Elevated-Temperature Wear

Study of HVOF spray Cr3C2–NiCr-

Coated Die Steels
Wear and surface damage of tools (die materials) in the hot metal forming industry is a crit-
Pankaj Chhabra ical problem observed and is producing an adverse effect on the process economy. The
I.K. Gujral Punjab Technical University, problem occurs when tool and workpiece interact at higher temperatures. However, the
Jalandhar 134003, India research related to the wear and friction of dies is still lacking. In the present investigation,
e-mail: [email protected] tribological (wear and friction) studies were conducted with an aim to explore the potential
of Cr3C2–NiCr surface coating. The high-velocity oxy-fuel (HVOF) spray technique was
Manpreet Kaur1 used to formulate the coatings. The microhardness, surface roughness, bond strength,
Baba Banda Singh Bahadur Engineering College, and porosity of the coated specimens were found and analyzed. Subsequently, elevated-tem-
Fatehgarh Sahib 140407, India perature wear and friction study of the uncoated and coated specimens were done in the
e-mail: [email protected] laboratory. The study was conducted at 25 N and 50 N loads. The coated specimens
showed an increase in wear resistance at all test parameters. The lowest value of coefficient
of friction (COF) and the specific wear-rate for the coated specimens were observed at
400 °C. Wear mechanisms were studied by the scanning electron microscopy (SEM) tech-
nique. The wear mechanisms were observed to be adhesive in nature at room temperatures
and the combination of abrasive/oxidative/adhesive in nature at higher temperatures for the
Cr3C2–NiCr-coated specimens. [DOI: 10.1115/1.4046017]

Keywords: die tool steels, HVOF spray, Cr3C2–NiCr, wear, friction, temperature,
adhesion, coatings, surface properties and characterization, wear mechanisms

1 Introduction likely originate from the die surface region [9]. Furthermore, the
ability to retain its dimensional stability under accelerated condi-
Hot forming of high-strength steel sheets has become the need of
tions is another important factor. Therefore it is necessary to
industry due to various problems occurring in the cold forming pro-
control the wear and friction of die materials [5,8,10–12].
cesses. The problems such as poor formability to complex shapes,
Surface engineering plays a vital role in mitigating the problems
high spring back, and inclination to work-harden are generally
occurring due to wear and friction. The surface coatings increase the
experienced during the cold metal forming operation [1].
life and performance of the substrate materials, protect them from
However, the hot forming process is complex from a tribological
wear, and improve the mechanical properties [13]. Large numbers
(wear and friction) point of view compared to cold forming pro-
of surface coatings have been developed on different materials.
cesses. Thermal fatigue, plastic deformation, wear, increased oxida-
Their wear and friction studies are reported [5,8,14–26]. The
tion, and changes in the mechanical properties of tool (dies) and
authors also observed the superior properties of the coatings at ele-
workpiece materials occur when they interact with each other at ele-
vated temperatures. However, the high-temperature tribological
vated temperatures [1–5]. These problems reduce the performance
behavior of surface coatings developed on die steel materials
and service life of dies. Failure of dies is mainly affected by material
have been given lesser attention. The tribological behavior of the
properties, temperature, loading conditions, and environment.
coatings has been studied more at room temperatures and on
Among these factors such as temperature and load, conditions
various other metallic materials. Different surface coating tech-
have a significant influence on the tribological properties of the
niques such as thermal spray, weld overlay coatings and vapor
die materials [1,6]. The hot forming operations at higher tempera-
deposition processes such as chemical vapor deposition/physical
tures above 300 °C greatly influence the wear and frictional beha-
vapor deposition, etc. reveal better wear resistance [8]. The
vior. This results in unwanted performance of the equipment
current investigation aims to investigate the wear and friction beha-
[1,6,7]. Literature studies reveal that there is a need to increase
vior of the uncoated steels and the high-velocity oxy-fuel (HVOF)
the understanding of wear and friction behaviors at elevated temper-
thermal spray coated tool steel materials at three temperatures (RT,
atures. Bournicon [2] reported in his study that in over 70% of cases
400 °C, and 800 °C).
the die life is affected by surface wear and friction. Despite such sig-
The HVOF spray technique has been chosen in this work because
nificance, the wear and friction studies of die steels have received
of its better characteristics than many other coating techniques. It
very little attention.
possesses higher particle velocities and lower flame temperatures
AISI H11 and AISI H13 are the commonly used tool steels in the
thereby avoiding substrate overheating. The technique has replaced
hot metal forging/forming industry. These materials are selected in
the hard chrome plating in many industries where frictional resis-
the present investigation to study their tribological behavior. The
tance is required [14]. Salman [15] investigated the wear and fric-
steels are high chromium tool steels and possess high toughness
tion behavior of HVOF-sprayed TiAl/Al2O3 coating deposited on
and hardness [5,8]. However, these materials fail due to wear and
AISI H13 steel used for aluminum high-pressure die casting. The
thermal/mechanical fatigue at higher temperatures and loads. The
authors showed the improved wear resistance of the coated speci-
die surface region suffers during operations. The defects most
mens. Moreover, Harvey [16] in his work mentioned that a
coating developed by the HVOF technique gives ten times more
1
adhesion at the coating and substrate interface than the other
Corresponding author. thermal spray techniques [16].
Contributed by the Tribology Division of ASME for publication in the JOURNAL OF
TRIBOLOGY. Manuscript received August 12, 2019; final manuscript received January Thermally sprayed Cr3C2–NiCr coatings are being developed on
13, 2020; published online January 17, 2020. Assoc. Editor: Nuria Espallargas. the materials where wear and oxidation resistance are required.

