Sådhanå (2021)46:149 Ó Indian Academy of Sciences

https://doi.org/10.1007/s12046-021-01667-4
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Sensitivity analysis and optimisation of HVOF process inputs

to reduce porosity and maximise hardness of WC-10Co-4Cr coatings
RESMI V PRASAD1,* , R RAJESH2, D THIRUMALAIKUMARASAMY3, S VIGNESH4 and
S SREESABARI5
1
Department of Mechanical Engineering, Lourdes Matha College of Science and Technology, Affiliated to
Kerala Technological University, Thiruvananthapuram, India
2
Department of Mechanical Engineering, Rohini College of Engineering and Technology, Affiliated to Anna
University, Kanyakumari, Tamil Nadu, India
3
Department of Mechanical Engineering, Government College of Engineering, Bargur, Affiliated to Anna
University, Bargur, Tamil Nadu, India
4
Department of Manufacturing Engineering, Annamalai University, Chidambaram, Tamil Nadu, India
5
Department of Mechanical Engineering, University of Coimbra, Coimbra, Portugal
e-mail: resmivprasad@gmail.com; rajesh1576@yahoo.co.in; tkumarasamy412@gmail.com;
vignesh_phd@yahoo.co.in; sreesabaridec2006@gmail.com

MS received 4 November 2020; revised 27 February 2021; accepted 23 June 2021

Abstract. This paper aims at developing an empirical relation to predict the porosity and micro-hardness, by
means of High Velocity Oxy Fuel (HVOF) sprayed WC-10Co-4Cr coatings. For determining the coating
performance, process parameters such as flow rate of LPG fuel, flow rate of oxygen, spray distance, flow rate of
carrier gas and feed rate of the coating powder play a significant role. Five-factors, five-level central composite
rotatable design (CCD) was employed in this analysis to reduce the number of experiments by covering all
possible combinations of the process variables. A mathematical model was established to assess the porosity and
microhardness of the coatings including HVOF process parameters and the appropriateness of the model was
examined using analysis of variance. Using RSM, process parameter optimizations were conducted. The
coatings produced using optimized process variables had a minimum porosity level of 0.2 Vol. percentage and a
maximum hardness of 1325.26 HVx compared to other coatings. This has been confirmed by the developing
response graphs and also by plotting contours. The optimization of HVOF parameters using RSM, as well as the
correlation of spray variables with properties of the coating, enables the recognition of the framework of the
characteristics to attain the preferred consistency of WC-10Co-4Cr coatings. Analysis of Sensitivity is also
performed to determine the most significant process parameter for the HVOF operation.

Keywords. Analysis of variance; mathematical model; sensitivity analysis; optimization; empirical

relationship.

1. Introduction surface corrosion and wear. But, due to some environ-

Actually, coatings by means of thermal spray technology
have been found to be used in almost all types of industries,
namely, aerospace, automotive, gas turbine and steam tur-
bine engines, chemical, oil and gas [1, 2]. One of the
important applications of thermal spray coatings, in par-
ticular High velocity oxy fuel (HVOF) coatings, is to
enhance the resistance to surface wear and corrosion. The
most commonly used coatings, to serve this purpose, are the
HVOF developed cermet coatings. A few years ago, hard
Chromium coatings were used to improve the resistance to
mental problems, they got replaced by chromium- carbide
and tungsten carbide based coatings [3, 4]. Due to the high
speed and less temperature of the powder particles during
the HVOF process, the decarburization of the coating
material is very minimal. In addition, HVOF coatings
exhibit low porosity and high adhesion strength [5, 6]
tungsten carbide (WC) cermet coatings have been com-
monly used to prolong the serviceability of various
mechanical components that are subjected to abrasive wear
conditions, such as in vehicles, construction machinery,
mining and power generation systems, etc. [7]. WC-Co-Cr
is an excellent coating material for the battle against

