4 XRD (a) WC-Co (b) NiCrBSi (c) Cr3C2-NiCr

From the XRD of WC-Co as in figure 4(a) the peaks of WC are of high intensity and some dissolved peaks
of Co are also observed. From figure 4(b) the new compounds formed are very much suitable for high corrosion
resistance and in 4(c) the highest intensity peaks observed are of Ni, Cr and Cr3C2 which are very much suitable for
excellent wear resistance at higher temperatures.
The interaction graphs obtained by using the ANOVA are as shown below in figures 5,6&7.

Figure 5 (a) Graphs showing variation of wear with respect to single parameter for WC-Co

Figure 5 (b) 3D graphs showingthe interaction effect of different parameters, for WC-Co
 Shabana et al. / Materials Today: Proceedings 2 (2015) 2654 – 2665 2661

Figure 6(a) Graphs showing the variation of wear with respect to single parameter for NiCrBSi Coating

Figure 6(b) 3D graphs showing the interaction effect of different parameters for NiCrBsi Coating

Figure 7(a) Graphs showing variation of wear with respect to single parameter for Cr 3C2-NiCr
2662 Shabana et al. / Materials Today: Proceedings 2 (2015) 2654 – 2665

Figure 7 (b) 3D graphs showing the interaction effect of different parameters for Cr 3C2-NiCr
From the model graphs it has been analysed that Cr 3C2-NiCr exhibited superior wear resistance at high loads,
temperatures to the other two coatings.

Table 6 ANOVA of WC-Co Coating

Std. Dev. 41.49 R-Squared 0.9611
Mean 166.11 Adj R-Squared 0.9432
C.V.% 24.98 Pred R-Squared 0.9286
PRESS 41112.02 Adeq Precision 21.928
The "Pred R-Squared" of 0.9286 is in reasonable agreement with the "Adj R-Squared" of 0.9432.
Table 7 ANOVA of NiCrBSi Coating
Std. Dev. 155.73 R-Squared 0.9429
Mean 421.21 Adj R-Squared 0.9096
C.V.% 36.97 Pred R-Squared 0.8257
PRESS 8.882E+005 Adeq Precision 14.396

The "Pred R-Squared" of 0.8257 is in reasonable agreement with the "Adj R-Squared" of 0.9096

Table 8 ANOVA of Cr3C2-NiCr Coating

Std. Dev. 140.71 R-Squared 0.8972
Mean 233.36 Adj R-Squared 0.8498
C.V.% 60.30 Pred R-Squared 0.6597
PRESS 8.522E+005 Adeq Precision 14.492

The "Pred R-Squared" of 0.6597 is in reasonable agreement with the "Adj R-Squared" of 0.8498

Wear Model for WC-Co:

Coded form
‡ƒ” ൌ ͳ͸͹Ǥͻͷ ൅ ͳʹ͹ǤͶͻ ൅ ͳͺǤͶͻ ൅ ͳͳͷǤ͹ͳ െ ͸Ǥ͸Ͳ ൅ ͳͳ͵Ǥͻʹ ൅ ͳ͸Ǥͷͺ൅‫( א‬Eq 1)
Uncoded form:
‡ƒ” ൌ ͳ͹ǤͲͷ͵ͻͻ ൅ ʹǤʹͻʹͺ ൈ ͳͲିଷ  ൅ ͺǤͶ͸ͳͺͶ െ ͲǤͷʹ͵ͺͷ െ ͳǤ͹͸ͳ͵ͻ ൈ ͳͲିଷ  ൅ ͻǤͺͲʹ͹ ൈ ͳͲିହ  ൅
ͲǤʹͳ͵ͻ͹൅‫( א‬Eq 2)
Wear Model for NiCrBSi:
Coded form
‡ƒ” ൌ ͷͲͺǤ͸Ͷͺͺ ൅ ʹͷͺǤͻͲͷͷ െ ͶͷǤͻ͸ ൅ ͶͲͶǤͲ͸ͷ ൅ ͸ͲǤͺ͹͸ͷ ൅ ʹͷ͵ǤʹͲͶͷ െ ͶͷǤͲͺʹ െ
ͳ͹ͶǤͺͺͶଶ ൅‫( א‬Eq 3)
Un coded Form:
‡ƒ” ൌ ʹʹ͵Ǥ͵ͷͶʹͲ െ ͲǤͲͶͺͷͷ͵ െ ͳͲͲǤ͵ʹʹͲ ൅ ʹǤͶʹ͸Ͷ͸ ൅ ͲǤͲͳ͸ʹ͵ͻ ൅ ʹǤͳ͹ͺͺ͵ ൈ ͳͲିସ  െ
ͲǤͷͺͳ͹Ͳ൅‫(א‬Eq 4)

