Materials Today Communications 31 (2022) 103370

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Materials Today Communications

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Evaluation of microstructure, nanoindentation and corrosion behavior of

laser cladded Stellite-6 alloy on Inconel-625 substrate
N. Jeyaprakash a, b, *, Che-Hua Yang a, b, Sundara Subramanian Karuppasamy a, S.
R. Dhineshkumar c
a
Graduate Institute of Manufacturing Technology, National Taipei University of Technology, Taipei 10608, Taiwan
b
Additive Manufacturing Center for Mass Customization Production, National Taipei University of Technology, Taipei 10608, Taiwan
c
Department of Aeronautical Engineering, Mahaveer Institute of Science & Technology, Hyderabad, Telangana 500005, India

A R T I C L E I N F O A B S T R A C T

Keywords: Inconel-625 (IN-625) is one of the widely used high-temperature alloys in various areas of application. Its
Inconel-625 outstanding characteristics like thermal stability, low density, higher yield strength and oxidation resistance
Stellite-6 cladding makes it to get implemented in areas including supercritical boilers, heat exchangers, nuclear and pressurized
Nanoindentation
water reactors. In severe aggressive environments, the surface of this alloy is prone to wear and corrosion attacks
Corrosion
which leads to sudden failure of the components. This work has attempted to improve the corrosion resistance of
EIS analysis
Roughness the IN-625 alloy by depositing the Stellite-6 particles through the laser cladding technique. The cladded sample
was cross-sectioned to analyze the microstructure using the FESEM technique. The nanohardness test has been
carried out to evaluate the hardness offered by both the base and the cladded region. The corrosion (uniform
type) behavior was analyzed in an electrochemical way on both the base and the cladded samples for different
time periods. In addition, the EIS technique was used to evaluate the enhancements in the corrosion resistance of
the samples followed by the surface roughness examination. Results showed that the hypoeutectic structure was
obtained on the cladded region due to the influence of Co-rich dendritic and Cr-rich inter-dendritic eutectic
phases. The cladded region exhibited higher hardness than the base region. Moreover, the cladded sample with
17 h time interval exhibited greater resistance towards corrosion compared with the other duration samples. The
formation of oxide has been the major key factor for the enhancement of corrosion resistance. In addition to that,
17 h cladded specimen experienced minimized surface roughness with increased corrosion resistance.

1. Introduction
Inconel-625 is one of the most widely used nickel-based superalloys
compared to other superalloys. This alloy is a combination of light and
heavy refractory metals which makes it to be used in high-temperature
environments above 500 ºC. This heat-resistant alloy contributes toward
50% wt. of aero-engines [1,2]. Besides the heat resistant feature, this
alloy is preferred for its low density, thermal stability, processability,
chemical affinity, low cost, etc. [3–5]. It consists of a significant amount
of nickel, chromium, molybdenum and niobium which makes it as a
solid solution strengthened material [6,7]. In addition, IN-625 exhibits
excellent properties such as yield strength, high level of fabricability,
tensile and fatigue strength. It also provides resistance towards oxida­
tion in intrusive environments [8] and is used for manufacturing control
rods, reactor core materials, heat exchanger tubes [9,10]. Since the
IN-625 alloy is used in many aggressive environments, prolonged
exposure of this alloy in such environments causes corrosion followed by
catastrophic failure, which leads to environmental hazards and property
losses. A rise in pressure, temperature and dissolved oxygen (marine
environments) may hasten the corrosion process in IN-625 [11]. If the
operating environment consists of chlorine, sulfur and carbon, IN-625
reacts with these elements and results in the formation of chlorides
and sulfates which get deposited on the surface. These precipitated salts,
under certain conditions contribute to hot corrosion attacks thereby
increasing the rate of degradation [12].
Moreover, the fuels employed in the boilers that operate with
biomass are rich in the chlorides of potassium and sodium along with
some heavy metal chlorides. These chlorides will react directly with the

* Corresponding author at: Graduate Institute of Manufacturing Technology, National Taipei University of Technology, Taipei 10608, Taiwan
E-mail addresses: prakash84gct@gmail.com, prakash@ntut.edu.tw (N. Jeyaprakash), chyang@ntut.edu.tw (C.-H. Yang), diwahar3@gmail.com
(S.S. Karuppasamy), aerodhinesh@gmail.com (S.R. Dhineshkumar).