*For correspondence
149 Page 2 of 23
abrasive wear owing to the combination of hard phase WC
particles and durable metallic matrix Co Cr.
Industries consider that in order to manufacture coatings
with high quality and optimum bond strength, based on
hard metal and carbide cermet, the most effective technique
is the HVOF process [8–10]. Subsequent changes in the
spraying process have resulted in significant improvements
in grain structure and the surface properties that were
required. The microstructural accuracy and the sprayed
coatings properties rely heavily on the thermal spray
parameters used [11, 12]. To ensure the best value of each
parameter, the effects of important spraying parameters can
be examined using the conventional approach by changing
a single variable at a time while keeping the remaining
variables at a non-changing level. This univariate method
has the drawback that since the effects of interactions
between the parameters are ignored, the best conditions
could not be achieved. If conventional approaches are used
to find the optimum conditions for a specific procedure, the
number of trial required are larger in number and hence
time consuming also. Analysing the effects of HVOF spray
parameters, namely oxygen flow rate, fuel flow rate, spray
distance, carrier gas flow rate and powder feed rate using
experiment design (DOE) that enables the main effects of
each parameter to be measured and clears the shortcomings
of customary methods of interaction effects between
parameters [13, 14].
Several researchers [15, 16] have proven that the effec-
tive usage of statistical design of experimental techniques
enables the application of analytical methods to integrate a
theoretical outlook in the issue of process optimization in
the HVOF spraying parameter. Response surface method-
ology (RSM) was used in various studies for the parameter
optimization of the thermal spray process [17, 18]. Few
literatures were focused on integrating DOE and mathe-
matical optimization techniques with thermal spraying
processes.
Fang et al [13] investigated the wear behavior impact of
HVOF process variables by depositing WC-CrC-Ni coat-
ings using Taguchi method. Oksa et al [19] examined dif-
ferent strategies for optimizing and characterizing HVOF
coatings and believed that there was a need for an in-depth
understanding of the spraying process, including precursor
materials, spraying processes, and particle-based interac-
tions, in order to achieve higher quality coatings with the
necessary properties and performance required for a
specific purpose. Mawdsley et al [20] carried out an
experimental study and a design of experiment statistically
to assess the influence on the hardness, thickness, and
permeability of plasma spray parameters. To compare the
empirical correlation between the control parameters and
the corresponding responses, they used regression analysis.
They suggested that minimum permeability and optimum
hardness cannot be reached simultaneously. Therefore,
their analysis was separately restricted to single thickness,
permeability, and hardness optimization of response. Lin
Sådhanå (2021)46:149
et al [21] examined the response surface methodology
(RSM) and Taguchi experiment design to compare the
empirical relation between the parameters of plasma
spraying technique and the percentage of oxidation. Using
analysis of variance (ANOVA) and confirmatory experi-
ments, they have attempted to validate their model. Also, in
terms of maximum oxidant percentage, their work did not
report the optimal factor combination. Ramachandran et al
[22] adapted the rotatable factorial design of RSM trials to
establish empirical relationships between plasma spraying
factors and mechanical properties. To systematically ana-
lyze the parametric effects on strength, porosity, hardness,
and bond strength also they applied the empirical models
established. The demonstration of the middle-level process
parameters selection (i.e., input power, primary gas flow
rate, stand-off distance, coating powder feed rate, and flow
rate of the carrier gas) ensures acceptable mechanical
properties. Weight factors were also considered to perform
multi-objective optimization equivalent for each answer,
but it is simpler. The literature survey found that the HVOF
process for depositing the WC-10Co-4Cr powder on
stainless steel was not properly used. Therefore, an effort
has been made to achieve the ideal condition of the spray
parameter for coating. Hardness and porosity were opti-
mized with RSM. In addition, the microstructural charac-
terization of the WC-10Co-4Cr coating developed by
different ways of processing conditions was made using
Energy dispersive X-ray spectroscopy (EDX), X-ray
diffraction (XRD), and scanning electron microscopy
(SEM) techniques. In addition, attempts were made to
correlate the hardness and porosity of the coating pro-
duced to the observed coating behavior. The sensitivity
of the process parameter and the calculation of the
incremental tuning specifications of those parameters in
coating deposition was the main focus of these investi-
gations. Current research has revealed substantial details
related to patterns in spraying parameters and optimal
coating conditions.
2. Experimental
For this research, the HVOF (HIPOJET-2700, Make:
Metallizing Equipment Co. Jodhpur, India) facility at the
Annamalai University, India, has been used to deposit WC-
10Co-4Cr (AMPERIT 507.074) powders on a steel sub-
strate of approximately 200 lm thickness. The coating
thickness was assessed using a digital micrometer (with
0.001 mm accurate) under every single condition. Four
times thickness for a single sample was measured and
finally achieved 200 micron coating thickness.
Before the HVOF process, surface preparation of the
substrate was done by degreasing and sandblasting methods
to improve coating adhesion to the base surface. The
parameters for sand blasting are jet pressure 2 bar, angle to
surface 80 degree and distance to surface 3 cm. The size of
Sådhanå (2021)46:149
the specimens used in this investigation is 15 mm 9 10 mm
9 8 mm, whose sides had a chamfer of 1 mm long and 45°.
These samples were cleaned through an ultrasonic cleaning
instrument using acetone. The surface roughness of the
substrate was enhanced using corundum, grit size of 320 ±
500 lm. The specifications of the grit are as follows: fused
Al2O3, morphology: blocky and sharp edged, density: 1.74
g/cm3 and hardness: 2.09 x 104 MPa. A surface roughness
tester (Make: Mitutoyo, Japan; Model: Surf test 301) was
used to measure the roughness of the surface. The average
surface roughness of the substrate after grit blasting was
8lm. The composition of conventional powders procured
from Metallizing Equipment Co, India is as follows: WC-
96 %, Co-10 %, and Cr-4%. The particle size range in the
powder is 15–45 lm. The process parameters of coatings
sprayed with HVOF are illustrated in table 1.
2.1 Coating characterization
In order to investigate the surface morphologies,
microstructural analysis of powders and coatings was
characterized using scanning microscopy (SEM) (Make:
JEOL, Japan; Model: 6410-LV). For the SEM micrograph
of the as-received powder with spherical morphology fig-
ures 1 (a-b) display a grain size range of -45 to ?15
lm. The small distribution of particle size and spherically
formed particles improve higher melting efficiency and
good flow capability. In figures 1 (c-d), the cross-sectional
scanning electron microscope micrographs of the coatings
are shown respectively.
The coating can be seen to be very thick and to have
close contact with the substrate. Because of the higher
velocity of HVOF spraying, this ensures the coating
includes a close to adhesion to the base. Usually, the
amount of porosity HVOF produces in the coating is very
small. Because of the high impact rate of the coating par-
ticles, individual splats are responsible for high density
associated with high cohesive strength.
Metallographic cross sections of the coatings were pre-
pared for the porosity measurements. The coated specimens
were first carefully cut to the specific dimensions using a
slow speed metallurgical sample saw (Make: Ducom, India;
Table 1. The parameters and levels of experiment.
Sl. No Variables Notations
1 Oxygen flow rate A 230
2 LPG flow rate B 40
3 Powder feed rate C 18
4 Spray distance D 180
5 Carrier gas flow rate E 9
Page 3 of 23 149
Model: MSS-10) equipped with resin bonded diamond
cutting disc. They were then mounted with low viscosity
epoxy resin under vacuum environment. The mounted
samples were successively ground with 600, 800, 1000 and
1500 grit SiC papers and eventually polished using dia-
mond slurries of 10-8, 8-5, 5-2, 2-0.5, 0.5-0 lm during 5, 5,
7, 10 and 10 min, respectively. Because of pullouts in
brittle materials, it is difficult to establish and evaluate true
porosity in a metallographically prepared spray coating. As
metallographic grinding and polishing, if not carried out
correctly, can introduce artifacts which are not part of the
coating structure. Ceramic coatings are brittle and particles
break out of the surface during grinding. If not polished
thoroughly, these breakouts leave an incorrect impression
of a high porosity. The optical microscope (Make: Meiji;
Japan, Model: MIL-7100) equipped with an image analysis
system (Metal Vison Version.6), according to ASTM B
276 [23], was used to measure the porosity on the metal-
lographically prepared cross sections of the coating. For
this study, images collected with an optical spectroscopy
below 1000 x were handpicked for porosity analysis to
view image attributes such as pores that are open and a
regular network of crack. Initially, a four hundred microns
square region was selected on the polished cross-section of
the coating and also the image was analyzed. The experi-
ment repeated at 5 different spots to conclude the average
percentage value of the amount of porosity. Microhardness
measurements were operated by indenting on the metallo-
graphic cross sections under 300 g load for 15 s using a
Vickers microhardness tester (Make: Shimadzu, Japan;
Model: HMV-2T). For each coating sample, the mea-
surement series comprised 20 random indentations.
Distance between indentations was kept three times
longer than the indentation diagonal to prevent the
effects of the stress field of nearby indentations. Using
the HV-5 Vickers hardness tester, the fracture strength of
the coatings was estimated using the indention cracking
method performed under a test load of 49 N on the
coatings’ cross section and a holding time of 15s and the
mean values of 20 readings have been taken as the
effectual fracture toughness values. The images obtai-
ned by means of image processing and measurements of
hardness were shown in figures 2 and 3.
Levels
-2 -1 0 1 2
235 240 245 250
45 50 55 60
24 30 36 42
200 220 240 260
11 13 15 17
149 Page 4 of 23
Figure 1. SEM micrographs and EDS analysis of WC-10Co-4Cr powder and coatings.
The coating bonding strength was analyzed follow-
ing the ASTMC-633-01 standard [24]. By using the E7 -
glue, the coatings sample was bonded to stainless steel 304.
The measurement was performed after solidification on a
universal tensile test equipment (Make: FIE Blue Star;
India, Model: UNITEK-94100). The equipment’s crosshead
speed was 1 mm/min.
2.2 Identifying important spray parameters
In experimental design, the first stage is to choose the
process parameters that come under the exploration. It’s
been usually accepted that within the thermal spray envi-
ronment, there are many parameters that will in the-
ory have an effect on the properties of the coating. All
Sådhanå (2021)46:149
potential variations of the parameters for economic (time
requirements) and theoretical (parameter interdependence)
reasons can’t be regulated. The prevailing factors that have
a greater influence on the coatings are selected according to
the literatures [13, 15–22] and the previous research carried
out in the laboratory [25]. They are the fuel flow rate, the
oxygen flow rate, the stand-off distance, the feed rate for
powder, and carrier gas flow rate. Trials were per-
formed to determine the feasible working ranges of HVOF
parameters.
2.3 Determining the parameter working limits
In order to decide the viable operating range of the above
variables, a significant number of spraying experiments
Sådhanå (2021)46:149 Page 5 of 23 149