Wear Model for Cr3C2-NiCr:

Coded form

‡ƒ” ൌ ͳͺ͵ǤͷͶ െ ͳ͸ͶǤͳͻ ൅ ͳͷͳǤʹͺ ൅ ͳͶͷǤͶͲ ൅ ͳͶͲǤͶͳ ൅ ͳͶ͵Ǥ͹Ͷ ൅ ͳ͵ͻǤͷͻ൅‫א‬

 Shabana et al. / Materials Today: Proceedings 2 (2015) 2654 – 2665 2663

(Eq 5) Uncoded form

‡ƒ” ൌ ͺͶͳǤͶͷͶͲͳ െ ͲǤͲͻͷͺͷͺ െ ͵ʹǤͻ͸͹ͳͺ െ ͶǤͶͻʹͻͲ ൅ ͵Ǥ͹ͶͷͶͺͳͲିଷ  ൅ ͳǤʹ͵͸ͻʹ ൈ ͳͲିସ  ൅
ͲǤͳͺͲͳʹ൅‫( א‬Eq 6)

The polarization curves of the deposited coatings obtained from the Gill Ac Electrochemical System are as
shown in figure 8. In this the NiCrBSi coating exhibited relatively more positive potential (or less negative
potentials) to have better pitting corrosion resistance. Cr3C2-NiCr showed little better positive potential and then
WC-Co was the least corrosion resistance.

Fig 8. Polarization curves of the deposited coatings

The parameters of the polarization curve are as presented in table 4.

Table 9 Parameter values of the corrosion test in 3.5%NaCl solution

Coating Corrosion potential Ucorr (mV) Current density Icorr(mA/cm2)

88WC-12Co -552 3.5

NiCrBSi -283 0.075
75Cr3C2-25NiCr -496 0.4

5. Conclusions:
Investigation of the three cermet coatings WC-12Co, NiCrBSi and Cr3C2-25NiCr has been measured and
characterized for tribologicalbehavior at room temperature and 3500C. The mechanical and corrosion properties are
also analyzed. HVOF thermal spraying process was applied for depositing the three cermet coatings.
1. Microstructural examination and evaluation of properties showed that the three coatings are dense (porosity
less than 2%), packed in and without defects and fractures.
2664 Shabana et al. / Materials Today: Proceedings 2 (2015) 2654 – 2665

2. As the temperature and load are increased Cr3C2-NiCr exhibited excellent wear resistances.
3. Corrosion test was conducted in aerated 3.5% NaCl solution revealed that the corrosion resistance of the
NiCrBSi was little higher than of the Cr 3C2-NiCr, WC-Co exhibited inferior corrosion properties.
4. This better corrosion behavior is influenced by the chemical composition differences of the metallic matrix.
5. It may be advised to prefer Cr3C2-NiCr for application where corrosion and wear are of prime concern.
Acknowledgement:
The authors thank DMRL, Hyderabad for giving us permission to carry on our tests for SEM, EDAX and
XRD. Thanks to VTC, Visakhapatnam for coating the samples needed for the experimentation.

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