Surface & Coatings Technology 357 (2019) 543–558

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Surface & Coatings Technology

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Comparative study on the friction-wear property of As-plated, Nd-YAG laser T

treated, and heat treated electroless Nickel-Phosphorus/Crab shell particle
composite coatings on mild steel
⁎
S. Arulvela, , A. Elayaperumala, M.S. Jagatheeshwarana, A. Satheesh kumarb
a
Department of Mechanical Engineering, Anna University, Chennai 600025, Tamil Nadu, India
b
Meera Laser Solution, Ambattur, Chennai, Tamilnadu, India

A R T I C LE I N FO A B S T R A C T

Keywords: Nickel-Phosphorus/Crab shell particle (NiP/CSP) composite coatings were prepared with different weight dis-
Mild steel persions of CSP (0.5 g/l, 1.0 g/l, 1.5 g/l, 2.0 g/l, 2.5 g/l and 3.0 g/l) on mild steel using electroless coating
Electroless coating process. Fabricated coatings were post treated with heat treatment and Nd:YAG laser treatment process and
Nickel-phosphorus followed by a comparative study on surface morphology, surface hardness, phase structure, and friction-wear
Crab shell
property with as-plated NiP and NiP/CSP composite coatings. The result showed the relative changes in the
ND:YAG laser
surface morphology of NiP/CSP composite coatings after Nd:YAG laser treatment. Dendrite structure was ob-
served for laser treated coatings and its formation was affected by the incorporation of CSP in the NiP matrix.
FeNi2P phase was formed for laser treated coatings in addition to the Ni3P and Ni12P5 phases. Higher surface
hardness of 966 Hv0.05 and 941 Hv0.05 was achieved for laser treated NiP and NiP/CSP composite coatings
compared to the heat treatment process and as-plated condition. On comparison with various weight dispersions,
higher surface hardness of 941 Hv0.05 was obtained for NiP/CSP (2.5 g/l) composite coatings as a result of the
high diffusion of Fe element from substrate to the surface. Low friction coefficient was seen for the heat
treatment process followed by the as-plated and laser treatment process. The formation of FeNi2P phase caused
an increase in the friction coefficient for laser treated NiP and NiP/CSP composite coatings. However, there was
an improvement in the wear resistance of laser treated coatings compared to the as-plated and heat treated
coatings.

1. Introduction engineering of steel components. Electroless coating technique is an

Friction and wear are the two surface degradation phenomena that
occur during the interaction of two surfaces. Hence, modification of the
materials surface could play a vital role on controlling friction and wear
of any material. The surface of mild steel had been the subject of in-
terest for researchers due to its poor friction wear property and so,
modification of the surface of mild steel and determination of its fric-
tion-wear property are very important. Mild steel is a low carbon steel
which was the accepted steel material in several industrial applications
due to its better malleability, weld-ability and low cost. A severe wear
transition mode places a limit on the use of the mild steel in friction
wear applications [1]. To overcome this, it is necessary to modify the
surface of mild steel relevant to the tribology application. Despite the
availability of several coating techniques, the electroless deposition
process has been the promising technique which finds use in surface
autocatalytic chemical reduction process used in various industrial
applications owing to its good lubricity hardness wear and corrosion
resistance [2]. Though as plated electroless NiP coating exhibits a better
wear and corrosion properties, it is improved further by the secondary
process and second phase particle incorporation in the electroless nickel
matrix. The choice of second phase particles depends upon the appli-
cations, where coating is desired. Reinforcement of soft or solid lu-
bricants like WS2, PTFE, MoS2, and graphene usually has a low friction
coefficient with reduced hardness and, hard particle reinforcement like
WC, SiC, and Al2O3 could increases the wear resistance with increased
hardness [3–5]. So, the second phase reinforcement particle is opted for
electroless composite coating depending upon the operating environ-
ment. Recently, a combination of solid lubricants and ceramics particles
is finding preference for use with NiP matrix for providing low friction
coefficient, high wear resistance, and better hardness [6]. Hence, the

⁎
Corresponding author.
E-mail address: gs.arulvel.research@gmail.com (A. S.).

