Accepted Manuscript

Title: Microstructure and mechanical performance of

TiC-Inconel825 composite coating deposited on AISI 304
steel by TIG cladding process

Authors: Sweta Saroj, Chinmaya Kumar Sahoo, Manoj

Masanta

PII: S0924-0136(17)30270-4
DOI: http://dx.doi.org/doi:10.1016/j.jmatprotec.2017.06.042
Reference: PROTEC 15295

To appear in: Journal of Materials Processing Technology

Received date: 28-1-2017

Revised date: 9-5-2017
Accepted date: 25-6-2017

Please cite this article as: Saroj, Sweta, Sahoo, Chinmaya Kumar, Masanta, Manoj,
Microstructure and mechanical performance of TiC-Inconel825 composite coating
deposited on AISI 304 steel by TIG cladding process.Journal of Materials Processing
Technology http://dx.doi.org/10.1016/j.jmatprotec.2017.06.042

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 Microstructure and mechanical performance of TiC-Inconel825 composite
coating deposited on AISI 304 steel by TIG cladding process

Sweta Saroj, Chinmaya Kumar Sahoo, Manoj Masanta*

Department of Mechanical Engineering, National Institute of Technology Rourkela, Rourkela

– 769 008, INDIA


Corresponding author: M. Masanta; Email: manoj.masanta@gmail.com, masantam@nitrkl.ac.in

Tel.: +91 6612462530; fax: +91661-2462501

Abstract
TiC reinforced Inconel825 based hard and wear resistance composite coating was fabricated
on AISI 304 steel by TIG cladding process utilizing in-house prepared Inconel825 powder
from the discarded chip of turning operation and commercial TiC powder. The proposed
coatings have inordinate potential applications, where resistance against wear and corrosion
are the foremost requirement. The TiC concentration, preplaced layer thickness and
processing current have shown significant influence on the microstructure and mechanical
performance of the coating. Owing to the superior wetting behavior of the Ni-based alloy
with TiC, and formation of intermediated phases excellent bond between the TiC particles
and Inconel825 matrix was achieved. The micro-hardness value of the coating reached upto
1100 HV0.05, and the sliding abrasive wear against alumina abrasive disc reduced more than
seven times as compared to the substrate.

Keywords: TIG cladding, Inconel825, MMC coating, wear resistance, micro-hardness

1. Introduction

High-performance nickel-based super alloys are in increasing demand for high-temperature

applications like turbo-engine, heat exchanger, turbines, industrial boilers in power plant,
reactor core in nuclear power plant, and various components in the chemical industry
(Aytekin et al., 2013). Thakur et al. (2009) demonstrated that owing to low thermal

1
conductivity, eminent shear strength, high work hardening rate, and high chemical affinity
with cutting tool materials, Ni based super alloys are known as most “difficult to machine”
materials. Therefore, fabrication of entire component with the Ni based super alloys become
more challenging and expensive. Nevertheless, making a layer of Ni based super alloy on
steel substrate found more economical, and an emerging research area.

Several research groups like Lambarri et al. (2013) and Jeshvaghani et al. (2014) have
taken the initiative to fabricate different grade Inconel based coating on relatively low
strength materials like stainless steel by laser cladding or tungsten inert gas (TIG)/ gas
tungsten arc weld (GTAW) cladding process. To improve the pitting corrosion resistance,
Abioye et al. (2015) fabricated single and overlapped beads of Inconel 625 layer on AISI 304
stainless steel by wire (Inconel 625) feeding laser cladding process. Heigel et al. (2016)
fabricated Inconel625 layer through laser cladding method using powder and wire feeding
mechanism. In order to identify the suitability of the laser cladding of Inconel718 for
manufacturing and repairing work of aeronautic components, Lambarri et al. (2013)
deposited Inconel718 clad layer on the same base material plate by laser cladding technique.
Nevertheless, because of limited hardness and poor wear resistance of the Ni based alloys,
their application is restricted in adverse abrasive or adhesive wear environment. Shi et al.
(2016) and Cooper et al. (2013) showed that the wear resistance property of the Ni based
alloys can be improved by reinforcing hard transition metal carbides like TiC, SiC or WC to
form nickel-based MMC, that retains high hardness, and high wear resistance at elevated
temperature. Wilson and Shin, (2012) established that the addition of hard ceramic particles
improved the mechanical properties of the matrix alloy without compromising its specific
strength and stiffness at elevated temperature. However, owing to poor wetting ability
between the reinforcing ceramic particles and metal matrix, particle-matrix interfacial bond
become inadequate to sustain under extreme loading condition that resulted in the premature
failure of MMCs during mechanical loading. Sahoo and Masanta, (2017) revealed that TiC
combines favorable properties such as high hardness, low thermal expansion coefficient and
good wettability with molten Ni or Ni based alloys. In addition, Shi et al. (2016) indicated
that owing to improved strength, hardness, modulus of elasticity and wear-resistance
properties, TiC reinforced Inconel718 MMC exhibits superior mechanical characteristics
compared to pure Inconel-718 parts, which effectively augments the service life of the
component. It was also established that due to the formation of an interfacial layer, the
wetting behavior of the TiC particle with Inconel718 matrix enhances and consequently a

2
superior bond between reinforced particles and the matrix material obtained (Hong et al.,
2013). Cooper et al. (2013) demonstrated that TiC reinforced Inconel625 MMC layer
produced by laser melting process exhibits superior hardness and fewer defects as compared
to SiC and Al2O3 reinforced MMC coating fabricated by the similar method. Jiang et al.
(2014) fabricated nano-TiCp reinforced Inconel-625 composite coating by laser cladding
process, which improved the hardness and modulus value of the coating approximately 10
and 12% respectively as compared to the laser cladded Inconel-625 substrate.