https://doi.org/10.1016/j.mtcomm.2022.103370
Received 28 May 2021; Received in revised form 4 January 2022; Accepted 10 March 2022
Available online 12 March 2022
2352-4928/© 2022 Elsevier Ltd. All rights reserved.
N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

excellent corrosion and wear resistance. It is a two-phase alloy repre­

senting the chromium carbide minor phase which makes it a superalloy
to resist corrosion in severe aggressive environments [25]. Ana et al.
[26] examined the microstructural features of multilayer laser cladded
Stellite-6 on 304 stainless steel substrates. Their results showed that fine
solidified microstructure with enhanced roughness was observed. Alain
et al. [27] studied the wear mechanism and the microhardness of the
laser cladded Stellite-6 on P91 and P22 bearing steel substrate. They
revealed that the development of pores and cracks is less which con­
tributes to an increase in hardness on the substrate material. Raghuvir
Singh et al. [28] analyzed the cavitation and erosion resistance of laser
cladded Stellite-6 on stainless steel. It is found that the laser cladding of
Stellite-6 has enhanced the erosion resistance.
Thus, from the above literature, it is evident that the laser cladded
Stellite-6 alloy exhibits resistance to corrosion in hostile environments.
The present study is attempted to analyze the corrosion behavior of the
laser cladded Stellite-6 on the IN-625 substrate. With the aid of FESEM,
Fig. 1. FESEM picture of as-received Stellite-6 particles. the microstructural analysis was carried out, followed by the corre­
sponding elemental analysis using the EDS technique. To examine the
IN-625 alloy and accelerate the rate of chloride active oxidation corro­ hardness, nanoindentation test was conducted on the base, interface and
sion mechanism [13]. Stress and pitting corrosion cracks were noticed cladded region. The corrosion test was performed electrochemically for
on the surface of IN-625 in supercritical water reactors [14]. Hence the various time intervals and the results were correlated with the substrate.
factors like high temperature, high pressure, presence of chlorides and The mechanism of corrosion was analyzed and the corresponding sur­
sulfates promote corrosion in IN-625 alloy. To overcome the corrosion face roughness was calculated.
effects in IN-625 alloy, several surface treatment techniques like hard­
facing, thermal spray coating, physical vapor deposition (PVD) and laser 2. Materials and methods
cladding were preferred. The major advantage of the PVD techniques is
that they can produce a finite surface on the substrate so that the 2.1. Materials
tribological properties can be analyzed effectively. But, the life span of
the PVD-treated surface will get worse due to the delamination effect Laser cladding was carried out by selecting IN-625 as the base
caused by the residual stress and adhesion over prolonged usage [15,
16]. In the case of thermal spray coating, this technique can be applied
to a wide range of substrate and spray materials with a lower environ­
mental impact. Still, it is difficult to achieve thick coating due to the
poor bonding strength [17], and the spray efficiency is low for small,
curvy and complex surfaces [18]. Another technique called the hard­
facing technique has been in vogue in which, the worn-out surfaces can
be rebuilt and it also reduces the need for replacing the parts. The major
drawback is the distortion effect due to the high-temperature arc which
is transmitted by the plasma. Laser cladding is one of the most used
surface modification techniques which consumes low energy [19] and
delivers lower heat distortion. This technique enhances the bonding
behavior between the substrate and the cladding material, and also
provides better surface uniformity. It is suitable for the defects of micron
size [20] and is an effective method to build up the surfaces [21,22].
Other advantages like high rate of deposition, reduced dilation,
ultra-thick layer and low porosity levels were obtained by using this
technique [23]. Thus, the above-mentioned advantages have paved the
way to implement the laser cladding technique in various areas such as
renovating the parts in IC engines, marine equipment, machine tools, etc
[24].
Stellite-6 is one of the most used Co-based alloys which offers Fig. 2. Schematic of the laser cladding process.

Table 1
Elemental composition of IN-625 and Stellite-6 materials.
Material Ni (%) Co (%) Cr (%) Fe (%) W (%) Si (%) C (%) Mn (%) Mo (%)

Substrate-IN-625 REM 1 23 5 – 0.05 0.10 0.50 10

Powder-Stellite-6 0.62 REM 28.21 0.82 4.39 1.27 1.22 0.14 –

Table 2
Laser parameters used for cladding process.
Material Power Feed rate Scanning speed Preheat temperature Shielding gas flow Carrier gas flow
o
Substrate – IN625 1400 W 9 g/min 600 mm/min 150 C 25 L/min 6 SD @ 100,000/Pa

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N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

Fig. 3. (a) Optical microscopy images of laser cladding cross-section with different three regions, and magnified view of (a), (c) FESEM images of laser cladded
region representing the solid solution of Co with Cr and carbides, (d) Elemental analysis graph (Inset - Image used for EDS point scan).