minimise the number of trials. By adopting the following

guidelines, the operating range of HVOF spray parameters
was defined: the emergence of cracks and the coating lay-
ers’ separation, coating thickness formation per pass, sur-
face roughness of more than five lm, and deposition
performance of 45-70 %.
Several experiments have been conducted by altering the
parameters of the HVOF spray, and also the observations
noted throughout spraying are shown in the figure 4.
(i) If the oxygen flow rate comes under 240 lpm, less
fuel was burned because of lower particle temper-
ature (mainly related to the transfer of heat from the
gas to the powdered particles in flight) and a weak
fusion was caused. If the flow rate of oxygen was
greater than 260 lpm, the combustion of fuel was
under high melting conditions of the in-flight
particles, resulting in higher particle temperatures,
substrate gets overheated, and cracking (due to the
extinguishing stress during the solidification of the
individual splats, as the splats already bind to the
underlying material, the tensile stress develops
during the cooling process. The naked eye noticed
a higher porosity of the coating when the fuel flow
rate was under 50 lpm. If the fuel flow rate was
higher than 70 lpm, unmelted particles were
observed to rebound.
(ii) The effect was a poor microstructure, pores and
splat boundaries, if the spray distance was less than
Figure 2. Steps involved in image analysis; (a) Binary image of
the selected image. (b) Selection of area to be analyzed. (c) Color 200 mm. If the distance to the standoff was more
coded image after porosity analysis. than 260 mm, the solidification of the liquefied
particles was found.
(iii) If the feed rate of the powder was under 24 gpm,
were performed on 5 mm thick grit blasted 304 stainless solely a little quantity of material was injected and
steel substrate coupons by altering one of the HVOF also the coating was observed to have a lower
parameters and keeping the others unchanged. In this study, deposition. If the feed rate of the powder was higher
the aim of experimental design (DOE) was used to

Figure 3. Coating indentation images.

