Chapter 11

Microstructural and Microhardness

Analysis of Nickel-Based Ceramic
Composite Coating on AISI 304 Stainless
Steel by TIG Coating Method

Anjani Kumar , Neeraj Singh , Sonu Nagar and Anil Kumar Das

Abstract In present work, nickel-based metal matrix composite (MMC) coating was
produced on AISI 304 stainless steel by tungsten inert gas (TIG) coating technique.
TIG heat source used to develop intermetallic bonding between coating and substrate.
The metal ceramics composition was employed viz. Ni + SiC and Ni + Si + B4 C.
Two different proportions of SiC and B4 C in coating mixture were used and assess
their effect on microstructure and microhardness. Field emission scanning electron
microscopy (FESEM) analysis revealed that fine martensitic microstructure evolved,
for S4 (85%Ni + 7.5%Si + 7.5%B4 C) sample. For this, maximum microhardness and
average hardness of coated layer were found 676 HV0.1 and 523 HV0.1, respectively,
whereas average hardness of substrate was 200 HV0.1 . The overall result concludes
that Si + B4 C is better choice in comparison to direct inclusion of SiC in nickel-based
MMC fabrication.

Keywords TIG coating · FESEM · Microhardness · Silicon carbide

11.1 Introduction

AISI 304 stainless steel is extensively used in various engineering application like
automobile, agricultural equipment, manufacturing industries, milk and food pro-
cessing unit [1–3]. Although, stainless steel has high stiffness, corrosion resistance
and strength, but their surface hardness and wear resistance are not enough to survive
sliding motion against high load [4]. This leads to hamper the multifaceted appli-
cation of AISI 304 steel in the practice [5]. The surface coating process is recently
evolving as attractive coating technique, which has potential to improve weakness
of steel and make it versatile and cost effective. In recent decades, incorporation of
metal matrix composites layer on ordinary metal through coating has been gained
attention to researcher. The metal matrix composite consists of two phases: one
is matrix (ductile phase) and other one is reinforcement (hard phase). The matrix
phase imparts ductility and toughness in composite, whereas reinforcements impart

A. Kumar (B) · N. Singh · S. Nagar · A. K. Das

Department of Mechanical Engineering, National Institute of Technology Patna, Bihar 800005,
India
© Springer Nature Singapore Pte Ltd. 2020 111
S. Yadav et al. (eds.), Proceedings of International Conference in Mechanical and Energy
Technology, Smart Innovation, Systems and Technologies 174,
https://doi.org/10.1007/978-981-15-2647-3_11
112 A. Kumar et al.

hardness and modulus of elasticity [6–8]. The ceramic material like, metal carbides,
hard oxides and nitrides such as SiC, TiC, TiB2 WC, B4 C and Al2 O3 are very hard
and wear resistance [9–14]. Moreover, alone ceramic material is incoherent for sur-
face coating on steel due to large melting-point difference, poor adhesion and low
fracture toughness. Typically, a transition metal is introduced in ceramic due to the
metal’s good ductility and toughness. Therefore, ceramics reinforced metal matrix
composite coating is good choice for surface improvement [4, 11]. Silicon carbide
is a promising ceramic material due to its excellent strength and wear resistance at
room and elevated temperature [15]. Silicon carbide is compatible with nickel (Ni)
because of high melting point and thermal conductivity almost similar.
In recent decades, several research groups are attempted to explore the TIG coating
characteristics and mechanical performance on steel with several compatible com-
bination of ceramic and transition metal. Bouyaz and Ulutan [5] reported in situ SiC
coating by TIG on 304 steel. Saroj et al. [16] fabricated TiC reinforced inconel825
metal matrix composite and achieved seven times more wear resistance than 304 steel
substrates. Çelik et al. [17] investigated SiC coating by TIG with different percent-
age of graphite powder and result found that improvement in wear characteristics.
Mridha [18] fabricated TiN in nitrogen environment by TIG on the surface of pure
titanium (Ti) plate and achieved hardness 2000 HV. Tosun [19] studied nickel-based
WC coating and observed microstructural changes and microhardness variation of
steel. All reported results evident that TIG coating is a viable technique for modi-
fication in stainless steel. There are still very few records available about SiC and
B4 C reinforced nickel-based composite, developed through TIG method. Through
this literature, authors try to add some more information in the field of TIG coating
by using some specific material.
In this investigation, the surface of AISI 304 stainless steel was coated with
preplaced layer of Ni + SiC and Ni + Si + B4 C, using TIG arc as heat source
for the melting of preplaced layer. The influence of SiC and B4 C proportion on
microstructure and microhardness is reported. It is hoped that this information could
give useful support to fabricate hard and wear resistant composite surface.

11.2 Experimental Procedure

First of all, AISI 304 stainless steel was taken as substrate material of size 100 × 50
× 10 mm3 and surface rubbed with 220 grades SiC emery paper to remove oxide
layer followed by cleaning with acetone to remove other oily contamination. The dif-
ferent powders: Silicon carbide (Size 400 mesh, purity 99%, make: Sigma Aldrich),
Boron carbide (Size 200 mesh, purity 98%, make: Sigma Aldrich), Silicon (Size 200
mesh, purity 98.5%) and nickel (Size 200 mesh, purity 98%) were used as coating
material; make: Sigma Aldrich. Four samples were prepared with different material
composition (shown in Table 11.1). The mixture of powders and 5% polyvinyl alco-
hol were blended with the help of magnetic stirrer to form homogeneous semisolid
paste. The polyvinyl alcohol works as binder and imparts strength in preplaced layer
11 Microstructural and Microhardness Analysis of Nickel-Based … 113