Literature revealed that most of the works related to Ni based alloy (Inconel 601, 625 or 718
series) accomplished by laser cladding using powder blown method. However, owing to high
capital cost and maintenance complexity, laser cladding process found uneconomical for
small scale industry or repairing work. It is well accepted that owing to smaller interaction
time, in laser coating/cladding process, dilution or mixing of the clad (reinforced) material
with the substrate is inadequate. In contrast, in weld-based method, owing to larger
interaction time and specific characteristic of the arc, Marangoni flow within the melt pool is
more prominent that enhances the probability of dilution of the clad material in the substrate
matrix and produces an MMC coating. Heigel et al. (2016) showed that large thermal
gradient and contraction of the molten material sometimes generates residual stresses in the
component during laser cladding process. Zhou et al. (2008) demonstrated that owing to
rapid solidification of the molten layer the tendency of crack formation is a foremost
deficiency of laser cladding processes. Weld based method specifically tungsten inert gas
(TIG) cladding is an economical alternate, which has potential to produce ceramic reinforced
MMC coating on various metallic substrates. Recently, Sandhua and Shahib (2016)
deposited Inconel625 clad layer on AISI 304L stainless steel by shielded metal arc welding
(SMAW) process. The test results revealed that Inconel625 overlay with higher clad content
exhibits enhanced wear resistance and fatigue strength as compared to the clad layer
produced with high level of dilution. Jeshvaghani et al. (2014) deposited Inconel617 clad
layer on ductile iron by TIG cladding process using 3 mm diameter filler wire and reported
superior hardness and wear resistance property in the clad layer as compared to the substrate
material due to the solution strengthening effect.

The above literature revealed that Inconel 601, 625 and 718 graded alloys were
predominantly used as matrix material to produce ceramic reinforced composite coating by
laser cladding process. Till date, no investigation on the Inconel825 alloy coating or
Inconel825 based MMC coating either by laser or TIG cladding process has been reported by

3
any research groups. Aytekin et al. (2013) reported that Incoloy825 is an advanced nickel-
iron-chromium alloy with titanium, copper and molybdenum additives that can perform under
extreme corrosive environments. However, to enhance the hardness and corresponding wear
resistance, reinforcement of hard particles in Incoloy825 become indispensable.

In consequence, there is a great prospect to develop a wear and corrosion resistance TiC-
Inconel825 clad layer on AISI304 steel by TIG cladding process. The proposed cladding
material has enormous potential to work under extreme abrasive and corrosive environment.
In the present work, TiC reinforced Inconel825 composite coating has been deposited on
AISI 304 steel to improve its mechanical properties i.e. hardness and wear resistance. The
effect of TiC content in the preplaced powder mixture, preplaced layer thickness and
processing current on the coating morphology and its mechanical performance has been
evaluated. The proposed coatings have potential application in down-hole drilling tool used
in crude oil exploration, where resistance against wear and corrosion are the foremost
requirement.

2. Experimental procedure

2.1.Powder preparation
The inconel825 powder was prepared from the chips obtained after the turning operation of
the Incolonel825 bar. The chips were first cut into small pieces (2-3 mm) by shearing action
using a snip cutter and cleaned in acetone bath using an ultrasonic cleaner for 1 h.
Subsequently, the chips were ball milled in a planetary ball mill with the help of hardened
high chromium high carbon alloy steel ball (C=0.95-1.1, Si=0.15-0.35, Mn= 0.5, P=0.012,
Cr=1.3-1.6, Mo=0.08, Ni=0.25, S=0.025, Fe= 96.5 - 97.32) submerged in toluene with a ball-
to-powder weight ratio of 10:1 for 2.5 h. Thus, a slurry of powder produced and after drying
it at room temperature, fine Inconel825 powder obtained for further application. Fig.1 shows
the scanning electron microscopy (SEM) image of the Inconel825 powder obtained after ball
milling and being used for the present experiments. Table 1 represents the chemical
composition of Inconel825. From the SEM image, it is revealed that 5-25 µm particle size
Inconel825 powder attained after ball milling of Inconel825 chips. Comparing the EDS
analysis of the Inconel825 powder (as illustrated in Fig.1) and composition of commercial
Inconel825 (demonstrated in Table 1) some discrepancy in the percentage of the elements
can be noted. This may attribute to the induction of ball material with the actual Inconel825
powder during the milling process, which causes enhancement in the Fe percentage in the

4
final Inconel825 powder. Higher percentage of C in the produced powder perhaps witnessed
due to the use of carbon tape for holding the powder. The XRD spectra for the Inconel 825
chip and the powder obtained from the chip after ball milling as illustrated in Fig.2 are
equivalent to the spectra of Ni-Cr-Co-Mo alloy, which is corresponding to the Inconel825.
Careful analysis of the XRD plot indicates the broadening of the peaks after ball milling,
which may attribute to the refinement of the Inconel825 powder.

2.2. Preplacement and TIG arc scanning

The mixture of the Inconel825 powder and commercial pure TiC powder (Size: 2–5 μm,
99.5%, make- Alfa Aesar) was used as preplaced precursor. The TiC powder in different
weight percentage (20, 40 and 60 wt.%) was mixed with Inconel825 powder as detailed in
Table-2 and ball milled for 1 h to attain a uniformly distributed TiC-Inconel825 powder
mixture. The powder mixture was then blended with 10 % poly-vinyl alcohol (PVA) solution
to make a semi-solid paste by continuous stirring. The paste like solution of TiC-Inconel825
with different percentage of TiC were then pre-placed on AISI 304 steel plate of 100 mm ×
50 mm × 8 mm dimension with the help of mask of different thickness (0.7 mm and 1 mm).
Consequently, different thickness TiC-Inconel825 preplaced coating with different
percentage of TiC was obtained on AISI 304 steel substrate after drying the pre-coated
samples at room temperature. The dry pre-deposited steel samples were then heated in a
muffle furnace within argon atmosphere at 80 oC temperature for 30 minutes to cure the PVA
and remove any moisture present in the pre-coated layer. After drying and curing, the pre-
deposited coating thickness varying within 5% deviation of the mask thickness. The TIG
cladding was accomplished with the help of a TIG welding setup (Make: Fronious), in which
the welding torch was attached to a semi-automated movable tractor to attain a uniform scan
speed. A series of parameters, including preplaced powder composition or percentage of TiC
(20, 40 and 60%), preplaced layer thickness (0.7 and 1 mm) and processing current
(depending on the preplaced powder thickness) were varied and experiments were carried out
as per the planning demonstrated in Table 2. For all the experiments scan speed was fixed at
2.3 mm/s.
To investigate the influence of TiC percentage on the microstructure of the composite
coating, three different types of samples with different percentage of TiC in the precursor
were prepared. Heat input during the TIG cladding process was varied by changing the