149 Page 6 of 23
Figure 4. Correlation graph (Porosity).
than 48 gpm, there were more un melted particles,
with few molten splats resulting in higher porosity.
(iv) If the carrier gas rate was less than 10 lpm, the
powder flow through the combustion gases would be
lower. When the flow rate of carrier gas reaches 14
lpm, the powder flows fastly through the combus-
tion gases that supply the powder with less dwelling
time, leading to poor melting of the powder [26].
Supported the above observations, the working
range for HVOF spray parameters was selected
and also the values are described in table 2.
2.4 Formulating the matrix of experimental design
Based on the above conditions, the possible operating limits of
the HVOF spray parameters are calculated in such some way
that the coating process ought to be carried out while not
inflicting substrate defects with smart adhesion to the coating.
So as to deduce the relation between important input factors
and one or more calculated responses, response surface
methodology is used. RSM is an optimization method used to
evaluate a process’s behavior and to work out the optimum set
of parameters for the input process. It is a mathematical
approach used to model and predict the input of the affected
response variables. Experimental design and optimization is
carried out using the ‘‘Design Expert Version 12’’ to predict
optimum parameters for low porosity and high hardness levels.
The range of individual variables was broad, with the option of
a five factor five level central composite rotatable design
matrix. The parameters identified for spraying and their levels
are shown in table 2. Table 3 displays 32 coded experimental
settings. The limits of HVOF parameters and their ranges were
outlined in order that porosity and hardness experiments could
be conducted without any difficulty. In order to minimise time
and cost, statistically designed experiments have been used to
explore the consequences of HVOF variables on responses.
Sådhanå (2021)46:149
The variables considered for the uncoated and coated 304 steel
with their ranges and mass loss are shown in tables 2 and 3.
Trials were performed randomly in this analysis to prevent the
method from infiltrating systemic errors. So as to verify
the reliability of the results, three experiments were con-
ducted for each experimental condition.
The linear (X), quadratic (X2), and two-way interactive
(XY) effects of the variables on the WC-10Co-4Cr sprayed
HVOF coatings will be calculated from the thirty two
experiments. The statistical significance of the predicted
full quadratic models was assessed through the analysis of
variance (ANOVA). The quadratic equations (Equa-
tion 2.1) were derived and given below, based on the
ANOVA analysis. As a consequence, micro-hardness and
porosity can be predicted for various formulations of
powder mixtures. The higher and lower values of the
variables are labeled ?2 and-2, respectively, for ease of
documentation and interpretation of test effects. We may
use the relationship to figure out the coded values of any
intermediate value as follows
Xi ¼ 2½2X  ðXmax þ Xmin Þ=ðXmax  Xmin Þ ð2:1Þ
where Xi = coded value needed for the X variable, X = any
variable value from Xmin to Xmax, Xmin=variable’s smaller
value, Xmax=larger value of the variable.
2.5 Build an empirical relation
In this experimental method, the relationship was calcu-
lated using the second- order polynomial equation between
the HVOF spray parameters and the obtained responses,
after analysis. It is computed as follows:
X X X
Y ¼ b0 þ bi x i þ bii x2i þ bij xi xj ð2:2Þ
where Y= predicted response, Xi, Xi2, Xij=variables in
coded values, b0=constant, bi= linear effect, bii= squared
effect, bij=interaction effect.
The responses porosity and microhardness are functions
of oxygen flow rate (A), LPG flow rate (B), powder feed
rate (C), spray distance (D), carrier gas flow rate (E) and it
can be expressed as
Responses ¼ f ðA; B; C; D; EÞ ð2:3Þ
For the five factors, the selected polynomial can be
expressed as
Y ¼ b0 þ b1 ð AÞ þ b2 ðBÞ þ b3 ðC Þ þ b4 ðDÞ þ b5 ðEÞ
   
þ b11 A2 þ b22 B2
     
þ b33 C 2 þ b44 D2 þ b55 E2 þ b12 ðABÞ
ð2:4Þ
þ b13 ðAC Þ þ b14 ðADÞ
þ b15 ðAEÞ þ b23 ðBC Þ þ b24 ðBDÞ þ b25 ðBEÞ
þ b34 ðCDÞ þ b35 ðCEÞ þ b45 ðCEÞ
Sådhanå (2021)46:149 Page 7 of 23 149

Table 2. The matrix of design and calculated responses.

Value coded Original value Reactions

Sl. No A B C D E A (lpm) B (lpm) C (gpm) D (mm) E (lpm) Porosity (Vol. %) Hardness (HVx)
1 -1 -1 -1 -1 1 235 45 24 200 15 1.73 826
2 1 -1 -1 -1 -1 245 45 24 200 11 0.79 1090
3 -1 1 -1 -1 -1 235 55 24 200 11 1.52 975
4 1 1 -1 -1 1 245 55 24 200 15 0.55 1224
5 -1 -1 1 -1 -1 235 45 36 200 11 1.66 835
6 1 -1 1 -1 1 245 45 36 200 15 1.45 878
7 -1 1 1 -1 1 235 55 36 200 15 0.68 1148
8 1 1 1 -1 -1 245 55 36 200 11 0.55 1213
9 -1 -1 -1 1 -1 235 45 24 240 11 1.33 900
10 1 -1 -1 1 1 245 45 24 240 15 0.25 1291
11 -1 1 -1 1 1 235 55 24 240 15 1.49 876
12 1 1 -1 1 -1 245 55 24 240 11 0.42 1221
13 -1 -1 1 1 1 235 45 36 240 15 2.05 756
14 1 -1 1 1 -1 245 45 36 240 11 1.93 772
15 -1 1 1 1 -1 235 55 36 240 11 2.1 803
16 1 1 1 1 1 245 55 36 240 15 0.7 1044
17 -2 0 0 0 0 230 50 30 220 13 2.02 805
18 2 0 0 0 0 250 50 30 220 13 0.45 1266
19 0 -2 0 0 0 240 40 30 220 13 2.04 797
20 0 2 0 0 0 240 60 30 220 13 1.3 1127
21 0 0 -2 0 0 240 50 18 220 13 0.48 1185
22 0 0 2 0 0 240 50 42 220 13 1.38 895
23 0 0 0 -2 0 240 50 30 180 13 0.75 1077
24 0 0 0 2 0 240 50 30 260 13 1.36 924
25 0 0 0 0 -2 240 50 30 220 9 0.58 1124
26 0 0 0 0 2 240 50 30 220 17 0.4 1203
27 0 0 0 0 0 240 50 30 220 13 0.47 1177
28 0 0 0 0 0 240 50 30 220 13 0.49 1168
29 0 0 0 0 0 240 50 30 220 13 0.5 1153
30 0 0 0 0 0 240 50 30 220 13 0.44 1187
31 0 0 0 0 0 240 50 30 220 13 0.41 1177
32 0 0 0 0 0 240 50 30 220 13 0.53 1159