Journal of Tribology Copyright © 2020 by ASME JUNE 2020, Vol. 142 / 061401-1
Cr3C2 provides wear resistance and NiCr enhances the oxidation at wear and friction are tremendous. Therefore, in the present study,
higher temperatures. The coatings showed good tribological proper- Cr3Cr2–NiCr coating was formulated by the HVOF spray technique
ties at higher temperatures and in the aggressive environment. on the selected die steel specimens. An in-depth study of the as-coated
However, the research was conducted more on the steam turbine specimens was done using several techniques. The results are
and boiler tube materials [13]. The authors recommended the reported in the paper. Further, the tribological studies of the speci-
deposition of Cr3C2–NiCr coatings onto various substrate materials mens were carried out on a high-temperature tribometer. The work
such as SA213 T22, T11, T91, and SAE-347H [13,17–19]. The was conducted under two load conditions and three temperatures.
sliding wear and friction studies of Cr3C2–NiCr coatings deposited
on the hot forming tool steels are still lacking. Sahraoui et al. [20],
Murthy and Venkataraman [21], Shabana et al. [22], Shunmuga 2 Experimental Procedure
et al. [23], and Roy et al. [24] studied the wear behavior of 2.1 Substrate Materials, Coating Formulation, and
Cr3C2–NiCr coatings deposited onto the surface of different sub- Characterization. In this study, the substrate materials, namely,
strates. The research was carried out at various temperatures. The AISI H11 (H11) and AISI H13 (H13) were selected after consulting
authors reported the lower wear-rates of the coated specimens. the actual hot press forging industry. Cylindrical-shaped pins with
Matikainen et al. [25] inspected the sliding wear behavior of 50 mm length and 8 mm diameter were prepared from the materials.
Cr3C2–NiCr coating accumulated on low carbon steel substrates The 20MnCr5-high-strength low-alloy steel was selected as the
(S235) by the HVOF spray method. The authors performed the workpiece (disc) material. The steel is used for preparing pinions
wear test on the ball-on-disk configuration using Al2O3 ball at by the hot press forging industry. Table 1 shows the composition
room temperature and an elevated temperature of 700 °C. Lowest of the tool (die) steel and the disc material. Round discs of
wear-rate was reported for Cr3C2–NiCr coating at elevated temper- 100 mm diameter and 8 mm thickness were made. To study the
atures. Further for the coated specimens, the authors observed that sliding wear behavior of pin (tool) materials, the disc should be
the coefficient of friction values and wear-rates got decreased with harder. Plasma nitriding and heat treatment were performed on
the increase in applied loads at a constant speed. Bolelli et al. [26] the disc material to increase the hardness. The hardness of the
planned to appraise the microstructure, micromechanical properties, disc was increased to 60–80 HRC.
and dry sliding wear conduct of two Cr3C2–NiCr cermet coating, Further, Cr3C2–25(80Ni20Cr) coating with a particle size of −45
deposited by the HVOF and the high velocity flame spary + 15 µm was developed onto the tool materials by the HVOF spray
(HVFS) techniques. The coating was accumulated on a low technique at the Metallizing Equipment Company, Pvt. Ltd.
carbon steel material and the ball-on-disc wear test at room temper- (MECPL), Jodhpur, India. The coating powder was supplied by
atures (RT) and was performed at 400 °C. The authors reported the the Powder Alloy Corporation, Cincinati, OH, and was available
better wear resistance of coating in comparison to the substrate. with (MECPL) Jodhpur. Before coating formulation, the specimens
From the literature, it has been concluded that tribological were mirror polished and grit blasted by alumina (Grit 60). The scan-
aspects of hot forming of metals are not studied in sufficient detail. ning electron microscopy (SEM) morphology of the Cr3C2–
Less work has been done in the field of friction and wear testing of 25(NiCr) powder is shown in Fig. 1. Irregular sized particles in the
Cr3C2–NiCr-coated steels at high temperatures. The losses due to form of lumps were identified. Few of them had a spherical

Table 1 Chemical composition of the tool and disc material

Chemical composition (wt%)

Tool steels C Mn P S Si Cr Mo Ni V Cu Fe

H11 0.33–0.43 0.20–0.50 <.03 <.03 0.80–1.20 4.75–5.50 1.10–1.60 <0.3 0.3–0.6 <0.25 Bal.
H13 0.32–0.45 0.20–0.50 <.03 <.03 0.80–1.20 4.75–5.50 1.10–1.75 <0.3 0.8–1.2 <0.25 Bal.