5
welding current at 70, 80 and 90 A for 0.7 mm thick pre-coated samples, and at 90, 100 and
110 A for 1 mm thick pre-coated samples respectively. Specific heat input for each condition
was assessed from the heat input equation for TIG welding as suggested by Rasool et al.
(2015) and illustrated in Table 2. For the present case, the heat absorption coefficient
considered as 48% and the voltage was fixed at 15 V. A 2.4 mm diameter tungsten electrode
was used to generate the arc and argon gas was supplied through the nozzle for shielding and
stabilizes the arc between the pre-coated substrate and the electrode. To retain a constant arc
interaction area with the sample for the entire set of experiments, the distance between the
electrode tip and the work-piece was maintained at 3 mm. Single line arc scan was performed
on the pre-deposited coating by varying the current for each type of coated sample i.e.
different composition and pre-deposited coating thickness. In order to avoid the influence of
previous scan, approximately 6 mm gap was maintained between two consecutive tracks, and
sufficient cooling time was allowed before scanning the next track. Fig.3 illustrates the
schematic of TIG cladding process employed for the present experiment.

2.3. Characterization of the coating

After the accomplishment of TIG cladding with different combination of TiC-Inconel825
powder and processing current, the residual powder from the un-melted zone was removed
and the processed samples were cleaned with acetone. The coated samples were then cut at
the transverse cross section of the track with the help of wire-EDM for further analysis.
Polishing was done at the cross-section of the coating with SiC-based polishing paper (220,
600, and 1200 grade sequentially) and finally with 1 μm diamond paste. The polished
samples were then undergone for the micro-hardness measurement and microstructural
analysis. The microstructure of the coating was evaluated through scanning electron
microscope (JEOL JSM-T330) with back scattered electron (BSE) detector. The elements
present in the produced composite coating and their distribution was analyzed through energy
dispersive spectroscopy (EDS) attached with the SEM. The phase constitution present on the
produced coating was investigated with a Rigaku Smart Lab X-ray diffractometer (XRD).
The micro-hardness of the coating was measured on the polished cross section using a
Vickers micro indentation tester (Leco LM810) with 50 gf load and 10 second dwell time.
The measurement was taken along the depth from the top surface of the coating at an interval
of 100 µm at the center region of the track.
To assess the wear behavior of the produced TiC-Inconel825 composite coating, at first 3.5
mm diameter pin was cut from each of the coating track. The coated pins were then tested
6
against fine graded alumina abrasive disc (as a counter plate) using a pin-on-disc type wear
test rig (ASTM G99, Make: Magnum). Fig.4 illustrates the schematic diagram as well as the
experimental setup of the pin-on-disc type sliding wear tester used for the present experiment.
Prior to performing the wear test, the coated surfaces of the pins were polished to remove any
major undulation induced at the track during the TIG cladding process. During the sliding
abrasive wear test, the variation of wear in terms of height loss of the pin was acquired
through an integrated data acquisition system attached with the pin-on-disc test rig. In
addition, the height loss of the coated pin was also measured directly by using a Vernier
caliper (least count of 0.01 mm). The coefficient of friction of the coating was also recorded
during the test and plotted against the test time.

3. Result and discussion:

3.1.Coating morphology
Since, microstructure of any coating has prevailing effect on its properties; a detailed
microstructural study of the produced coating is indispensable to evaluate its mechanical
performance. In this study, the morphology of the coating microstructure was investigated to
comprehend the effects of TiC content in the Inconel825 matrix and the processing current.
Fig. 5(a-c) illustrates the SEM images of the cross-section of TiC-Inconel825 composite
coating produced with preplaced layer thickness of 0.7 mm and processing current of 70 A
for using different percentage of TiC (20, 40 and 60%) in the precursor. The images of the
coating cross-section clearly indicate that almost uniform thickness composite layer formed
on the substrate for using a particular percentage of TiC in the precursor. It is also evident
that for using 20% TiC in the precursor, no interfacial gap formed between the coating layer
and the substrate. On the other hand, for using higher percentage of TiC (40 and 60%), an
interfacial gap appeared between the coating and the steel substrate. As the melting
temperature of TiC (~3000 oC) is considerable higher than the Inconel825 alloy (1400 oC), it is
postulated that with the increases in TiC percentage in the precursor, the amount of heat
energy require to melt the pre-deposited layer become higher. As a result, for using higher
percentage of TiC in the precursor, melting of the substrate surface restricted, and a gap
appeared at the coating substrate interface.

The EDS analysis of the selected coating zone corresponding to Fig. 5(d-f) was performed
and the percentages of elements present in the entire area of the images are illustrated in

7
Table 3. The table clearly indicates that for the lower content of TiC (20%) in the precursor,
Ti and C percentage in the coating layer is relatively low and with the increase in TiC
percentage in the precursor, the percentage of Ti and C in the coating region enhances
gradually. In contrast, the percentage of Fe, Ni, Cr, and Mn decreases with the increase in
TiC percentage in the precursor.