Fig. 4. Load to depth plot at the base, interface and cladded region obtained from the nanoindentation test.

material. Commercially available Stellite-6 alloy powder was preferred
as the cladding material. By using the FESEM, the shape and size dis­
tribution of the as-received Stellite-6 particles were analyzed as in Fig. 1.
The average size of these particles was found to be 129 ± 10 µm. Table 1
represents the chemical composition of the IN-625 and Stellite-6 alloys.
2.2. Laser cladding technique
Before laser cladding, acetone was used to clean up the substrate and
then sandblasted for achieving a surface roughness of ~ 5 µm to obtain a
good metallurgical bonding between the substrate and the cladding
material. With the aid of Yb: YAG disc laser having 1060 nm wavelength
and 6 kW power output, the Stellite-6 powder particles were evenly

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N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

Fig. 5. Tafel graph of: (a) Base and (b) cladded samples with different hours of testing.

was fixed at one end. The equilibrium potential was made to stabilize for
Table 3
30 min. By varying the scan rate from 0.05 V to 1.2 V, the cyclic po­
Corrosion test data.
larization curves were plotted. Finally, with the help of the Tafel tech­
Duration E-current (V) I-current (A/cm2) nique, the corrosion potential and the current density were measured for
Base 0 h -0.227419355 4.32174278 × 10-7 various timings as 0, 17, 24 and 33 h (h). After that, the EIS analysis with
Base 17 h -0.189219015 3.0884465 × 10-7 the frequency ranging from 106 to 10-2 Hz was carried out on the sam­
Base 24 h -0.205093379 3.69198104 × 10-7 ples. The obtained spectrum was fitted using the NOVA software and
Base 33 h -0.22385399 5.40204428 × 10-7
Clad 0 h -0.196880306 2.62975941 × 10-7
with the help of Nyquist and Bode plots, the values were analyzed.
Clad 17 h -0.160186757 1.226948 × 10-7 Moreover, the morphologies of the corroded surface were examined
Clad 24 h -0.172693831 1.59671397 × 10-7 using FESEM, and the corresponding elemental analysis was done by
Clad 33 h -0.180510753 1.81867318 × 10-7 EDS. Also, the surface roughness of the corroded samples was investi­
gated and measured.
deposited on the substrate material. Fig. 2 shows the schematic of the
3. Results and discussion
laser cladding process. The process parameters selected for laser clad­
ding were speed (mm/min), power (W), carrier gas flow rate, feed rate
3.1. Microstructure analysis
(g/min) and shielding gas flow rate. The laser cladding process was
carried out by optimizing these parameters based on the defect-free and
The cladded specimens were collected and it can be observed that the
good bonding nature of the coating. Table 2 describes the process pa­
Stellite-6 particles were evenly deposited on the Inconel-625 substrate
rameters used for the laser cladding process. After the cladding process,
(Fig. 3(a)). The thickness of the clad layer was found to be 600 µm. The
the specimens were collected and cross-sectioned with the dimensions of
cladded morphology and its elemental mapping are presented in Fig. 3
10 mm × 10 mm x 10 mm. By using the SiC sheets, the cross-sectioned
(b-d). Fig. 3(a) represents the three regions namely substrate, interface
specimens were polished and then subjected to diamond polishing. The
and cladded regions. At the solid-liquid interface, the microstructure
electrolytic chemical etching was performed on both samples with the
formation is entirely dependent on the supercooling of elements. Fig. 3
etching solution containing 15 ml of HNO3, 15 ml of distilled water,
(b) shows the magnified view of the optical microscopic image of Fig. 3
15 ml of CH3COOH and 60 ml of HCl for revealing the obtained mi­
(a) to reveal the microstructure in the cladded region. It is found that the
crostructures. JEOL 6500 F FESEM was used to analyze the micro­
Stellite-6 alloy particles are uniformly distributed during the cladding
structure of the cross-sectioned cladded specimens. Further, the
process and denote the existence of the hypoeutectic structure. Fig. 3(c)
nanoindentation test was conducted using TI 980 TriboIndenter with a
represents the hypoeutectic structure as a combination of both dendritic
force of 2000 µN.
and inter-dendritic eutectic phases. This dendritic structure is rich in
cobalt which exists in the α-Co form [29], whereas the inter-dendritic
2.3. Corrosion test eutectic phases are said to be rich in chromium carbides [30]. The
presence of carbides made the Stellite-6 alloys to have high resistance to
The corrosion test was carried out in an electrochemical way under wear and improved hardness. These carbides are generally distributed in
room temperature conditions. First, the cladded sample was cut into the grain boundaries and inter-dendritic areas [31].
cubic cross-sections and the cross-sectioned sample was kept in an EDS point scan analysis is carried out with the accelerating voltage of
electrochemical setup having the base solution made by mixing 3.5% wt. 12 kV and the energy range of 20 keV for evaluating the concentration
of NaCl in 100 ml deionized water. Since the chloride ions are consid­ of the elements in the cladded region (Fig. 3(d)). In the EDS analysis, the
ered to be more aggressive towards metals, they can create serious elemental peaks were observed for the elements like Co, Cr, Si, W, C and
corrosion attacks by destroying the passivation layer in materials. The O. This figure reveals that the Co content is higher with fewer amounts
setup consisted of three electrodes in a flat cell. The sample itself acted of C content. From this, it is confirmed that it is a solid solution of the Co
as one electrode and the other two electrodes were auxiliary electrodes element. The highest peak is obtained for Co because the SEM image
(AgCl and Pt electrodes). The cladded sample was kept rigidly in a proved that it contains the Co-rich matrix. There is an increase in the
Teflon disc to measure the corrosion resistance so that the cladded area fraction of the carbides and are generally distributed in the grain
surface is exposed to the electrolytic solution. boundaries. During the cladding process, the high-power laser beam will
The procedure for the corrosion test is described as follows: First, the cause the decomposition of metallic bonds in the Stellite-6 alloy and as a
prepared solution was filled in the flat cell and the sample (electrode)