Disc material (20MnCr5) C Mn P S Si Cr Fe - - - -

0.17–0.22 1.1–1.4 Max 0.025 Max 0.035 Max 0.4 1.0–1.3 Bal - - - -

Fig. 1 SEM and EDS analysis Cr3C2–25(NiCr) powder

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 record the temperature and velocity of spray particles. The gun trav-
erse speed used was 2.5 mm/s and the thermocouple was used to
measure the flame temperature. The powder feed rate for the
Cr3C2–NiCr powder was 25 g/min. To maintain the temperature of
the substrate during the spraying process, cooling them after spraying
was done with the aid of compressed air jets. Table 2 shows the spray-
ing parameters adopted. The coating thickness was kept in the range
of 200 ± 50 µm on both the substrates.
Further, the surface roughness value (Ra) of the coatings was
recorded before and after polishing the samples. The Mitutoyo
Japan Digital Surface Roughness Tester- Model-SJ-301 (least
count of 0.1 μm) with the sampling length as 4 mm was used.
The values were recorded at three different places on the same
line on the specimens. The average of the Ra values before and
Fig. 2 X-ray diffraction pattern for the Cr3C2–25(NiCr) powder after polishing is reported.
Surface porosity of the coated specimens was measured using an
Image Analyser attached with an Inverted Metallurgical Micro-
Table 2 Spray parameters used during the formulation of scope. The bond strength of the coating was evaluated using an
coating epoxy resin adhesive with ultra bond 100 and nominal strength of
about 12,000 psi. Three tests were conducted. The average of the
Oxygen flow rate (SLPM) 300–350 readings was obtained. The ASTM standard C-633 was followed.
Fuel (LPG) flow rate (SLPM) 60–80 The digital microhardness tester with a pyramidal diamond
N2 flow rate (SLPM) 15–20 indenter (Model: WILSON) was used to obtain the microhardness
Oxygen pressure (kg/cm2) 9 on the surface as well along the cross section of the coated speci-
Fuel pressure (kg/cm2) 5.6 mens. The load of 2.45 N was considered. The 10 s dwell time of
Powder pressure (kg/cm2) 3
Spray distance (mm) 250 indentation was fixed. A mean of three observations was consid-
Flame temperature (°C) 2800–3200 ered. The microhardness along the cross section of the as-sprayed
Particle temperature (°C) 2200 specimens was plotted.
Particle velocity (m/s) 450–500 The XRD analysis of as-sprayed specimens was conducted on the
equipment procured from The Netherlands. The company is Expert
Pro PAN analytical company (Model: MPD). The analysis was per-
formed with Cu Kα radiation and nickel filter at 20 mA under a
morphology. X-ray powder diffraction diffractogram for the HVOF voltage of 35 kV. The goniometer scanning speed was taken at a
spray powder is shown in Fig. 2 on reduced scales. The Cr3C2 phase chart speed of 1 cm/min. The speed of 2 deg/min in the 2θ range
was observed as the strong intensity phase in the Cr3C2–NiCr of 30–100 deg was considered. The XRD diffractogram was
powder. NiCr was observed as the medium intensity phase. The coat- plotted with defined d′ values in EXPERT HI score software. It includes
ings were deposited by a commercial HVOF (HIPOJET-2700) appa- the coating elements and identifies various phases.
ratus. The equipment uses oxygen and liquid petroleum gas (LPG) as The surface as well as the cross-sectional morphology of the
the input gases. The OSEIR spray watch equipment was used to as-sprayed specimens along with the elemental composition were

Fig. 3 High-temperature tribometer setup

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 Table 3 Typical test parameters for wear and friction tests

Test parameter Values

Constant load 25 N and 50 N

Temperature RT, 400 °C and 800 °C
Sliding speed 0.5 m/s
Sliding distance 1500 m
Test duration 50 min

Fig. 6 Microhardness profiles along the cross section of coated

steels

Fig. 4 Drawing of the pin-on-disc wear test

Fig. 5 The camera pictures of the as-sprayed coatings

studied with a field emission-scanning electron microscope

(FE-SEM, FEI, Quanta 200F Company) attached with EDS GENESIS
software (Czech Republic). The equipment was used to study the
coating microstructural features and to analyze the composition Fig. 7 The SEM microstructure along the cross section of the
of the coating. Electron beam energy of 20 keV was considered. HVOF spray Cr3C2–25 (NiCr) coating: (a) H11 tool steel and (b)
To study the cross-sectional details, the specimens were cut, H13 tool steel