Vigilant investigation of the high magnified SEM images (Fig. g-i) revealed that for using
lower percentage of TiC (20 and 40%) in the precursor, equiaxed type TiC structure induces
in the coating morphology. This may attribute to the fact that, for using lower percentage of
TiC, the applied heat facilitates to melt both the Inconel825 and TiC powder in the preplaced
layer. During solidification of the molten pool, owing to higher melting temperature of TiC,
and fast cooling (for a moving heat source), the molten and dissolved TiC starts nucleating
and grow as equiaxed structure in the Inconel825 matrix. Careful observation of the images
clearly shows the dispersion of blocky or equiaxed shaped TiC particles in the matrix. In this
respect, work of Hong et al. (2013), on laser direct metal deposition of TiC-Inconel718
composite can be referred. They revealed that at elevated specific energy, the TiC
reinforcement appeared in the matrix either as smooth, rounded, and un-melted particles
surrounded by an interfacial layer or as refined dendritic structure, which formed after
complete melting of TiC particle and re-solidification. It is also relevant to point out that
cooling rate of the melt-pool enhances with the increase of TiC particles in the preplaced
powder mixture (Wilson and Shin 2012). As thermal conductivity of TiC particle (30
W/m/K at room temp) is much higher than that of Inconel825 (11.1 W/m/K at room
temperature), it may anticipate that the heat accumulation within the melt pool must be lower
for higher percentage of TiC in the precursor. Consequently, the melting of base material
should be restricted due to low temperature resulted from lower heat accretion in the molten
pool.

In order to identify the different shaded region (black and white) in the coating morphology,
high magnified SEM image and corresponding EDS analysis were performed for the coating
produced with 60% TiC as demonstrated in Fig.6. The EDS elemental analysis corresponding
to this black or dark and white or light shaded region is tabulated in Table 3. The table
illustrates that the dark reinforced particles (marked as ‘1’) are predominantly composed of
high percentage of Ti and C. In contrast, the white matrix zone as marked ‘2’ shows the
presence of Cr, Fe, and Ni elements in combination with minor amount of Ti and C.
Therefore, it may infer that the TiC particles (dark region) are uniformly reinforced in

8
Inconel825 matrix (light shaded zone) and yielded a composite layer after the TIG cladding
process.

Fig.7 illustrates the SEM images (at different magnification) of TiC-Inconel825 coating
produced with 60% TiC, 0.7 mm thick preplaced layer and different processing current i.e.
70, 80 and 90 A. From the images of the coating layers (Fig.7a-c), it is evident that for all
different current condition, a thick and almost uniform coating layer deposited on the steel
substrate. It is also revealed that due to the presence of large percentage of TiC in the
precursor, for all different current condition, interfacial gap appeared between the coating and
the substrate. As discussed earlier, in consequence of high melting temperature of TiC, the
required energy for the melting and mixing of the coating layer with the substrate is
significantly higher. For the present condition, the employed processing current perhaps
inadequate to melt and mix the TiC-inconel825 layer with the substrate and produces
interfacial gap.

From the magnified images (Fig.7d-f) of the coating zone, highly dense TiC particle
reinforced Inconel825 MMC can be seen for all different current condition. The images also
revealed that the reinforced TiC particles are partially melted during the TIG arc scanning
and produces spherical shaped morphology. No dendrite or equiaxed structure formed in the
coating microstructure, which indicates inadequate melting of TiC particles within the
Inconel825 matrix for using 60% TiC in the precursor. Careful investigation of the high
magnified SEM images (Fig.7g-i), and corresponding EDS analysis as illustrated in Table 5
revealed that with the increase in processing current, the percentage of Ti and C in the
coating reduces gradually. In contrast, the percentage of Fe along with other elements of
Inconel825 i.e. Ni, Cr, and Mn on the coating zone augmented as the processing current
increases. This is perhaps due to the enhancement of the matrix percentage owing to partial
dilution of steel substrate with the Inconel825 matrix at relatively higher temperature attained
at higher processing current.

The mechanical performances of metal matrix composites (MMCs) are governed by the
interfacial strength between the reinforced particles and the metal matrix. In consequence of
poor wettability of the ceramic particle with the metal matrix, the particle-matrix interfacial

9
bond is very poor that causes impulsive failure of the composite, especially under high
mechanical load. This is attributed to differences in physical, thermal and mechanical
properties of the reinforced particles and the matrix. Hong et al. (2013) demonstrated that
suitable combination of matrix material and ceramic particles, those are having high mutual
affinity, may augment the interfacial bond. It is also postulated that at elevated temperature,
formation of a reaction layer between the reinforced particle and metal matrix improves the
wettability between them that resulted in a superior interfacial bond.

High-magnified SEM image of the TiC-Inconel825 composite coating produced with 60%
TiC, for 1 mm preplaced thickness and 100 A processing current as depicted in Fig. 8, shown
that a relatively light shaded interfacial layer of approximately 0.6 μm thickness formed
surrounding the reinforced TiC particle. The EDS line-scan performed through this region
between the reinforced TiC particle and matrix as marked in Fig. 8 revealed that the
reinforced dark particle is rich in Ti and C (between c-d zone) while Cr, Fe, and Ni are highly
concentrated in the matrix zone (between a-b). Careful investigation of the EDS line scan
revealed that in addition to Ti and C, the light shaded interfacial zone (between b-c) contain
significant amount of Cr, Fe, and Ni. Therefore, it may postulate that the elements of
Inconel825 matrix partially reacted with the TiC and produces some intermetallic or Ni/Cr
carbides. A similar type of observation was reported by Hong et al. (2013) for laser cladding
process, where the authors shown that in the interface zone of TiC-Inconel 718 composite
coating, the concentration of Nb and Mo elements enhanced significantly due to the
formation of (Ti-Nb/Mo)C interfacial layer.

Similarly, the morphology of the TiC-Inconel825 coating produced with 60% TiC, 1 mm
preplaced layer thickness and different processing current (90, 100 and 110 A) are shown in
Fig.9. It is worth to emphasize that owing to higher preplaced layer thickness relatively
higher current was considered to melt the preplaced layer. The SEM images taken at the
cross-section of the coating revealed that for employing 90 A current, a uniform coating
formed. However, it was found that the bonding of coating layer with the substrate formed at
the center region of the track only, where the intensity of the arc is maximum. In contrast, for
applying higher processing current (100 and 110 A), the preplaced layer melt along with the
upper layer of the base material and produces a coating with superior bonding.