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N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

Fig. 6. Corroded surface morphologies and the elemental mapping of IN-625 substrate at: (a-b) 0 h, (c-d) 17 h, (e-f) 24 h, (g-h) 33 h.

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N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

Fig. 7. Corroded surface morphologies and the elemental mapping of cladded samples at: (a-b) 0 h, (c-d) 17 h, (e-f) 24 h, (g-h) 33 h.

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N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

Table 4
The elemental compositions at the surfaces of different specimens after corrosion test.
Element CK OK Si K Cr K Fe K Ni K Nb L Mo L Mn K Co K WM Totals

Base 0 h Weight% 17.37 15.29 0.15 16.29 1.62 39.73 2.72 6.82 – – – 100.00
Atomic% 41.01 27.10 0.15 8.88 0.82 19.18 0.83 2.02 – – –
Base 17 h Weight % 17.75 20.90 0.05 12.89 1.60 33.46 4.22 9.14 – – – 100.00
Atomic % 39.16 34.63 0.05 6.57 0.76 15.10 1.20 2.53 – – –
Base 24 h Weight % 21.01 19.53 0.29 14.34 1.30 33.03 4.13 6.38 – – – 100.00
Atomic % 44.26 30.88 0.26 6.98 0.59 14.23 1.12 1.68 – – –
Base 33 h Weight % 19.81 13.94 0.19 19.20 1.67 38.29 3.28 3.63 – – – 100.00
Atomic % 45.17 23.86 0.19 10.11 0.82 17.86 0.97 1.03 – – –
Clad 0 h Weight% 13.57 3.42 1.39 26.85 0.22 5.68 – – 1.78 42.09 5.00 100.00
Atomic% 40.59 7.67 1.78 18.55 0.14 3.47 – – 1.17 25.65 0.98
Clad 17 h Weight% 17.22 7.40 1.22 24.61 0.15 1.75 – – 1.34 41.90 4.40 100.00
Atomic% 44.73 14.43 1.36 14.77 0.09 0.93 – – 0.76 22.19 0.75
Clad 24 h Weight% 13.01 3.71 1.28 31.05 0.31 1.84 – – 1.59 42.18 5.03 100.00
Atomic% 39.15 8.37 1.65 21.59 0.20 1.14 – – 1.05 25.87 0.99
Clad 33 h Weight% 12.02 3.52 1.16 30.08 0.53 2.16 – – 1.71 43.04 5.78 100.00
Atomic% 37.35 8.21 1.55 21.58 0.35 1.37 – – 1.16 27.25 1.17