Table 4 Properties of Cr3C2–25(NiCr) coated specimens

Thickness Hardness Porosity Bond strength Surface roughness as sprayed (µm) before
Coating (µm) (Hv 0.3 @ VHN) (%) (MPa) polishing/after polishing

HVOF spray Cr3C2-25(NiCr) 175 ± 9 750 ± 37 2.26 ± 0.45 72.98 ± 4 4.68/0.83

coated H11 steel
HVOF spray Cr3C2-25(NiCr) 235 ± 12 790 ± 39 2.06 ± 0.41 73.43 ± 4 4.92/0.87
coated H13 steel

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 wear tests. The Ra values of all the specimens were reduced to
1 µm before the experimentation. The test parameters given in
Table 3 were chosen based on the typical values used in the hot
forging/ forming processes. The test parameters including tempera-
ture have been selected based on the literature studies on other
surface techniques and for different high-temperature applications
[7,27]. In actual hot forming industries, the workpiece is heated
well above 1000 °C. The hot workpiece is then placed between
the dies and the process is done. Sometimes the tool steel (dies)
is preheated. During the operations, the temperature of the tool
surface rises above 400 °C. After some time in operation, the hard-
ness of the dies decreases due to sliding and the wear debris is gen-
erated. The dies suffer wear and lose their dimensions. Similar as in
Fig. 8 X-ray diffraction pattern for the HVOF-sprayed Cr3C2– the industry, the disc was heated up to the desired temperatures
25(NiCr) coating on H11 steel using an induction heater before loading against the coated pin spe-
cimen. The pyrometer was employed to measure the temperature of
the disc specimen. On obtaining the desired disc temperature, the
pin was loaded onto the disc surface and the wear test was per-
mounted, and mirror polished. The procedure has been explained formed under unidirectional dry sliding conditions. The schematic
elsewhere [8]. The cross-sectional SEM images gave the coating of the wear test is shown in Fig. 4. The frictional force was obtained
thickness values. by the strain gauge force transducer and the change in pin height
was measured by linear variable differential transformer (LVDT).
The computerized data acquisition for monitoring and controlling
2.2 Tribological (Wear and Friction) Testing. A high- the different parameters was equipped to high-temperature trib-
temperature tribometer (Fig. 3), Model-TR-20LE-DHM-PHM-800, ometer. The wear weight loss of the pins was examined by the elec-
was used to study the tribological characteristics of the coated and tronic microbalance. The pins were weighed before and after
uncoated specimens. The tribometer was procured from Ducom the tests. The tests were repeated to obtain good reproducibility.
Bangalore. ASTM G99-04 was followed for carrying out the The specific wear-rates (mm3/Nm) and the average value of the

Fig. 9 The SEM morphology and EDS examination results for the coated specimens in as-sprayed condition: (a) on AISI
H11 and (b) on AISI H13

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coefficient of friction (COF) were evaluated. The wear-rates were both the substrate were grayish in color. Smooth coating surfaces
calculated by the following equations: free from any defects were obtained.


m1
Coating density (ρ) g/cm = ρ1
3
(1)
ma − m1 3.2 Surface Roughness, Bond Strength, and Porosity.
Table 4 shows the Ra values, the porosity, and the bond strength
where ρ1 is the density of water (1 g/cm ) at RT, ma the weight
3
values for the HVOF spray Cr3C2–NiCr-coated specimens.
of the coating in the air (g), and m1 is the weight of coating in Before polishing, the Ra value for the coated H11 and H13 speci-
water (g). mens was obtained as 4.68 µm and 4.92 µm, respectively. After pol-

 ishing, the value was reduced to 0.83 µm and 0.87 µm, respectively.
Mass loss
Volume loss (mm3 ) = × 1000 (2) Due to better properties of the HVOF spray technique, the values
ρ were obtained below 1 µm. Miguel et al. [28] also mentioned in
their study that the lower surface roughness was attributed to the
Specific wear − rate (mm3 /Nm) superior properties of the HVOF spray technique. The characteristic
feature of the technique is the higher velocity of the spray particles.
Volume loss
= (3) The bond strength of the as-sprayed H11 and H13 steel specimens
Sliding distance × applied load was evaluated as 72.98 ± 4 MPa and 73.43 ± 4 MPa, respectively.
Glue failure was observed during the testing for both the substrate
The worn-out samples were analyzed using the finite element materials. Singh et al. [8] opined in their study that due to higher
(FE)-SEM/energy-dispersive X-ray spectroscopy (EDS) technique particle velocities in the HVOF spray process, on impinging on
with an aim to understand the wear mechanisms. the substrate the powder particles partially melt. The authors also
found higher bond strength values for the HVOF-sprayed coatings
in their study. Xie et al. [29] deposited Cr3C2–NiCr coating on the
stainless steel substrate and also reported near similar values of
3 Results and Discussion bond strength. The authors reported that better adhesive perfor-
3.1 Visual Examination. The camera macrographs of the mance of the coating was possibly due to firm embedment of the
as-sprayed pin specimens are shown in Fig. 5. The coatings on powder particles on the substrate and moreover residual