10
From the magnified images of the selected region as depicted in Fig.9 (d-f), it is apparent that
the coating produced with 90 A current, predominantly consist highly dense TiC particles;
whereas, in the coating produced with 110 A current, the TiC particles are diluted in the
matrix and produces a low dense TiC reinforced coating layer. It is interesting to note that for
using 100 A current, the produced coating exhibits non-uniform distribution of TiC (Fig.9e
(i) and (ii)). Depending on the variation in heat intensity and solidification rate at different
region, highly dense TiC reinforced zone or almost diluted TiC reinforced zone appeared in
the coating layer. It may be postulated that for 100 A current, the induced heat energy
completely melt the Inconel825 matrix along with partially melting of preplaced TiC powder.
The EDS analysis corresponding to Fig.9 (d-f) as illustrated in Table 6 revealed that for
applying 90 A current, the percentage of Ti in the coating region is reasonably high (35.53%),
whereas for employing 110 A current, the percentage of Ti in the coating reduces
significantly (10.86%). Remarkably, for the coating processed with 100 A current, it is found
that indiscriminate morphology of the coating in different region contains variable percentage
of Ti, i.e. for dense zone 31.58% and for diluted zone 7.15%.

3.2. Micro-hardness
To assess the hardness value of the produced TiC-Inconel825 composite coating and its
variation with the depth of the coating, micro-hardness was measured at the cross-section of
the coating. Fig.10 -12 represent the micro-hardness profile measured against the depth of the
coating from the top surface for the samples processed with different conditions.
Fig. 10 shows the variation of micro-hardness value for the coatings produced with precursor
containing 20, 40 and 60 % TiC, 0.7 mm preplaced layer thickness and processing current of
70 A. The plot indicates that the micro-hardness values along the cross section of the coated
samples are varying significantly with the distance from the top surface of the coating.
Furthermore, a large variation in the coating hardness also observed for using different
percentage of TiC in the precursor. It is clearly evident that for using 60 % TiC in the
precursor, the maximum micro-hardness value of the coating zone reaches upto 1100 HV0.05.
Nevertheless, for using 20 and 40 % TiC, the maximum hardness value at the coating region
recorded approximately 600 and 700 HV0.05 respectively. It was also found that for using 60
and 40% TiC in the coating, the hardness value suddenly reduced to 400 HV0.05 after a depth
of approximately 500 µm. On the contrary, for the coating produced with 20 % TiC, the
hardness value reduces gradually with the depth of the coating and reaches the hardness value
of the substrate material (240 HV0.05).

11
As the hardness of the composite predominantly depends on the percentage of hard particles,
it is expected that with the increase in TiC content in the precursor, the micro-hardness value
of the TiC-Inconel825 coating should be enhanced gradually. In contrast, for using a lower
percentage of TiC, the concentration of TiC in the coating zone is relatively less, which is
responsible for lower micro-hardness of the coating. This variation in the hardness values
along the depth of the coating attributed to the variation of TiC concentration in the
Inconel825 matrix or due to the microstructural changes along the cross-section because of
the variation in cooling rate. The SEM images of the cross-section of the coating (Fig.5b-c)
revealed that for using 60 and 40% TiC, no interface zone between the coating and substrate
formed, which causes a steep reduction in the hardness value as compared the coating layer.
On the other side, for using 20% TiC in the coating (Fig.5a), owing to the formation of an
interface zone for proper mixing of the pre-deposited coating layer with the substrate surface,
a gradual reduction in the hardness value observed.
Similarly, to evaluate the effect of applied current, micro-hardness value was measured for
the coating produced with different current, when other conditions are unchanged. Fig.11
shows the variation of micro-hardness value along the depth of the coatings produced with 60
% TiC, 0.7 mm preplaced thickness and processing current of 70, 80 and 90 A. It is evident
from the plot that, the hardness value at the coating region is in the range of 700 to 1100
HV0.05, and beyond that the micro-hardness value reduces gradually. Careful observation of
the plot revealed that the hardness value is relatively higher for the coating processed with 70
A current, and with the increase in processing current, i.e. for 80 and 90 A, the hardness value
of the coating reduces marginally. With a higher percentage of TiC (60%) in the precursor,
all the coatings produced with different processing current exhibits high value of micro-
hardness in the coating region, and with the increase in depth, the hardness value diminishes
steadily. No significant difference in the hardness value was observed in the coating zone for
the variation of processing current. The precise evaluation of the plot revealed that in
consequence of higher heat input and corresponding dilution of TiC in the molten Inconel825
matrix and partially melted steel substrate, the hardness of the coating reduces marginally for
higher processing current (80 and 90A).
Fig.12 illustrates the hardness profiles of the coating produced with 60% TiC, 1 mm
preplaced layer thickness and processing current of 90, 100 and 110 A. From the plot it is
clearly evident that for using 90 A current, the micro-hardness value of the coating zone is

12
reasonably high (upto 1000 HV). Nevertheless, the hardness value of the coating zone
reduced significantly for employing higher current (100 and 110 A). It is obvious that the
micro-hardness value of the coating predominantly differs depending on the concentration of
the TiC particles. In the present case, for employing lower current (90A), a uniform and
densely distributed TiC layer formed (as shown in Fig.9a), which exhibits relatively higher
micro-hardness. In contrast, for using higher processing current (100 and 110 A), high
temperature induces in the processed zone, and the pre-deposited layer melted completely
along with the upper layer of the substrate and consequently a diluted TiC reinforced coating
layer yielded on the substrate surface. In addition, when the TiC particles completely melted,
during solidification of the molten pool, part of the molten TiC particles nucleated, and a
small fraction of the molten TiC diffuses within the molten matrix of Inconel825. It is also
possible that this molten TiC reacted with other constituents of the matrix material and
produces carbides with relatively lower hardness value than those of TiC. The EDS analysis
corresponding to the high magnified SEM image (Fig.8) clearly indicates the presence of C
in the matrix zone of the coating, which confirms the dilution of TiC within the molten
matrix.