result, other elements can’t withstand that temperature thereby forming the IN-625 alloy was exposed to high temperatures, Cr and Mo were
carbides with a subsequent increase in the C percentage [32]. Since the oxidized to form dichromate and molybdate compounds. The formed
inter-dendritic eutectic structure along the grain boundaries contains dichromate was dispersible resulting in the dissolution of the oxide layer
high Cr and C contents, it is suggested to be rich in Cr carbides [33]. which promotes corrosion [37]. Eqs. (1–7) represent the corrosion
When a small amount of molten metal is submerged into a cooler sub­ mechanism [38].
strate, it results in rapid solidification which forms a fine microstructure
with high hardness [34]. Due to this rapid solidification, laser cladded Ni → Ni2+ +2e- (1)
Stellite-6 forms a fine dendritic microstructure. In addition to that, the Ni2+ + 2 H2O ↔ Ni(OH)2 + 2 H+ (2)
produced microstructure reveals that the carbide formed during the
laser cladding is distributed along the grain boundaries and forms a Ni(OH)2(aq) ↔ NiO(s) + H2O (3)
continuous network of Co-rich grains. Thus, the carbides of Cr act as a
Cr → Cr 3+
+ 3e −
(4)
barrier by promoting the Cl- ions attraction, which enhances the passive
film properties followed by improving the corrosion resistance of the Cr 3+
+ 3 H2O ↔ Cr(OH)3 + 3 H +
(5)
cladded specimen.
Cr(OH)3 + Cr → Cr2O3 + 3 H+ + 3e− (6)

3.2. Nanohardness examination 2Cr3+ + 7 H2O → Cr2O72− + 14 H+ + 6e− (7)

The corrosion results of base and cladded samples were plotted as the
Hardness is an important property in ensuring the safety of materials.
Tafel graph as shown in Fig. 5(a-b), respectively. The linear regions in
It is the ability to resist wear and it is a key factor to determine the
the Tafel graph play a vital role in evaluating the corrosion rate. The x
strength and ductility [35]. Since the cladding process is a surface
and y-axes of this graph represent the current density and potential
treatment technique, it is a need to ensure the hardness of the cladded
which serve as a factor for calculating the corrosion resistance and
sample. For this purpose, the nanoindentation technique has been per­
stability [39]. The polarization curves represent the passivation ten­
formed and the hardness changes were studied. Fig. 4 represents the
dency, which indicates that the current is unchanged while increasing
load to depth plot at the base, interface and cladded region which was
the potential. It is evident that no active to passive transitions are seen,
obtained from the nanoindentation test. From this plot, it is evident that
indicating that the oxide film was formed continuously. The corrosion
the higher indentation depth experiences a lower hardness and
parameters calculated from the potentiodynamic polarization curves for
vice-versa. Moreover, for 2000 µN load, the depth is high at the substrate
0, 17, 24, 33 h are summarized in Table 3. The current density is high
(~83 nm) and low indentation depth has been obtained at the cladded
(4.322 ×10-7 A/cm2) for the base region and decreases to 2.630 × 10-7
region. Correspondingly, the nanohardness values have been calculated
A/cm2 for the cladded region at 0 h. This denotes that, after the cladding
at the various three regions. The value at the interface tends to be high
process, there is a notable change in the corrosion resistance of the
(7.74 GPa) compared with the values of the base (5.07 GPa) and the
cladded sample. For different time intervals, the Tafel graph for both
cladded (7.69 GPa) region. The existence of the intermetallic phases like
base and cladded specimens was plotted as in Fig. 5. It is seen that there
Co, Cr and carbide phase in the interface region accounts for a higher
is much difference between the base and laser cladded specimens, which
hardness value than the cladded region. Besides, the low dilution of
means that their behavior to corrosion resistance is similar during the
Stellite powder with the base material is also another reason for the
initial stage of oxidation; but, laser cladded Stellite-6 exhibits better
slight increase in the hardness value at the interface when exposed to
resistance to electron transferring or corrosion resistance due to the
high laser density [36]. Thus, the presence of Cr carbides in the cladded
lower current density and highest polarization resistance values. These
region enhances the hardness compared with the substrate material.
results reveal that the laser cladded specimens have high electro­
chemical stability compared with the Inconel-625 substrate at all in­
3.3. Corrosion analysis tervals. This is because of their passive film and good corrosion
resistance. Also, the cladded sample exhibits a large passive region than
Corrosion analysis was carried out in an electrochemical environ­ the IN-625 alloy. This is because of the Cr2O3 film which was formed on
ment at ambient conditions. This analysis was aimed at measuring the the cladded sample is more substantial and has better resistance to
corrosion resistance of the cladded sample at different time intervals. corrosion in the NaCl solution [40].
The electrochemical setup consisted of a base solution containing 3.5% Fig. 6(a-h) represents the morphologies and the elemental mapping
wt. of NaCl in deionized water where both the base and cladded samples of IN-625 substrate at 0, 17, 24, 33 h. On comparing these figures, the
underwent corrosion analysis to examine the corrosion resistance. When