where bo is an average of responses. The coefficients b1,
b2.........b45 depend on the parameters’ respective primary
and interactive effect. The tool used to calculate the
coefficients was the design expert software package
(version 12.0). The student t-test and p-values were
employed to determine the importance of each coefficient.
Analysis of variance (ANOVA) test was conducted to
classify significant factors. The results obtained are shown
in tables 4 and 5.
Final empirical relationships have been established using
these coefficients, including significant factors on their
own, and are given as follows
Coating porosity ðP1Þ ¼ ½0:48  0:38A  0:19B
: respectively. This implies that 99.51 percent and 99.46
þ 0:20C þ 0:11D  0:073E  0:076AB þ 0:14AC
0:089AD  0:005AE  0:18BC þ 0:093BD
ð2:5Þ
 0:059BE þ 0:22CD  0:082C
0:074DE þ 0:19A2 þ 0:29B2 þ 0:11C 2
þ 0:14D2  0:0068E2  vol: %
Coating Hardness ðHVx Þ ¼ ½1173:27 þ 105:67A
:
þ 75:67B  63:92C  34:67D þ 16:33E þ 11:63AB
55:25AC þ 23:25AD þ 3:00AE þ 48:62BC  44:12BD
 4:63BE  54:50CD þ 10:75CE þ 19:25DE
36:77A2  55:15B2  35:65C 2  45:52D2
 4:77E2  HV
ð2:6Þ
The terribly low likelihood value (P model [ F=0.0001)
obtained in the Fisher F-test suggests that the empirical
relationship regression model for predicting porosity and
hardness of very high significance. The R2 values for
porosity and hardness were found to be 0.9951 and 0.9946,
percent of the experimental results indicate an agreement
with the evidence expected by the established observational
relationship. The value of R2 is always between 0 and 1 and
its value means that the empirical relationships established
are suitable. The value of R2 should be close to 1.0 and it
149 Page 8 of 23 Sådhanå (2021)46:149

Table 3. Microstructural observations during HVOF coating trials.

Sådhanå (2021)46:149 Page 9 of 23 149

Table 3. continued
149 Page 10 of 23 Sådhanå (2021)46:149

Table 3. continued
Sådhanå (2021)46:149 Page 11 of 23 149

Table 3. continued
149 Page 12 of 23 Sådhanå (2021)46:149

Table 3. continued
Sådhanå (2021)46:149 Page 13 of 23 149

Table 3. continued

Table 4. ANOVA analysis.

Source Sum of squares Df Mean square F value p-value prob[ F

Model 11.76 20 0.59 112.47 \0.0001 Significant
A-Oxygen flow rate 3.42 1 3.42 654.07 \0.0001
B-LPG flow rate 0.90 1 0.90 173.04 \0.0001
C-Powder feed rate 0.98 1 0.98 186.66 \0.0001
D-Spray distance 0.27 1 0.27 52.22 \0.0001
E-Carrier gas flow rate composition 0.13 1 0.13 24.68 \0.0004
AB 0.093 1 0.093 17.79 \0.0014
AC 0.30 1 0.30 57.85 \0.0001
AD 0.13 1 0.13 24.10 \0.0005
AE 4.000 x 10-4 1 4.000 x 10-4 0.076 \0.7872
BC 0.54 1 0.54 103.31 \0.0001
BD 0.14 1 0.14 26.18 \0.0003
BE 0.055 1 0.055 10.56 \0.0077
CD 0.78 1 0.78 149.78 \0.0001
CE 0.11 1 0.11 20.83 \0.0008
DE 0.087 1 0.087 16.64 \0.0018
A2 1.01 1 1.01 193.17 \0.0001
B2 2.54 1 2.54 485.93 \0.0001
C2 0.35 1 0.35 67.04 \0.0001
D2 0.58 1 0.58 110.84 \0.0001
E2 1.364 x 10-5 1 1.365 x 10-5 2.608 x 10-3 \0.9602
Residual 0.058 11 5.229 x 10-3
Lack of Fit 0.048 6 8.031 x 10-3 4.30 0.0654 Not significant
Pure Error 9.33 x 10-3 5 1.867 x 10-3
Cor Total 11.82 31
149 Page 14 of 23 Sådhanå (2021)46:149

Table 5. ANOVA analysis.