https://doi.org/10.1016/j.surfcoat.2018.10.051
Received 29 August 2018; Received in revised form 12 October 2018; Accepted 18 October 2018
Available online 20 October 2018
0257-8972/ © 2018 Elsevier B.V. All rights reserved.
A. S. et al.
focus of several works which is still on reinforcing hybrid particles with
NiP matrix for improvement of friction wear property [7–10] and also
been a success in the past. Hybrid combinations of amorphous phase
and crystalline phase were observed in crab shell particles as reported
in author's previous article [11]. The presence of an amorphous phase
(organic polymer and protein) could enhance the interface strength of
CSP with NiP matrix during the deposition process. Presence of an
amine group in CSP also have an advantage of increasing the rate of
deposition arising as a result of the chelating ability, which typically
not exists for ceramic particle reinforced NiP coating. The dissolving
phenomenon of CSP also has the advantage of improving the solid so-
lution strengthening of NiP matrix in terms of lubrication for friction
wear application. Hence, this work is focused on the utilization of CSP
at various weight percentages as reinforcement with NiP matrix.
In spite of reinforcing the second phase particles with NiP matrix,
secondary processes are regularly followed for the enhancement of
surface properties. The low temperatures of electroless NiP coating
process do not have much influence on the strengthening of the inter-
face of matrix and particles. Hence, several authors have reported the
effect of the secondary process on improving the chemical interaction
between the particle matrix and substrate [12]. Generally in the heat
treatment process, both coating and the substrate are heated to a
temperature of 400 °C–600 °C [13] and allowed to cool at a constant
rate. This leads to the crystallization process and inter-diffusion reac-
tion between NiP coating and the substrate. Crystallization process is
initiated with the formation of stable Ni crystallites and followed by the
formation of Meta stable precipitates like Ni3P, NiP, Ni5P, and Ni12P5
[14]. The formation of stable and Meta stable phases during the sec-
ondary heat treatment could enhance the properties such as hardness,
corrosion resistance, and wear. In the case of the laser treatment, the
surface undergoes rapid melting and is followed by rapid self-
quenching. This produces a structure with ultra-fine grains on the
coating surface and increases the bonding strength between the coating
and the substrate. Therefore, the laser treatment process had been the
widely accepted secondary treatment process for improving hardness,
wear, and corrosion resistance. A study of the laser treatment on cor-
rosion and wear properties has been reported by various authors and
concluded that the laser treated coatings is superior to heat treated
coatings [15]. In addition, laser treatment leads to the formation of
both the amorphous phase and the crystalline phase in the structure of
NiP coating. This phase combination certainly improves the friction-
wear property of NiP coating. However, laser treatment induces a crack
formation on the surface, which is considered as a drawback of using
the laser treatment process for friction-wear and corrosion application.
This crack certainly plays a significant role in the introduction of the
fracture phenomenon during the sliding of two surfaces. Hence, it is
very important to discuss the comparative study of using various sec-
ondary processes on the fabricated electroless composite coatings in
terms of friction-wear behavior.
In author's previous article, friction-wear property of heat treated
electroless NiP/CSP composite coating was determined at various load
conditions [16]. The conclusion reached was that crab shell particles
can be effectively used for controlling adhesive wear under a high load
condition. However, a detailed study on the effect of various weight
percentages of CSP in NiP matrix on microstructure, coating thickness,
hardness, and friction-wear property has not reported in respect of as-
plated, Nd:YAG pulsed laser treatment, and heat treatment process.
Hence, this work presents the study on the friction-wear property of
NiP/CSP composite coating with various dispersions of CSP fabricated
Table 1
Chemical composition of mild steel in weight percentage.
Element (wt%) Carbon Copper Iron
Mild steel 0.25–0.29% 0.20% 98%
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Surface & Coatings Technology 357 (2019) 543–558
using electroless coating process. The friction-wear property of as-
plated NiP/CSP composite coating is compared with the heat treatment
process and Nd:YAG pulsed laser treatment process to suggest a better
secondary post treatment process for NiP and NiP/CSP composite
coatings.
2. Materials and method
2.1. Matrix and reinforcement particles
Crab shell particle (Carpilioidea species) was used as the re-
inforcement particle. Extraction and processing of crab shell particles
from crab shell have been described in the author's previous article
[11]. Nickel - Phosphorus was used as a matrix for reinforcing crab shell
particles through electroless coating process involving several chemical
reactions in an aqueous solution of electroless NiP bath.
2.2. Particle characterizations
The particle size, elemental composition, and morphology of CSP
were characterized using a scanning electron microscope (SEM) with
energy dispersive spectrum mapping (EDS) (Hitachi S-3400N).
Diffraction pattern and EDX analysis of CSP was obtained using high
Resolution Transmission Electron Microscope (HR-TEM) (Tecnai, G2 20
Twin) to discuss the different phases of the constituents of CSP.
2.3. Fabrication of electroless NiP and NiP/CSP composite coatings
Mild steel with an average surface roughness of 0.50 μm with ele-
mental composition shown in Table 1 was used as a substrate material
for the deposition of NiP and NiP/CSP composite coatings.
The chemical reactions and the formation mechanism of NiP and
NiP/CSP composite coating on mild steel have been referred to in the
author's previous article [16]. A typical bath composition and para-
meters used for the fabrication of electroless NiP and NiP/CSP com-
posite coatings are shown in Table 2.
Prior to the coating process, specimen was pre-treated at room
temperature with the procedure shown in the flow chart (Fig. 1). Fol-
lowing the pretreatment process, the specimen was immersed in an
alkaline electroless bath with pH in the range of 7 to 7.5, which was
monitored using digital pH meter. Ph was maintained at the same level
throughout the coating process using glacial acetic acid.
2.4. Heat treatment and Nd:YAG laser treatment process
The fabricated coating samples were heat treated to 400 °C using a
conventional furnace at a heating rate of 0.5 °C and allowed to cool
[16]. Nd:YAG laser was used as the source for the laser treatment
process with the parameters shown in Table 3. All samples were treated
with a constant laser power of 150 W at a constant scanning speed of
30 mm s−1 of the laser beam. Argon gas was used for reducing the
surface oxidation that resulted during the laser processing.
2.5. Hardness analyses
Surface hardness of fabricated NiP and NIP/CSP composite coatings
(as-plated, heat treated, and Laser treated) was measured on the surface
of the coatings using a micro Vickers hardness tester (ECONOMET VH
1D) under a load of 50 g at a dwell time of 15 s.
Manganese Phosphorous Silicon Sulfur
1.03% 0.040% 0.280% 0.50%
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Table 2 with various grades and finally polished with a velvet cloth under the
Bath parameters of electroless bath. suspension of alumina powder.
Component Concentration
2.7. Phase structure analysis
Nickel sulfate 20 g/l
Sodium hypophosphite 23 g/l
The phase structure of coatings was determined using X- ray dif-
Sodium citrate 13 g/l
Lead acetate 0.001 g/l
fractometer (XRD) using CuKα radiation with wavelength of 1.54 Å in a
Acetic acid 3–5 ml diffraction angle of 2theta from 10° to 70° at a step size of 0.02.
Crab shell particle (CSP) 0.5 g/l, 1.0 g/l, 1.5 g/l, 2.0 g/l, 2.5 g/l and 3.0 g/l
Agitation speed 350 rpm 2.8. Friction-wear characterization
Temperature 80 °C–90 °C