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N. Jeyaprakash et al.
Fig. 8. EDS point scan images of base (a) 0 h, (b) 17 h, (c) 24 h, (d) 33 h and clad (e) 0 h, (f) 17 h, (g) 24 h, (h) 33 h samples.
17 h corroded base material is found to have a high amount of oxide
content (20.90%) with irregular surface morphology. The oxide content
of the base material is decreased to 19.53%, 15.29%, and 13.94% for 24,
0, 33 h respectively. Also, the current density of the IN-625 specimen for
17 h is lower, which indicates that this material provides better resis­
tance towards corrosion among the base samples. Fig. 7(a-h) describes
the FESEM morphology and the EDS spectra of the cladded sample at
different time intervals. The 17 h treated cladded specimen is reported
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Materials Today Communications 31 (2022) 103370
to have maximum oxide content in comparison with other intervals and
it also represents the formation of fine crystalline structure of oxide
which results in excellent corrosion resistance compared with other
intervals. This crystalline structure of oxide is evidence for enhancing
the corrosion resistance at the cladded region. As time increased, the
formed structure began to become fragile and started to depart from the
surface and also left patches in some places on the surface. After the
corrosion test, the EDS point scan analysis has been performed to
N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

Fig. 9. Schematic of passivation mechanism: (a) Cladded stellite-6 surface consisting of Co2+, Cr3+ ions, (b) Co, Cr ions present in the stellite reacts with oxygen, (c)
Formation of passive (oxide) layer containing Cr2O3 and CoO that protects from corrosion, (d) Breakage of fragile oxide patches from the surface.

Fig. 10. Nyquist and Bode plots of: (a-b) Base, and (c-d) Cladded specimen.

evaluate the elemental compositions of the passive film formed on both
samples. Based on this point scan analysis, the obtained elemental
compositions of elements like C, O, Cr, Fe, Si, Co, Ni, Nb were tabulated
in Table 4 for both samples. It can be inferred that the film formed on the
cladded samples has high Co content followed by Cr, C and O content
since the cladded samples have the Co-rich matrix with carbides at their
grain boundaries. Hence, these elemental compositions have paved the
way to form a stable passive film on the cladded surface compared to the
base material. The EDS point scan images used for EDS analysis with the
voltage and energy range of 5 kV and 10 keV for both the base and
cladded samples were represented in Fig. 8. Moreover, the 17 h treated
cladded sample is found to have a lower current density (1.227 ×10-7 A/
cm2) compared with its respective base sample (3.089 ×10-7 A/cm2).
This result also proves that the cladded sample exhibits high resistance
to corrosion compared with the IN-625 substrate. The passivation
mechanism behind the chromium oxide layer formation is presented in

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N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