Source Sum of squares Df Mean square F value p-value prob[ F

Model 9.081 x 105
20 45406.33 101.62 \0.0001 Significant
A-Oxygen flow rate 2.680 x 105 1 2.680 x105 599.73 \0.0001
B-LPG flow rate 1.374 x 105 1 1.374 x 105 307.53 \0.0001
C-Powder feed rate 98048.17 1 98048.17 219.44 \0.0001
D-Spray distance 28842.67 1 28842.67 64.55 \0.0001
E-Carrier gas flow rate composition 6402.67 1 6402.67 14.33 \0.0030
AB 2162.25 1 2162.25 4.84 \0.0501
AC 48841.00 1 48841.00 109.31 \0.0001
AD 8649.00 1 8649.00 19.36 \0.0011
AE 144.00 1 144.00 0.32 \0.5816
BC 37830.25 1 37830.25 84.67 \0.0001
BD 31152.25 1 31152.25 69.72 \0.0001
BE 342.25 1 342.25 0.77 \0.4002
CD 47524.00 1 47524.00 106.36 \0.0001
CE 1849.00 1 1849.00 4.14 \0.0668
DE 5929.00 1 5929.00 13.27 \0.0039
A2 39665.52 1 39665.52 88.77 \0.0001
B2 89210.64 1 89210.64 199.66 \0.0001
C2 37275.64 1 37275.64 83.42 \0.0001
D2 60788.02 1 60788.02 136.05 \0.0001
E2 668.18 1 668.18 1.50 \0.2469
Residual 4914.98 11 446.82
Lack of Fit 4114.15 6 685.69 4.28 0.0654 Not significant
Pure Error 800.83 5 160.17
Cor Total 9.130 x 105 31

3. Results and discussion

For this study, the porosity and hardness of the as sprayed

Figure 5. Correlation graph (Hardness).
means that the statistical model established are better.
It could be concluded from the figure that the straight
line’s residual fall showing the errors is normally dis-
tributed. Furthermore, as shown in figures 4 and 5,
each observed value corresponds well to its experi-
mental value.
coating have been decided on the numerical and graphical
optimization responses. Since the inverse association
between porosity and hardness has been well-developed in
thermal spray coating, to obtain an optimised condition, it
was taken to maximise the hardness and minimise the
degree of porosity. The optimal condition was reached by
imposing restrictions on contingent elements (hardness and
porosity) and on independent elements (oxygen flow rate,
fuel flow rate, powder feed rate, spray distance and carrier
gas flow rate). The degree of porosity of the coating was
anticipated and plotted on the basis of the produced
regression (Equation 2.5), as shown in figure 6.
To assess the effect of the operating parameters on
porosity and hardness, the three dimensional diagrams were
plotted against defined operating states. At about the same
time, visually searching for the best solution remains to
formulate the desirable values for both answers is con-
ceivable from the contour plot. This displayed from figure 7
that the porosity can be reduced by increasing process pa-
rameters including oxygen flow rate, flow rate for LPG,
feed rate for powder, spray distance and flow rate for carrier
gas. The response graph valley offers minimal porosity;
these graphical representation of responses are used for
predicting feedback (porosity) in any field. Proper
Sådhanå (2021)46:149
Figure 6. Perturbation plots.
combustion of LPG fuel and complete melting of the par-
ticles in the in-flight results in strong splat formation on the
substrate through the oxygen gas flow rate. The outcome is
low porosity and high resistance to bonding between the
surface of the coating and the base. The flame temperature
is also low when the LPG fuel is very low, and this con-
tributes to the poor particle melting of the coating. Once the
LPG fuel is just too significant or too high, it causes the
coating particles to oxidize. Oxygen gas and LPG flow
levels are important operational parameters and have an
influence on the in-flight particle that infers the consistency
of the coating.
In addition, with both oxygen and fuel flow, the porosity
of the coating has decreased. The upper oxygen rate and
also the LPG fuel rate induce higher particle velocity,
which results in enhanced pressure within the combustion
chamber and spread of the particle, and the degree of
contact is increased to extend the kinetic energy. With
Page 15 of 23 149
increased particle temperature, the porosity will decrease
and thus result in a denser microstructure. Similarly, coat-
ing hardness was plotted from regression (Equation 2.6), as
seen in figure 8. From figure 8, it is concluded that the
coating hardness increased to a peak level and then
decreased with the rise in factor levels. Maximum hardness
indicates the highest point of the response graph. The
influence of the powder feed rate to measure porosity and
hardness is related to the size of the spray. The quantity of
powder feed (C) is therefore directly proportional to the
porosity percentage and reciprocally proportional to the
hardness. Porosity at lower and higher rates maximises the
powder feed rate (C) and minimises the hardness due to
powder vaporisation and/or excessive melting. The feed
rate of the powder is correlated with heat transfer and
impact behaviour during spraying. Due to the high heat
energy obtained from the particles, a very small amount of
powder coating is pumped into the chamber, resulting in
ample particle melting and improvement of the good splat
formation, resulting in low porosity. By increasing the
powder feed rate, very high amounts of coating powder are
pumped into the chamber as a result of lower powder
temperatures and large unmelted particles. Owing to an
inadequate cooling rate, recrystallization occurs, thus
increasing the porosity of the coating. At an optimum feed
rate, the consistency of the coatings is high, so that most
particles are melted.
The thickness of the coating will quantitatively demon-
strate deposition quality. The thickness of the coating
decreases as the angle to the spray decreases. The shortest
distance of the spray causes microstructure defects, in
particular, splat edges, pores, etc. The velocity and tem-
perature of the powder particles can decide the properties of
the coating during HVOF spraying. As the particle velocity
increases, the kinetic energy of the inflight particles
decreases, and a change in the temperature of the particles
leads to a decrease in the particle velocity. Both result in a
decreased thickness of splat, and fast splashing. It is
ascertained that once the spray distance is reduced, the
porosity will increase considerably and also the hardness
decreases because of in-flight particle K.E. variations. For
the intermediate spray distance, a better suggestion was
introduced. Therefore, a multi-objective optimal approach
needs to be found where the criteria satisfy the desired
properties at the same time. In this way, there is a balance
between the conditions to be achieved for the two methods.
To attain such an objective, the multi-objective optimiza-
tion technique is used with a particular end target. Several
responses are found by graphical optimization. The super-
imposing or very crucial response contours are employed in
the contour plots to describe the regions that are feasible to
fulfill the proposed criteria. At that point, it is possible to
visually check for a better conciliation. It is suggested that
analytical optimization be at first conducted due to the
management of multiple responses; otherwise, it may be
difficult to determine the feasible region. Graphic
149 Page 16 of 23 Sådhanå (2021)46:149

Figure 7. Response graphs for coating porosity.