Fig. 10 The average coefficient of friction of the uncoated and the coated speci-
mens subjected to sliding wear tests on a high-temperature tribometer under a
constant load of 25 N for 50 min run at different temperatures

Fig. 11 The average coefficient of friction of uncoated and the coated specimens
subjected to sliding wear tests on a high-temperature tribometer under a constant
load of 50 N for 50 min run at different temperatures

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 Fig. 12 The coefficient of friction as a function of time for uncoated and the coated specimens at (a) RT, (b) 400 °C, and (c)
800 °C under 25 N load and at (d ) RT, (e) 400 °C, and ( f ) 800 °C under 50 N load, respectively

Table 5 Specific wear-rates [(mm3/Nm) × 10−6] of the specimens after wear tests

RT 400 °C 800 °C

Specimen details 25 N 50 N 25 N 50 N 25 N 50 N

Uncoated H11 steel 609.91 ± 13 487.18 ± 10 42.39 ± 0.85 28.21 ± 0.56 30.77 ± 0.62 26.67 ± 0.53
Uncoated H13 steel 795.18 ± 16 552.26 ± 11 61.25 ± 1.25 33.38 ± 0.67 36.13 ± 0.72 29.25 ± 0.59
HVOF spray Cr3C2–25(NiCr) coated H11 steel 4.49 ± 0.09 6.05 ± 0.12 3.57 ± 0.13 3.46 ± 0.07 6.91 ± 0.14 5.7 ± 0.11
HVOF spray Cr3C2–25(NiCr) coated H13 steel 6.21 ± 0.12 7.35 ± 0.15 3.76 ± 0.08 2.59 ± 0.05 9.82 ± 0.20 6.73 ± 0.13

Journal of Tribology JUNE 2020, Vol. 142 / 061401-7

 (a)

(b)

(c)

Fig. 13 The SEM micrographs and the EDS examination results for the uncoated H11 steels after wear testing at 25 N load:
(a) room temperature, (b) 400 °C, and (c) 800 °C

compressive stresses also contribute to better strength of the values of the coated specimens on H11 and H13 steels were
coating. Kasparova et al. [30] and Tan [31] also reported similar obtained as 750 ± 37 HV and 790 ± 39 HV, respectively. The
values of bond strength, and glue failure was observed for the microhardness values for the coating were measured along the
HVOF-sprayed Cr3C2–NiCr coating. The porosity of the developed cross section and plotted as shown in Fig. 6. Microhardness of
coating was also evaluated. The ASTM E2109-01 standard was coating on the H11 steel was in the range of 450–825 HV with an
used to measure the porosity of the coatings. The value of porosity average of value of 712 HV. Microhardness of coating on H13
of the coating on the H11 steel was found as 2.26% ± 0.45% and on was in the range of 425–800 HV with an average value of
the H13 steel as 2.06% ± 0.41%. 700 HV, while the substrates H11 and H13 have an average micro-
hardness value of 247 ± 12 HV and 233 ± 11 HV, respectively. The
3.3 Microhardness, Cross-sectional Scaning Electron uniform heating and the higher kinetic energy of coating particles in
Microscope, and Coating Thickness. The surface hardness the HVOF spray system resulted in higher microhardness values of

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 (a)

(b)

(c)

Fig. 14 The SEM micrographs and the EDS examination results for the coated H11 steels after wear testing at 25 N load: (a) room
temperature, (b) 400 °C, and (c) 800 °C

coated specimens. Further, Xie et al. [29] opined that the high hard- was reported in Refs. [25,26,29]. The carbides are evenly distribu-
ness values provide better wear resistance because hard carbides ted in the binder phase with depth.
could counteract external pressure effectively [29].
The cross-sectional SEM images for the coated steel specimens
are shown in Fig. 7. The micrographs show three regions, 3.4 X-ray Powder Diffraction Analysis. The X-ray diffracto-
namely, substrate, coating, and epoxy. The average thickness of grams for the coated H11 die steel are shown in Fig. 8. The analysis
the coating on H11 and H13 steel was measured along the cross revealed the formation of Cr3C2 and Cr7C3 as the strong intensity
section as 175 ± 9 µm and 235 ± 12 µm, respectively. The micro- phases, NiCr as the medium intensity phase, and Ni3Cr and C as
graphs showed a dense coating with uniform thickness. The the weak intensity phases. Similar phases were identified on the
coating was free from defects. Some superficial pores were as-sprayed H13 steel. David et al. [14], Xie et al. [29], Ji et al.
observed in the coating. Similar cross-sectional microstructure [32], Picas et al. [33], and Houdkova et al. [34] developed

Journal of Tribology JUNE 2020, Vol. 142 / 061401-9

 (a)

(b)

(c)

Fig. 15 The SEM micrographs and the EDS examination results for the uncoated H11 steels after wear testing at 50 N load:
(a) room temperature, (b) 400 °C, and (c) 800 °C