Table 5 and cladded samples at different intervals are given in Table 5. The
Parameter values of different elements obtained from EIS analysis. higher value of Rp results in greater resistance to corrosion [46]. For
Duration Element Rs Rp CPE 17 h, the value of Rp for the cladded sample is 55743 which is almost
Parameter R R Y0 N twice the base sample value (26410). On comparing the Rp values of
Base 0 h (χ2 = Value 10.808 9809.3 4.5372E- 0.81942 both the samples at the other intervals, a higher Rp value is observed in
0.42516) 05 the cladded sample than the base, which proves that the laser cladded
Estimated 4.937 8.168 17.995 6.642 Stellite-6 has excellent resistance towards corrosion and particularly for
Error (%) 17 h, the cladded sample experiences high corrosion resistance.
Base 17 h(χ2 Value 11.276 24233 5.9136E- 0.83543
= 0.41601) 05
Estimated 1.911 2.792 2.291 0.526
Error (%) 3.5. Corroded surface roughness analysis
2
Base 24 h(χ Value 8.4997 5187.3 4.2504E- 0.85055
= 0.70981) 05 The corrosion resistance of any metal is greatly influenced by the
Estimated 2.702 2.454 4.536 0.861
surface roughness [47,48]. This surface roughness analysis is used to
Error (%)
Base 33 h(χ2 Value 6.3238 50431 1.6735E- 0.71553 study the corrosion effect on the surface by measuring the value of the
= 0.18074) 05 roughness. The average roughness values (Ra) of the sample before and
Estimated 3.678 1.693 1.638 0.318 after cladding were obtained to evaluate the deposition of cladded
Error (%) particles [49]. Fig. 11(a-d) represents the 3D surface plot and their
2
Clad 0 h(χ = Value 5.7347 26410 1.6532E- 0.6978
0.29092) 05
corresponding Scanning Probe Microscopy (SPM) images generated on
Estimated 5.971 1.830 2.421 0.460 the base and cladded region before the corrosion test. The roughness
Error (%) value at the cladded region (4.76 nm) is higher than the roughness value
Clad 17 h(χ2 Value 7.2336 55743 2.0516E- 0.70244 at the IN-625 substrate region (2.00 nm). This increased roughness
= 0.23867) 05
proves the distribution of Stellite-6 particles on the substrate. Corrosion
Estimated 3.907 2.173 1.790 0.367
Error (%) resistance is inversely proportional to the roughness value. Table 6
Clad 24 h(χ2 Value 7.8252 52863 1.593E- 0.71467 represents the roughness values (Ra) of both base and cladded samples
=0.32007) 05 at different time intervals. The corresponding 3D plot and its 2D graph
Estimated 4.447 2.252 2.202 0.435 for the base samples at 0, 17, 24 and 33 h are shown in Fig. 12(a-h). On
Error (%)
Clad 33 h(χ 2
Value 9.9171 18652 4.7744E- 0.88677
comparing these roughness values obtained from the plots, the value of
=0.27435) 05 the 0 h treated base sample has the highest value (0.6013 ± 0.1895 µm)
Estimated 1.493 1.940 2.008 0.427 and this sample experiences worse resistance towards corrosion. Among
Error (%) the different time intervals, the sample treated for 17 h shows the least
roughness value (0.337 ± 0.132 µm) thereby increasing the corrosion
resistance.
Fig. 9.
Fig. 13(a-h) represents the corroded 3D surface and its correspond­
ing 2D graph for the cladded specimens at different time intervals. From
3.4. Electrochemical impedance spectroscopy (EIS) analysis Table 6, by correlating the roughness values of both the base and clad­
ded samples, the cladded samples are found to have a reduced roughness
The EIS technique is used to evaluate the electron transfer mecha­ value than the base samples at various time intervals. This is due to the
nism and the corrosion resistance of the samples. Fig. 10(a-d) represents formation of oxide layer on the surface. This proves that the laser
the Nyquist and Bode plots of the base and cladded region. It is found cladded Stellite-6 surface exhibits excellent corrosion resistance than the
that the Nyquist plot of the base and cladded regions consists of single base sample. Besides, the 17 h treated cladded sample has the least
capacitive loop. It also indicates that, within the measured frequency roughness value with high corrosion resistance. The corrosion resistance
range, the electrochemical reaction dominates the reaction that takes of the cladded sample for 24 and 33 h is greatly influenced because, after
place at the electrode [41]. Moreover, the semicircular arc in these plots 17 h, the formed oxide layer becomes delicate and brittle, and breaks.
represents the mechanism of charge transfer on an uneven surface [42]. Due to this, patches are formed, decreasing the corrosion resistance at 24
Generally, the larger semicircular arc radius will have higher corrosion and 33 h. Thus, the surface roughness greatly influences the corrosion
resistance [43]. From Fig. 10(a), the loops of the 17 h treated base resistance property of both the samples at different time intervals.
sample has a larger radius and thus it is evident that this sample has
higher corrosion resistance compared with the 0, 24, 33 h treated 4. Conclusions
IN-625 sample. The radii of the capacitive loops obtained from the
cladded sample (Fig. 10(c)) are higher than that of the base for all the With the aid of the laser cladding technique, the Stellite-6 alloy
intervals. It also indicates that Stellite-6 exhibits good corrosion resis­ powder was evenly deposited on the IN-625 substrate. The cladded
tance at various time intervals. Moreover, the radius of the 17 h treated sample was cross-sectioned and then subjected to morphological anal­
cladded sample is higher than the base sample at the same time interval. ysis with elemental mapping to reveal the microstructure. The corrosion
This proves that the 17 h treated cladded sample exhibits higher resis­ resistance of the cladded sample was analyzed electrochemically, and
tance towards corrosion. Fig. 10(b and d) represents the Bode plot of the nanoindentation, EIS analysis, surface roughness results are
both samples at 0, 17, 24, 33 h. It can be observed that the corrosion presented.
resistance is directly proportional to the area covered below the curve
[44]. From this figure, it is evident that the 17 h treated samples in both • From the morphological analysis, the cladding is said to be uniform
base and cladded region have a larger area that experiences an increased with even particle distribution in the cladded region. The cladded
corrosion resistance. Thus, in both the plots, the 17 h treated sample region consists of a hypoeutectic structure. This is due to the influ­
exhibits higher resistance against corrosion. ence of Co-rich dendritic and Cr-rich inter-dendritic eutectic phases
Fig. 10(b) shows the schematic representation of the equivalent along with the carbides at their grain boundaries.
circuit for fitting the EIS data where Rp is the polarization resistance, Rs • The hardness study reveals that lower indentation depth experiences
is the solution resistance and CPE is the constant phase element [45]. a higher hardness. The cladded region exhibits a higher hardness
The results of spectra fitting using the equilibrium circuit for both base value than the base region. Hence, the higher hardness value