Sådhanå (2021)46:149 Page 17 of 23 149

Figure 8. Response graphs for coating hardness.

149 Page 18 of 23
Figure 9. Overlay plot.
Figure 10. Relationship graph between porosity and hardness of
coating.
optimization is usually seen in the field of feasible regions
in factor space. The regions that aren’t appropriate for the
optimization criterion will be shaded. The final stage was to
overlap the specified advisable areas of each response to
establish a locality of intrigue or a large plot. The overlay
patterns of reactions (porosity and hardness) are described
in figure 9 for the expected meanings. The light-reducing
shade remains for definitions of most hardness and mini-
mum porosity.
As shown in figure 10, the porosity of the coating and the
micro hardness resulting from the experimental results are
related. One straight line fits the experimental data points.
The straight line shall be plotted by the following
regression equation.
Micro - Hardness ðHVxÞ ¼ 266:65x
þ 1313:2 ðporosity in Vol %Þ
ð3:1Þ
Sådhanå (2021)46:149
The approximate regression equation’s slope (– 266.65)
is negative, meaning that microhardness increases as
porosity decreases. The determination coefficient is R2 =
95.8 percent. It can be represented by the approximate
regression equation as the percentage of the total sum of
squares that can be clarified. A fit-goodness estimate of the
expected regression equation [27] is the determination
coefficient R2.
For two purposes, the constructed regression line
(Equation 3.1) are often used:
To estimate the norm of the micro hardness given in
relation to the porosity of the coating
Predicting the individual value of micro hardness for a
given degree of porosity of the coating
The correctness of the results of the regression is shown
by the confidence interval (CI) and the probability interval
(PI). Smaller intervals offer a better degree of exactness
(figure 10). CI is anapproximate interval between the y’s
mean value and the x’s value. PI is an approximate indi-
vidual value interval of y for a given value of x. A point
estimate of the mean value of hardness is provided by the
derived regression equation for a given value of porosity.
The distinction between CI and PI is because of the actual
fact that it is possible to measure the mean value of hard-
ness more accurately than the individual hardness value.
The larger PI dimension reflects the additional uncertainty
generated by predicting a random variable value, rather
than estimating a mean value. This can be also inferred
from figure 11 that the closer the value to ‘‘X’’ (15.36 vol.
percent) the lower the range will be.
4. Validation
It is important to see whether or not the relationship formed
correctly predicts responses in the creation of empirical
relationships. The predictive capacity of the empirical
relationships formed was tested by conducting 3 further
experiments using spray process variables not defined in the
design matrix (table 2). The experimental and anticipated
outcomes were shown in tables 6 and table 7.
The expected values of porosity and hardness derived
from current relationships are consistent with the experi-
mental values and are within ±5 percent of the variance.
The HVOF tests were carried out with the proposed spray
parameters of the model in order to verify the findings by
computer modeling (suggested solutions), namely the
maintenance of the oxygen flow rate, LPG flow rate,
powder feed rate, spray distance, carrier gas flow rate at
246.2 lpm, 55.37 lpm, 24.86 g/min, 220.95 mm, 14 lpm.
Furthermore, above and below the optimized spraying
conditions, two separate sets of experiments were consid-
ered, and the results are described in table 7. From these
results, it is ascertained that deviations of spraying
Sådhanå (2021)46:149 Page 19 of 23 149

Figure 11. SEM micrograph of coating deposited using optimized HVOF spray condition.

Table 6. Validation results for proven empirical associations of sprayed HVOF coatings.

HVOF spray parameters Porosity (vol. %) Hardness (HV 0.3)

Carrier
Flow rate Fuel flow Feed rate Stand off gas flow
Exp. of oxygen rate of powder distance rate By By Variation By By Variation
no. (A) (lpm) (B) (lpm) (C) (gpm) (E) (mm) (F) (lpm) experiment model (%) experiment model (%)
1 254 64 35 235 13 0.78 0.79 ?3.88 1234 1286 ?4.08
2 252 65 40 232 14 0.83 0.79 -2.47 1199 1257 ?4.64
3 261 67 37 234 15 0.86 0.83 -4.74 1298 1290 -0.9

Table 7. Validation outcomes for HVOF sprayed coatings optimization process.

HVOF spray parameters

Coating Coating
Exp. Oxygen flow LPG flow rate Powder feed rate Spray distance Carrier gas flow porosity (vol. hardness (HV
no. rate (A) (lpm) (B) (lpm) 9 (C) (gpm) (D) (mm) rate (E) (lpm) %) 0.3)
1 256 59 31 225 13 0.329 1326
2 244 54 32 216 12 2.7 789
3 255 65 43 245 14 2.4 801

parameters from ideal conditions will lead to an increase in
coating porosity and decrease in coating hardness because
of inadequate and/or enthalpy from the flames to the
powder particles, variations in the residence time of particle
flame, and differences in the HVOF coating spray w has the
most effective surface finish compared to different thermal
spray processes. The plastic deformation of the unmelted
particles can be identified by the microstructure analysis.
This deformation leads to the rapid solidification of the
impinged droplets upon the specimen under investigation.
Coating powder with suitable particle size and optimized
process parameters can assist in the proper melting of the
flight particles. This is useful in achieving the efficient
creation of splat coating on the base surface. The coating
was deposited under optimized process conditions showed
less porosity and high hardness and can be seen
in figure 11.
5. Sensitivity analysis
The sensitivity analysis is that the initial and important
step within the optimization challenges. In relation to the
design parameter, it offers details on the proneness of the
design objective function to increase or decrease [28].
149 Page 20 of 23 Sådhanå (2021)46:149

Figure 12. Sensitivity analysis results, (A) Oxygen flow rate sensitivity of porosity, (B) LPG flow rate sensitivity of porosity,
(C) Stand-off distance sensitivity of porosity, (D) Powder feed rate sensitivity of porosity and (E) Carrier gas flow rate sensitivity of
porosity.