3.3.XRD analysis
X-ray diffraction (XRD) patterns of TiC-Inconel825 composite coating produced on AISI
304 steel by TIG cladding process for using different percentage of TiC (20, 40, 60 %) in the
precursor, preplaced layer thickness of 0.7 mm and 70 A processing current are illustrated in
Fig.13. The analysis of the XRD patterns revealed the presence of TiC and Ni-Cr-Co-Mo
(which represent the Inconel825) phases on the coating surface for all the samples produced
with different percentage of TiC. Nevertheless, other than TiC and Inconel825, no other
phase was detected in the coating surface. Careful analysis of the patterns also revealed that
the relative intensity of TiC peaks at [200], [220], [311] and [222] plane increases, whereas
the intensity of Inconel-825 peak at [200] and [220] plane reduces for the increasing TiC
percentage in the precursor from 20 to 60 %. Concurrently, it is also observed that the
intensity of TiC [111] peak reduces and intensity of Inconel825 [111] peak increases with the
increase in TiC percentage. However, the relative percentage of TiC in the TiC-Inconel825
composite coating as measured from the relative peak height intensity by considering all the
peaks show that for increasing the TiC content in the precursor, the percentage of TiC in the
coating gradually enhances. It was revealed that for using 20, 40 and 60% TiC in the
precursor, the measured TiC percentage in the coating are 21.52, 37.55, and 42.95 %

13
respectively. It is interesting to note that for using 20 and 40 % TiC in the precursor the
percentage of TiC in the coating almost equal to the supplied TiC; however, for using 60%
TiC, relatively low percentage of TiC attained in the coating through XRD analysis. This is
perhaps due to the fact that during TIG coating process, with the increase in TiC percentage,
a certain fraction of TiC powder diluted in the Inconel825 matrix as well as in the steel
substrate. Consequently, the percentage of TiC phase in the upper layer of the coating reduces
as compared to the supplied TiC, which causes a reduction in the TiC percentage in the
coating as measured through XRD analysis.

3.4.Sliding Abrasive Wear

In order to assess the wear characteristic of the produced TiC-Inconel825 MMC coating, the
pin cut from the coated samples were slid against fine graded Al2O3 abrasive disc (average
roughness of 15 µm), using a pin-on-disc type sliding wear test rig. The wear of the coated
pins due to sliding against abrasive disc was measured in terms of height loss of the pin. Fig.
14 shows the wear or height loss of the coated pins (processed with different current) and the
uncoated steel pin after the sliding abrasive wear test performed with a sliding speed of 157
mm/s and normal load of 10 N. From the plot it is clearly evident that the sliding abrasive
wear or the height loss of the TiC-Inconel825 coated steel pin largely depends on the
processing current. It is obvious that the height loss of the coated samples after the wear test
is reasonably lower than the height loss of the uncoated steel pin under equivalent condition.
It is also found that the height loss of the coated pin increases with the increase in processing
current employed to produce the coating. Depending on the processing condition, the height
loss of the coated pins was recorded in the range of 0.1 to 0.34 mm, whereas for uncoated
steel pin, the height loss was noted as 0.7 mm under similar test condition.

The cumulative wear of the coatings with the time of test was also acquired during the test
through a data acquisition system attached with the wear test rig. Fig. 15 illustrates the
cumulative wear of the TiC-Inconel825 coating processed with 60% TiC, 1 mm coating
thickness and different processing current. The plot indicates that the wear characteristics of
the coatings are almost comparable with the height loss measured directly by Vernier caliper.
For all the cases, at the initiation of the test, a rapid and inconsistent wear in terms of height
loss was recorded, and after a specific period of time, the rate of removal of the coating
become steady.

14
Since, the test samples (coated pin) were acquired from the single line scan by TIG cladding
process, some undulation was present on the coating surface, specifically a concave curved
surface formed on the coated pin. Therefore, at the initiation of the test, the contact area
between the coated pin surface and the alumina abrasive disc was found relatively less, which
leads to an enhancement of force per unit area on the coated surface. Subsequently, a rapid
removal of the coating surface occurred at the contact region. However, with an assumption
of similar phenomenon for all the samples, a relative wear behavior has been illustrated in the
present study. The cumulative wear or height loss (Fig. 15) represents the collective wear of
the coated pin as well as the counter-body (alumina disc) as obtained through the data
acquisition system. It is expected that at the initiation of the test, due to high frictional force
per unit area, lightly bonded Al2O3 particles from the abrasive disc removed out, which shows
higher total height loss as compared to the wear measured through Vernier caliper.

It may also comprehend from the plot that the TiC-Inconel825 composite coating produced
with lower current (90A) exhibits lower height loss as compared to the coating produced with
100 and 110 A current. For using 60% TiC in the preplaced powder mixture and 90 A
processing current, owing to low heat input, dilution of TiC particles become less within the
Inconel825 matrix as well as partially melted steel substrate. Nevertheless, with the increase
in applied current, the heat input in the processing zone enhances which causes a larger melt-
pool volume, and consequently stimulates the TiC particles to dilute in the matrix with a
larger depth. Thus, a relatively softer coating layer formed, which leads to high wear of the
coating under similar test condition. It is interesting to note that the cumulative height loss
recorded from the wear test rig is marginally higher than the height loss of the coating
measured through Vernier caliper. As discussed earlier, during the wear test, along with the
removal of the coating, the abrasive disc was also eroded owing to the dislodging of the
loosely bonded abrasive particles. Thus, the height loss acquired by the test rig is the
combination of actual wear of the coated pin and wear of the abrasive disc. In this context, it
is relevant to mention that the coating produced with lower processing current found not
suitable for wear test due to the formation of interfacial crak between the coating and the
substrate.

Fig.16 shows the SEM images of the worn surface (after the sliding abrasive wear test against
alumina abrasive disc) of the TiC-Inconel825 composite coating produced with 60%TiC and
processing current of 90, 100 and 110 A. The images indicate that after the wear test, almost
smooth and flat surface appeared without bulk removal or delamination of the coating. The

15
magnified images of the selected region show the scratches or micro cavities formed on the
worn surfaces owing to rubbing effect of the alumina abrasive particles. Careful investigation
of the images revealed that for the coating processed with higher current i.e. 100 and 110 A,
relatively wider scratches or grooves induces in combination with bulk removal of the
coating material. These wide grooves are appeared in the TiC-Inconel825 composite coating
due to the plowing action of the alumina particles on the coating surface for lower
concentration of TiC (due to dilution at higher processing current), which leads to severe
wear of the coating for the samples produced at higher current.