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N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

Fig. 11. 3D surface plot and their corresponding Scanning Probe Microscopy (SPM) images before the corrosion test: (a-b) Base, and (c-d) cladded samples.

of the 17 h treated cladded sample has a higher value and also pro­
Table 6 vides greater resistance against corrosion.
Roughness values of base and cladded surface after corrosion • The surface roughness analysis also confirms that the cladded sam­
test. ples have a lower roughness value which enhances the corrosion
Specimens Roughness value - Ra (µm) resistance compared with the base samples at different time in­
Base 0 h 0.6013 ± 0.1895
tervals. Also, the roughness value obtained for the 17 h treated
Base 17 h 0.337 ± 0.132 sample is very minimum and delivers a greater corrosion resistance.
Base 24 h 0.4182 ± 0.09058
Base 33 h 0.4638 ± 0.1758 In summary, Stellite-6 particles can be utilized to enhance the
Clad 0 h 0.6507 ± 0.1818
corrosion resistance of engineering components in aggressive
Clad 17 h 0.1776 ± 0.0351
Clad 24 h 0.2955 ± 0.1080 environments.
Clad 33 h 0.4752 ± 0.09095
CREdit authorship contribution statement
indicates a greater resistance to wear, thus extending the service life
N. Jeyaprakash: Conceptualization, Methodology, Data curation,
of the components.
Writing – original draft preparation., Che-Hua Yang: Visualization,
• The corrosion analysis was carried out electrochemically for various
Investigation, Funding, Writing – reviewing and editing. Sundara
timings as 0, 17, 24 and 33 h. From the Tafel plot, it is found that the
Subramanian Karuppasamy: Visualization, Software, Validation. S.R.
17 h cladded sample consists of a large passive region than the
Dhineshkumar: Software, Validation.
substrate. This is due to the formation of Cr2O3 film which made it to
exhibit better corrosion resistance.
• The Nyquist and Bode plots obtained from the EIS technique show
Declaration of Competing Interest
that the higher loop area experiences greater corrosion resistance.
On comparing both the plots of base and cladded samples, the
The authors declare that they have no known competing financial
cladded sample is found to exhibit higher resistance towards corro­
interests or personal relationships that could have appeared to influence
sion. Moreover, by fitting the EIS spectra, the polarization resistance
the work reported in this paper.

11
N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

Fig. 12. Corroded 3D surface and its corresponding 2D graph for the base specimens at: (a-b) 0 h, (c-d) 17 h, (e-f) 24 h, (g-h) 33 h.

12
N. Jeyaprakash et al. Materials Today Communications 31 (2022) 103370

Fig. 13. Corroded 3D surface and its corresponding 2D graph for the cladded specimens at: (a-b) 0 h, (c-d) 17 h, (e-f) 24 h, (g-h) 33 h.

Data availability statement Acknowledgments

The experimental datasets obtained from this research work and then We are grateful for the support from the Ministry of Science and
the analyzed results during the current study are available from the Technology, Taiwan and the Additive Manufacturing Center for Mass
corresponding author on reasonable request. Customization Production, National Taipei University of Technology,

13
N. Jeyaprakash et al.
Taiwan for providing the financial support.
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