Cr3C2–NiCr coating using the HVOF spray technique on different shown in Fig. 9. The microstructure of the coated H11 steel is
substrate steels and reported similar phases. The authors further found to have splat-like morphology with distinct white boundaries
mentioned that the Cr7C3 phase was formed due to decarburization surrounding the splats (Fig. 9(a)). The morphology of the coated
of Cr3C2 during spraying. H13 steel (Fig. 9(b)) showed small splats distributed all over the
surface. The flattened portion depicts fully molten areas. The
coating exhibits uniform microstructure. The EDS analysis of the
3.5 Surface Finite Element-Scanning Electron Microscope/ coating on both the substrates shows the occurrence of mainly Ni
Energy-Dispersive X-ray Spectroscopy Analysis. The FE-SEM and Cr. Large amounts of carbon and oxygen in the coating were
morphologies of the as-sprayed coating on both the substrates are also seen. These elements attribute to the formation of carbides and

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 (a)

(b)

(c)

Fig. 16 The SEM micrographs and the EDS examination results for the coated H11 steels after wear testing at 50 N load: (a) room
temperature, (b) 400 °C, and (c) 800 °C

oxides in the coating. Similar microstructures of the HVOF-sprayed specimens obtained after the experimentation at the three test tem-
Cr3C2–NiCr coating deposited on different substrate steels were peratures and at two loads. Figure 12 shows the plot of COF with
reported by Bolelli et al. [26], Picas et al. [33], David et al.[14], Pru- time. Table 5 shows the specific wear-rate values for all the tested
denziati et al. [35], Chatha [36], and Cunha et al. [37] in their studies. specimens at both the loads and at different temperature conditions.
After experimentation at RT, the average COF values were found
as ∼0.48 and ∼0.40 for the uncoated H11 steel at 25 N and 50 N
3.6 Wear and Frictional Behavior. Figures 10 and 11 show loads, respectively. For the uncoated H13 steel, the values were
the graphical plots of the average values of the COF for all the recorded as ∼0.58 at both the test loads. The coated H11 and

Journal of Tribology JUNE 2020, Vol. 142 / 061401-11

 (a)

(b)

(c)

Fig. 17 The SEM micrographs and the EDS examination results for the uncoated H13 steels after wear testing at 25 N load: (a)
room temperature, (b) 400 °C, and (c) 800 °C

H13 specimens showed a higher value of COF as ∼0.71 and ∼0.64 the uncoated H11 and H13 steels during their studies on a
at 25 N load, respectively. At 50 N load, the COF for the coated tribometer.
H11 and H13 specimens reduced to ∼0.57 and ∼0.53, respectively. On the other hand, in the coated specimens, dry sliding devel-
The lower values of COF for the uncoated steels might be due to oped high local pressures between the contacting carbide asperities
the large difference of surface hardness values between the disc that led to the plastic deformation, adhesion, and formation of local
and the pin specimens that resulted in the easier removal of the par- junctions. This resulted in higher COF values [39]. Bolelli et al.
ticles from the pin surface. Barrau et al. [38], King et al. [39], and [26], Picas et al. [33], and Houdkova et al. [34] also reported
Lakshman and Vignesh [40] observed similar values of COF for the COF values for the Cr3C2–NiCr-coated specimens in the

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 (a)

(b)

(c)

Fig. 18 The SEM micrographs and the EDS examination results for the coated H13 steels after wear testing at 25 N load: (a) room
temperature, (b) 400 °C, and (c) 800 °C

range of 0.7–0.79. Huang et al. [41] studied the wear behavior of increased, the temperature of the frictional surface increased.
Cr3C2–NiCr coatings deposited on low carbon steel. The wear That gave rise to the decrease of plastic deformation resistance
tests were performed at loads from 10 N to 150 N. The authors of frictional pair. The decrease of mutual hindering effect
observed the decreased COF values at the higher loads. The between micro peaks in the surface also occurred and reduced
authors explained that the magnitude of the normal load was the friction coefficient [41].
important because it increased the area of contact between the The COF versus time plots for uncoated and coated samples at
pin and the disc surface. The depth below the surface at which room temperature were observed to be unstable at room tempera-
the maximum shear stress occurred was also increased and they tures. Houdkova et al. [34] opined that in case of Cr3C2–NiCr
both affected the elastic or plastic deformation states. In addition, coating due to its lower fracture toughness, a higher amount of car-
owing to the frictional heating the increase in temperature contrib- bides and bigger wear debris were pulled out and caused the fluctu-
uted to reducing the friction coefficients. As the load was ation of the coefficient of the friction curve. The fluctuation in the

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 (a)

(b)

(c)

Fig. 19 The SEM micrographs and the EDS examination results for the uncoated H13 steels after wear testing at 50 N load: (a)
room temperature, (b) 400 °C, and (c) 800 °C