3.5. Coefficient of friction

During the sliding abrasive wear test of TiC-Inconel825 composite coating against alumina
abrasive disc, the coefficient of friction (COF) was also recorded through online data
acquisition system. Fig. 17 shows the COF of the coating for applying 10 N normal load and
157 mm/s sliding velocity. From the plot, it is seen that at the initiation of the test, when a
rapid height loss occurred, the COF of the coating enhances significantly with a random
variation. Nevertheless, after a certain period of time (depending on the processing condition
of the samples), the COF value reduces and become steady at a value of 0.59. Under similar
test condition, it was observed that the COF of the uncoated steel is almost steady at 0.48. It
is expected that at the initiation of the test, the rough surface or the curved edges of the
coating removed rapidly due to lower contact area and corresponding high frictional force,
which leads to higher COF. After a certain period of test, as the rough surface of the coating
become smooth or the curved edges become flat, full contact between the coated pin and the
alumina abrasive wheel occurred and exhibits a steady COF value. Critical evaluation of the
plot indicates that the coating produced with lower current reaches the steady state condition
faster than the coating processed with higher current. At higher current, because of higher
heat energy, the possibility of deformation of the top surface of the coating layer is high,
which induces a larger curved surface. Now, during wear test, to attain a smooth surface or
reach the steady state condition, the sample processed with higher current required a longer
time. It is also evident from the plot that for the coating produced with 90 A current, the COF
value increased after 125 S. This is perhaps due to the exposure of rough surface or
occurrence of three-body abrasive wear due to removal and entrapment of the abrasive

16
particles between the coated surface and the abrasive wheel, which may be considered as
unexpected result in the test.

Conclusions

A hard and wear resistance TiC reinforced inconel825 based metal matrix composite coating
has been deposited on AISI 304 steel by TIG cladding process, which has inordinate potential
to work under extreme abrasive environment.

The pre-deposited coating thickness, TiC percentage in the precursor mixture, and the
processing current have significant effect on the morphology of the coating, which leads to
specific variation in the hardness value and the wear resistance properties of the coating.

Owing to higher percentage of TiC in the precursor and for employing relatively lower
current the induced heat energy become inadequate that leads to formation of interfacial gap
between the coating and the substrate.

The employed processing current has significant effect on the the microstructure of the
coatings, which directly govern the micro-hardness and wear characteristic of the produced
TiC- inconel825 composite coating.

The micro-hardness value of the produced TiC-Inconel825 coating found in the range of 400-
1100 HV0.05 depending on the TiC content and processing conditions, which is more than four
times higher than the as received steel substrate.

Owing to superior wetting behavior of Ni based alloy with both TiC and steel, inordinate
bond between the TiC particle and the matrix occurred that leads to restriction of the removal
of TiC particles during sliding wear test and subsequently enhances the sliding abrasive wear
resistance of the coating.

Acknowledgement

The authors thankful to Tijo D and Kamlesh Kumar (Ph.D. scholars, Department of
Mechanical Engineering, NIT Rourkela) for their technical support to conduct the
experiments in various stages. The authors also acknowledge the financial support of SERB

17
(DST), New Delhi (SB/FTP/ETA- 0295/2013) for the “micro-hardness tester” and “Pin-on-
disc wear tester”.

18
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19
 Element Wt.%
Ni 36.9
Fe 28.08
Cr 19.98
Mo 2.72
Ti 3.44
Mn 1
C 7.4

Fig. 1: SEM image and corresponding EDS spectroscopy of Inconel825 powder (obtained from the
ball milling of Inconel825 chip) used for present experiment

1600
[111]

1400
[200]

1200 [220]
Peak Intensity [a.u]

1000
Inconel 825 powder
800

600

400

200
Inconel 825 Chip
0
30 40 50 60 70 80 90 100
2 

Fig. 2: XRD spectra of Inconel825 chip and powder obtained from the ball milling of Inconel825 chip

20
Fig. 3: Schematic of TIG cladding process

Normal Load
Pin
Holder

Coated Pin

Rotating
Abrasive disc

Fig. 4. (a) Schematic and (b) actual experimental setup of pin-on-disc sliding abrasive wear test rig

21
(a) (b) (c)

(d) (e) (f)

(g) (h) (i)

(20%TiC) (40%TiC) (60%TiC)

Fig. 5: SEM images of the cross-section of the coating (at different magnification) produced with
preplaced layer thickness of 0.7 mm, welding current 70 A, and scan speed of 2.3 mm/s for using
different percentage of TiC in the precursor

Fig. 6: High magnified SEM image and corresponding EDS analysis of the dark reinforced particle
and light shaded Fig matrix zone of the coating produced with 60% TiC, preplaced layer thickness of
0.7 mm, and welding current 70 A

22
(a) (b (c
) )

(e (f
) )

(g (h (i
) (70 A) ) (80 A) ) (90 A)

Fig.7: SEM images of the cross-section of the coating (at different magnification) produced with
preplaced layer thickness of 0.7 mm, 60% TiC in the precursor and welding current of (a) 70 A, (b) 80
A and (c) 90A

b c

Fig.8: High magnified SEM image of the reinforced particle and EDS line-scan through the dark
particle, light shaded interface and white shaded matrix region between the reinforced TiC particle
and matrix

23
(a) (b (c
) )

(i) (ii)
(d) (e) (f)
(90 A) (100 A) (110
A)
Fig.9: SEM images of the cross-section of the coating (at different magnification) produced with
preplaced layer thickness of 1 mm, 60% TiC in the precursor and processing current of 90,100,110A.