Table 11.1 Sample

identification and
corresponding composition
Sample identification Composition (by weight%)
S1 Ni (95) + SiC (5)
S2 Ni (85) + SiC (15)
S3 Ni (95) + [Si + B4 C = 1:1] (5)
S4 Ni (85) + [Si + B4 C = 1:1] (15)

to withstand arc pressure; higher concentration of polyvinyl alcohol causes forma-

tion of void and porosity. The paste was uniformly dispersed over the clean surface
and dried up to 72 h to remove moisture.
A semi-automatic TIG set-up, make: Electra TIG 200 DC, was used to generate
arc. The heat input was controlled by regulating current and scan speed of arc; the heat
input was calculated with the assistance of mention Eq. 11.1. The preplaced dried
sample was processed with TIG arc at optimum parameter (current 120 A, voltage
25 V, speed 2.297 mm/s and heat input 626.905 J/mm); the preplaced powder got
melted and form metallurgical bond with substrate upon solidification of melt pool.
The coated sample were sectioned and cold mounted for microhardness test. The
mounted sample was polished with standard metallurgical process; initially, sample
was polished on SiC emery paper from 220 to 3000 grades followed by diamond
paste on polishing cloth for mirror-like finishing. The morphology of coated sample
was carried out on FESEM (Make: ZIESS) to examine evolution of microstructure.

Q = η × V × I /v (11.1)

where, Q = heat input in (J/mm), ï = efficiency of heat transfer (0.48), V = voltage

in (Volt), I = current in (A) and v = scan speed in (mm/s).

11.3 Results and Discussion

11.3.1 Microstructural Analysis

The mechanical properties of coated layer depend on the morphology and distribution
of ceramic particle in the region. The details of composition are listed in Table 11.1.
Figure 11.1a shows different zone of coating; the coated layer, the interface layer
and the substrate. Figure 11.1a–c shows the microstructure of S1; which shows small
size SiC particles distribution in phases and irregular dendritic solidification occurs
for sample S1. Figure 11.2a–d shows micrograph of sample S2, in which Fig. 11.2b
shows a thick interface layer; the grain near to the substrate surface is equiaxed and
near to coated layer is irregular due to different solidification rate. As the percentage
of SiC increased the interface layer thicker and coated zone retain a fine dendritic
structure reinforced with grey SiC particle. This results due to rapid solidification and
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other reason also dominated due to larger different in melting point. In addition, the
dissociation of SiC will also form hard carbide phases in the coating. Furthermore,
the Marangoni effect in the melt pool increased the rate of heat dissipation, along with
the mixing of the hard phase, leading to the formation of finer dendritic structures.
Figure 11.3a–d shows morphology of sample S3 in which SiC formed by reaction
between Si and B4 C. A mixed grain was observed; the equiaxed grain, and irreg-
ular larger grains. Moreover, the eutectic phases also observed in coated layer in
Fig. 11.3c, d. Figure 11.4a–d shows micrograph of sample S4, in which 15% (Si
+ B4 C = 1:1) was used in powder mixture composition (details of composition in
Table 11.1). A thin layer of interface layer was observed in Fig. 11.4c, also micro-
graph revealed that solidification front starts from the interface due to high cooling
rate facilitated near the interface. At the bottom, heat dissipation rate is higher than
that of middle and top layer, the undercool region also more at the bottom. Moreover,
if the rate of nucleation is high, it impedes the growth of grains, leading to a finer
martensitic microstructure and disordered eutectic phases, which would be able to
improve mechanical performance of coated layer.
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11.3.2 Microhardness Analysis

The microhardness test was performed (on Vickers hardness tester, make: INO-
VATEST, FALCON-503) to investigate the mechanical performance of coating. The
microhardness is mainly depending upon the microstructure and phases present in
coating. The microhardness graph shows that as the percentage of ceramic increased
microhardness value increases, the variation in hardness shown in Fig. 11.5. More
interestingly, microhardness value observed better for introducing Si + B4 C in nickel
matrix rather than direct inclusion of SiC. The higher hardness is possible due to evo-
lution of fine homogenous microstructure, also Vickers hardness of B4 C is slightly
higher than that of SiC. The maximum hardness was observed 676 HV0.1 and average
hardness was 523 HV0.1 for S4 as compared to average microhardness of steel was
200 HV0.1 . In sample S3, maximum hardness observed 318 HV0.1, whereas maximum
hardness for S1 and S2 were observed 240 HV0.1 and 353 HV0.1, respectively.
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Fig. 11.5 Microhardness profile of coated sample across the crosssection from the top surface of
sample

11.4 Conclusions

The nickel-based MMC was developed on 304 steel through TIG coating method.
In coating composition, directly employed SiC and Si + B4 C in nickel-based matrix
and their results were investigated.
• The MMC coating on 304 steel was successfully developed and good interfacial
bonding was observed.
• A eutectic phases and homogenous growth of microstructure were observed for
S3 and S4.
• The higher hardness was observed for Si + B4 C than SiC for same proportion
(shown in Table 11.1) taken in nickel-based coating.
• For sample S4, Maximum microhardness and average microhardness were
observed 676 HV0.1 and 523 HV0.1, respectively, due to formation of fine
martensitic structure, whereas average hardness of the substrate was 200 HV0.1 .
• A thin and homogeneous interface layer was observed for S4, whereas thick inter-
face layer for S2 with varying grain from equiaxed at bottom to irregular large
grain at top.