COF values was observed to be more at 50 N loads at the same tem- load and ∼80 and ∼75 times at 50 N load for H11 and H13, respec-
peratures. The specific wear-rate for the uncoated H11 and H13 tively. The lower wear-rates for the coated specimens might be due
specimens showed higher values as 609.91 ± 13 mm3/Nm × 10−6 to the higher hardness and the cohesive strength of the HVOF-
and 795.18 ± 16 mm3/Nm × 10−6 at 25 N. The wear-rates decreased sprayed Cr3C2–NiCr coating.
to 487.18 ± 10 mm3/Nm × 10−6 and 552.26 ± 11 mm3/Nm × 10−6 at The FE-SEM images of the uncoated steels (Figs. 13(a), 15(a),
50 N for the H11 and H13 steels, respectively. On the other hand, 17(a), and 19(a)) show excessive material removal, plow marks,
the specific wear-rates for the coated H11 and H13 steels were material pull-outs, and adhered wear debris. The wear mechanism
recorded to be 4.49 ± 0.09 mm3/Nm × 10−6 and 6.21 ± 0.12 mm3/ was found to be predominantly adhesive for both the uncoated
Nm × 10−6 at 25 N and 6.05 ± 0.12 mm3/Nm × 10−6 and 7.35 ± steels at the two testing loads. With an increase in load, at 50 N
0.15 mm3/Nm × 10−6 at 50 N. The specific wear-rates for the more adhered material, larger material pull-outs, and delamination
coated specimens got reduced by ∼134 and ∼127 times at 25 N of the compressed top layers were observed.

061401-14 / Vol. 142, JUNE 2020 Transactions of the ASME

 (a)

(b)

(c)

Fig. 20 The SEM micrographs and the EDS examination results for the coated H13 steels after wear testing at 50 N load: (a) room
temperature, (b) 400 °C, and (c) 800 °C

The FE-SEM images of worn-out Cr3C2–NiCr-coated H11 and carbide particles resulting in pulling out of coating surface. The
H13 specimens after the wear and friction experimentation at EDS analysis showed the presence of coating elements (Cr, C,
room temperatures are shown in Figs. 14(a), 16(a), 18(a), and and Ni) in the worn-out surface along with Fe and O in small per-
20(a), respectively. Wear tracks were mild and shallow on the centages. This showed that the coating was intact with the substrate
coated specimens. The wear mechanism was found to be adhesive material after 50 min of wear experimentation.
in nature. Mild abrasive grooving was also observed. Small At 400 °C test temperature, there was an appreciable decrease in
craters, material pull-outs, and wear debris were observed on the the average COF values. The values for the uncoated H11 and H13
worn surfaces. Houdkova et al. [34] reported in their work that were recorded as ∼0.43 and ∼0.44 at 25 N load, respectively. The
the wear mechanism for Cr3C2–NiCr-coated specimens at RT was values were observed to be 0.4 and ∼0.39 for the uncoated H11 and
due to the gradual loss of the metal matrix that weakened the H13 at 50 N load, respectively. In case of the coated H11 and H13