1200
Current-70 A
Preplaced thickness- 0.7 mm
1000
Scan speed - 2.3 mm/s
TiC content
Micro-hardness (HV0.05)

800 20%
40%
60%
600

400

200

0
0 200 400 600 800 1000 1200 1400
Distance from top surface (m)

Fig.10 Variation in micro-hardness value against the depth for the TiC-Inconel825 coating produced
by TIG cladding process with 70 A current, 0.7 mm thick plreplaced layer for different percentage of
TiC in the precursor

24
 1200
TiC-60%
Preplaced thickness 0.7 mm
1000 Scan speed - 2.3 mm/s
Current
Micro-hardness (HV0.05)

800 70A
80 A
90 A
600

400

200

0
0 200 400 600 800 1000 1200
Distance from top surface (m)

Fig.11 Variation inmicro-hardness value against the depth of the TiC-Inconel825 coating produced by
TIG cladding process with 60% TiC, 0.7 mm thick preplaced layer and different processing current
1600

TiC -60%
1400
Preplaced thickness- 1 mm
Scan speed - 2.3 mm/s
1200
Micro-hardness (HV0.05)

Current
1000 90 A
100 A
800 110 A

600

400

200

0
0 300 600 900 1200 1500
Distance from top surface (m)

Fig.12 Variation in micro-hardness value against the depth of the TiC-Inconel825 coating produced
by TIG cladding process with 60% TiC, 1 mm thick preplaced layer and different processing current

25
 TiC
=Inconel 825

 [111]
/(Ni-Cr-Co-Mo)

 [200]

 [200]

 [311]

 [222]
 [220]
 [111]

 [220]
Relative intensity

60%TiC

40%TiC

20%TiC
0
20 40 60 80 100
2

Fig. 13: XRD spectra for the TiC-Inconel825 coating produced by TIG cladding process for using 0.7
mm thick preplaced layer, 70 A processing current and different percentage of TiC (20, 40, 60 %) in
the preplaced powder mixture

0.8
Preplaced thickness-1 mm
TiC content-60%
Sliding Speed-157 mm/s
0.6 Normal load-10 N
Wear (height loss) [mm]

0.4

0.2

0.0
Substrate 90 100 110
Processing Current [A]

Fig. 14: Height loss after the pin-on-disc type wear test against alumina abrasive disc of uncoated
ASIS 304 steel substrate and TiC-Inconel825 coated pins produced with 1 mm thick preplaced layer,
60% TiC and different processing current

26
 Current
Preplaced thickness-1 mm
Cumulative wear or height loss (m)
300 90 A
TiC content-60%
100 A
Sliding speed- 157 mm/s
110 A

200

100

0 50 100 150 200 250 300

Time (S)

Fig. 15: Cumulative height loss or wear characteristic of TiC- Inconel825 coating produced with 1
mm thick preplaced layer, 60% TiC and different processing current (90, 100, 110 A) against alumina
abrasive disc during the wear test

Scratches

Micro-cavities

(a)

Plowing

Wide scratches

(b)

Plowing
Scratches

(c)

Fig. 16: SEM images of the worn out surface of 60%TiC-Inconel 825 coating produced by
TIG cladding process with processing current of (a) 90A, (b) 100 A, and (c) 110 A

27
 1.0
90 A Preplaced thickness-1 mm
100 A TiC content-60%
0.9
110 A Sliding speed- 157 mm/s
Substrate
0.8

0.7
COF

0.6

0.5

0.4

0.3
0 50 100 150 200 250 300
Time(secs)

Fig.17: Variation in coefficient of friction (against alumina disc) of uncoated steel substrate and TiC-
Inconel825 coating produced with 1 mm thick preplaced layer, 60% TiC, and different processing
current (90, 100, 110 A)

28
Table 1: Chemical composition of commercial Inconel825 (wt.%)

Ni Fe Cr Mo Cu Ti Mn Si Al C S
38–46 22 19.5–22.5 2.5–3.5 1.5–3 0–1.2 1 0.5 0.2 0.05 0.03

Table 2: Experimental condition and basic observation from the coating cross-section
Expt. Preplaced TiC% Current Heat Observation
No. thickness [A] Input
[mm] [J/m]
1 0.7 20 70 0.2191 Gradient mixing with
substrate
2 0.7 40 70 0.2191 Interfacial crack
3 0.7 60 70 0.2191 Interfacial crack
4 0.7 60 80 0.2504 Interfacial crack
5 0.7 60 90 0.2817 Interfacial crack
6 1 60 90 0.2817 Partial crack at the interface
7 1 60 100 0.313 Coating layer partially
diluted with substrate
8 1 60 110 0.3443 Coating layer diluted and
gradient mixing with the
substrate

Table 3: EDS analysis corresponding to SEM images shown in Fig5(d-f)

Sample C Ti Cr Mn Fe Ni
20% TiC (Fig.5d) 12.15 9.87 14.69 3.65 40.93 18.71
40% TiC (Fig.5e) 16.70 23.72 12.63 1.21 30.91 14.83
60% TiC (Fig.5f) 24.78 35.62 9.19 0.49 17.47 12.45

Table 4: EDS analysis corresponding to SEM images of Fig 6

Sample C Ti Cr Mn Fe Ni
Black zone (1) 27.01 52.41 4.50 1.09 12.47 2.52
White zone (2) 15.45 6.73 14.87 3.81 28.96 32.45

29
Table 5: EDS analysis corresponding to SEM images of Fig.7(g-i)
Sample C Ti Cr Mn Fe Ni
70A (Fig.7g) 24.78 35.62 9.19 0.49 17.47 12.45
80A (Fig.7h) 22.06 32.5 10.18 1.08 21.07 13.1
90A (Fig.7i) 21.39 26.55 10.22 2.75 28.88 10.22

Table 6: EDS analysis corresponding to Fig. 9(d-f)

Sample C Ti Cr Mn Fe Ni
90A (Fig.9d) 21.50 35.53 9.07 1.35 23.34 9.21
100A (i) (Fig.9e) 9.79 7.15 14.14 7.06 58.77 3.60
100A (ii) (Fig.9e) 20.67 31.58 10.68 0.80 21.29 14.97
110A (Fig.9f) 8.09 10.86 15.93 6.28 56.25 5.10

30