Analysis of sensitivity correctly plays an important role in
deciding which process parameter would be established for
feasible improvement. The sensitivity of a design objective
function to a design variable is a partial derivative of that
function to its variables, mathematically [29]. The sensi-
tivity equations for measuring porosity and hardness are
acquired by differentiating process parameters from the
above empirical relationships. Equations (2.5 and 2.6) are
distinguished by design parameters, including oxygen gas
flow rate (A), LPG flow rate (B), powder feed rate (C),
spray distance (D), and carrier gas flow rate (E), in order to
obtain sensitivity equations.
In equations (5.1), (5.2), (5.3), (5.4) and (5.5) respectively,
porosity sensitivities with respect to gas flow rate, LPG flow
rate, coating powder feed rate, spray distance and carrier gas
flow rate is specified. The sensitivity equations indicate ten-
dencies of porosity and hardness to be increased or
decreased regarding the changes in one of their process
parameters:
oP=oA ¼ 0:38A þ 0:14C  0:076B  0:089D  :38
 :005E
ð5:1Þ
Sådhanå (2021)46:149 Page 21 of 23 149

Figure 13. Sensitivity analysis results, (A) Oxygen flow rate sensitivity of hardness, (B) LPG flow rate sensitivity of hardness,
(C) Stand-off distance sensitivity of hardness, (D) Powder feed rate sensitivity of hardness and (E) Carrier gas flow rate sensitivity of
hardness.

oP=oB ¼ 0:58B þ 0:093D  0:076A  0:18C  0:19 oP=oE ¼ 0:073  0:005A  0:059B  0:082C  0:074D
 0:059E  0:0136E
ð5:2Þ ð5:5Þ

oP=oC ¼ 0:22C þ 0:14A þ 0:22D  0:18B  :20 Likewise the sensitivity equations. (5.6), (5.7), (5.8),
 0:082E ð5:3Þ (5.9), and (5.10) represent the sensitivity of hardness
for oxygen flow rate, LPG flow rate, powder feed rate,
oP=oD ¼ 0:28D þ 0:093B þ 0:22C  0:089A þ :11 standoff distance, and carrier gas flow rate,
 0:074E respectively.
ð5:4Þ
149 Page 22 of 23
oh=oA ¼ 105:67 þ 11:63B  55:25C þ 23:25D þ 3E
 73:54A
ð5:6Þ
oh=oB ¼ 75:67 þ 11:63A þ 48:62C  44:12D  4:63E
 110:3B
ð5:7Þ
oh=oC ¼ 63:92  55:25A þ 48:62B  54:5D  71:3C
þ 10:75E
ð5:8Þ
oh=oD ¼ 34:67 þ 23:25A  44:12B  54:50C  91:04D
þ 19:25E
ð5:9Þ
oh=oE ¼ 16:33 þ 3A  4:63B þ 10:75C þ 19:26D
 9:54E
ð5:10Þ
In this research, the objective is to predict the properties
of porosity and hardness because of a small modification in
process parameters for the HVOF process. The mathemat-
ical definition of derivatives can be used to interpret
knowledge of sensitivity. That is to say, positive sensitivity
values mean that the design parameter is slightly modified
to increase the objective function, while negative values
imply the opposite.
The porosity and hardness sensitivity maps of oxygen
gas flow rate, LPG flow rate, stand-off distance, powder
feed rate, & carrier gas flow rate are displayed in fig-
ures (12-13). The slight difference in the flow rate of
oxygen produces great differences in porosity and hardness.
The findings show that the porosity and hardness are more
prone to the flow rate of oxygen than the LPG flow rate,
standoff distance, powder feed rate, and carrier gas flow
rate.
6. Conclusions
i. Empirical relationships were formed from the
experimental data that can be used to analyze the
relationship between the variables of the HVOF
technique and the quality characteristics of the
coating, particularly the porosity and hardness of
WC-10Co-4Cr coatings using response surface
techniques.
ii. The most prevalent factor affecting the porosity and
hardness of the coatings was found to be oxygen flow
rate, followed by LPG flow rate, stand-off distance,
powder feed rate, carrier gas flow rate, from the
ANOVA study results.
iii. The HVOF sprayed coatings produced with opti-
mized oxygen flow rate of 246.20 lpm, LPG flow rate
Sådhanå (2021)46:149
of 55.37 lpm, Stand-off distance of 220.95 mm,
powder feed rate of 24.86 gpm, and Carrier gas flow
rate of 14 lpm of showed a maximum hardness of
1325.26 HVx .and a porosity level of 0.2128 Vol %.
iv. In order to represent the efficiency of processing
parameters on these empirical equations, coating
sensitivity analysis was studied and showed that
oxygen flow rate was the factor that had a greater
impact on porosity and hardness, followed by LPG
flow rate, stand-off distance, powder flow rate and
carrier gas flow rate.
List of symbols
A Oxygen flow rate
B LPG flow rate
C Powder feed rate
D Stand-off distance
E Carrier gas flow rate
HVx Hardness value
Acknowledgements
The authors wish to express their deepest gratitude to the
Department of Manufacturing Engineering, Annamalai
University, Tamil Nadu, India for providing the facilities
for coating characterization.
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