Journal of Tribology JUNE 2020, Vol. 142 / 061401-15

specimens, the COF values were ∼0.4 at 25 N and 50 load condi- parameters. The SEM images for the uncoated and the coated
tions. The decrease in the COF values from the room temperature worn-out specimens at 800 °C are shown in Figs. 13–20.
was notable. The decrease in the COF values was attributed to In uncoated specimens, the presence of compressed oxide layers,
the formation of solid compact layers of oxide and wear debris multilayered flakes, and cracking in the top layer was observed. The
due to oxidation at elevated temperatures. The oxidized layers fatigue wear mechanism was observed. The SEM images for
acted as the continuous solid lubricant throughout the whole wear worn-out coated specimens showed the presence of abrasive wear
track, thus giving rise to lower friction coefficients [25–27]. marks, adhered material, and the compact oxide layer. The wear
The friction of coefficient versus time graphs show a steady-state mechanism was found to be the combination of abrasive, oxidative,
regime, the plots were much stable as compared to room tempera- and adhesive. The EDS analysis of the coated specimens confirms
ture curves. The curves were similar for both the load conditions. the presence of coating elements, with significant amounts of
Small fluctuations in the values might be due to the delamination oxygen and iron present in the top surface layer. Zhou et al. [43]
of the oxide layer and abrasive grooving by wear debris. The spe- and Poirier al. [44] reported similar wear mechanisms for the
cific wear-rate values for uncoated H11 and H13 specimens Cr3C2–NiCr coatings at higher temperatures in their studies.
showed a sharp decrease at both the load conditions. At 25 N
loads, the wear-rates were observed as 42.39 ± 0.85 mm3/Nm ×
10−6 and 61.25 ± 1.25 mm3/Nm × 10−6 for the uncoated H11 and 4 Conclusions
H13 steels, respectively. The values further decreased to 28.21 ±
0.56 mm3/Nm × 10−6 and 33.38 ± 0.67 mm3/Nm × 10−6 for the • The Cr3C2–NiCr coating developed by the HVOF spray
uncoated H11 and H13 steels at 50 N loads, respectively. The process exhibited higher hardness, higher bond strength,
coated specimens also showed a decrease in specific wear-rate dense, and was free from any defects. The average value of
values. At 25 N loads, the specific wear-rates were recorded as microhardness of the coating was found to be 750 ± 37 HV
3.57 ± 0.13 mm3/Nm × 10−6 and 3.76 ± 0.08 mm3/Nm × 10−6 for and 790 ± 39 HV on the H11 and H13 steels, respectively.
the coated H11 and H13 steels, respectively. At 50 N loads, the • The specific wear-rate values for the uncoated specimens
values for both the coated specimens were recorded as 3.46 ± decreased with the increase in temperature and load.
0.07 mm3/Nm × 10−6 and 2.59 ± 0.05 mm3/Nm × 10−6, respec- However, the values were found to be more than that of the
tively. At elevated temperature, the oxidation of wear debris and coated specimens. Better wear resistance was observed in
counterface material occurred under the compressive forces the coated specimens at all test temperatures.
between the mating surfaces. Hardell [27] explained in his work • The coefficient of friction values for the coated specimens
that the compact layers consisted of oxides of coating and the decreased at elevated temperatures. The lowest specific wear-
counter material debris. These layers acted as the solid lubricant rate values and the COF values were observed at 400 °C
which further lowered the value of friction and specific wear-rates. temperature.
The increase in compressive forces due to the increase in load made • The slight increase in specific wear-rate values at 800 °C was
such a layer more compact, thus further decreasing the specific observed. This might be endorsed to the softening of the mate-
wear-rate [27]. rial and few disintegrated oxide layers that resulted in three-
The SEM images of the worn surfaces of the uncoated H11 and body abrasive wear.
H13 are shown in Figs. 13(b) and 15(b), respectively, at 25 N. At • The mechanism of wear was found to be predominantly adhe-
50 N, the images for the uncoated specimens are shown in Figs. sive at RT for the coated specimens, whereas the mechanism
17(b) and 19(b). The wear mechanism was found to be adhesive was found to be the combination of oxidation–abrasion–
for the uncoated steels. The SEM images indicated the presence adhesion at both the 400 °C and 800 °C temperatures.
of adhered material, abrasive marks. The presence of oxygen
along with other elements in the EDS analysis indicated the forma-
tion of some oxide layers on the surface. The SEM images for the Acknowledgment
Cr3C2–NiCr-coated specimens are shown in Figs. 14(b), 16(b), The authors gratefully acknowledge the research grant from
18(b), and 20(b) at 25 N and 50 N loads, respectively. The Department of Science and Technology, New Delhi (India) under
adhered wear debris, shallow abrasive wear marks, and the solid SERB, Science and Engineering- Engineering Scheme (File No.
compact oxide layers were observed. In Fig. 20(b) material pull SR/S3/MERC/0072/2012, Dated February 28, 2013) titled—Devel-
out and craters could be seen. The wear mechanism was found as opment of Thermal Spray Coatings to Control Wear During High-
the combination of adhesive, abrasive, and oxidative wear. Temperature Applications, and (EMR/2015/000234, Dated March
At 800 °C temperature, the values of the coefficient of friction for 11, 2016) titled—Development of Thermal Spray Coatings to
the uncoated steels decreased at 25 N load and nearly constant at Control Wear During High-Temperature Applications-Phase II, to
50 N loads. The values enhanced to 0.43 and 0.51 for the coated carry out this research and development work. Moreover, the
H11 and H13 specimens, respectively, at 25 N loads. The minor authors would like to thank the Metallizing Equipment Company
increase in the values was noticed at the higher loads also. Lesser Pvt. Ltd. Jodhpur (India) for providing the HVOF and Plasma
fluctuations in the COF with time were observed during the exper- spray coatings services for the die materials. The authors owe
imentation (Figs. 12(c) and 12( f )). special thanks to Dr. Harpreet Singh for extending the necessary
Furthermore, the specific wear-rates for the uncoated H11 and H13 facilities and support in conducting the detailed analysis at the
steels were recorded to be 30.77 ± 0.62 mm3/Nm × 10−6 and 36.13 ± Indian Institute of Technology Ropar, Roopnagar, Punjab, and
0.72 mm3/Nm × 10−6, respectively, at 25 N load. The values were Dr. S. Parkash at the Indian Institute of Technology Roorkee,
lower than those obtained at 400 °C at both the loads. On the other Roorkee. The authors would also like to thank IKGPTU, Jalandhar,
hand, the wear-rates for all the coated specimens increased at 800 India, for supporting this work.
deg C. The values were higher than that obtained at 400 °C. The
increased wear-rates for the coated specimens at elevated tempera-
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