Friction and wear behavior were tested against hardened EN-31

steel using a pin on disc apparatus (DUCOM) with a constant sliding
velocity of 0.7 m s−1 at load of 14.71 N in dry sliding condition at room
temperature. The preliminary step prior to friction-wear test and wear
rate calculation has been referred to in the author's previous article
[16]. SEM images of the wear track were used for characterizing the
wear mechanism occurred during the dry sliding test.

3. Result and discussion

3.1. Particle characterization (SEM and TEM analysis)

Surface morphology of CSP (Carpilioidea species) obtained using

SEM is shown in Fig. 2. The particles exhibited a non-uniform surface
morphology with varying particle sizes (Fig. 2a).
The average particle size of CSP was between 5 and 18 μm. EDS
mapping confirmed the existence of C, Ca, Mg, Si, O and P in CSP,
which implied a hybrid combination of inorganic and organic elements.
The spectrum depicted Ca and O as major constituents of CSP and
elements like Mg, Si and P were presented as impurities. The presence
of carbon indicated the presence of organic constituents such as chitin
polymer and protein matrix, which is combined with the inorganic
elements.
Fig. 3 shows the morphology, EDX, and diffraction pattern of CSP
obtained using TEM. The presences of both inorganic and organic
constituents were seen in the morphology of CSP along with non-uni-
form particle size (Fig. 3a). A transparent white region indicated the
presence of organic elements while the dark region showed the pre-
sence of inorganic elements. Both these regions were found randomly
distributed in the CSP, indicating the distribution of amorphous and
crystalline phases. The obtained diffraction pattern of CSP is shown in
Fig. 3b. The diffraction pattern of CSP exhibited a random distribution
of various crystal orientations. This was due to the presence of elements
Ca, Mg, Si and organic constituents. The presence of these elements was
also confirmed through EDX analysis as shown in Fig. 3c. The random
Fig. 1. Flowchart of pretreatment procedure before coating process. orientation of bright spots within the diffraction ring evidences that
crab shell particles was a combination of polycrystalline and amor-
Table 3 phous structure.
LASER hardening parameter.
3.2. Surface morphology study
Parameters Type/units

Laser type Nd:YAG Fig. 4 depicts the surface morphology of NiP, and NiP/CSP (as-
Power 150 W plated, heat treated, and laser treated) composite coatings. As-plated
Frequency 12 Hz
NiP coating exhibited a typical cauliflower nodular structure (Fig. 4a),
Pulse duration 6 μS
Wave length 1064 nm
which is consistent with many articles [17].
Laser spot dia 4 mm No morphological change was observed for heat treated NiP coat-
Scanning speed 30 mm s−1 ings apart from the refined grain boundaries (Fig. 4b). The strong re-
fined grain boundaries were presumably related to the transformation
of the amorphous phase to the crystalline phase during the heat treat-
2.6. Microstructure ment process. To discuss the grain boundary refinement, grain
boundary width of as-plated and heat treated NiP coating measured
Surface morphology and cross section images of NiP and NIP/CSP using SEM is shown in the inlay image of Fig. 4a and b. The grain
composite coatings were obtained using a scanning electron microscope boundary width of as-plated NiP coating was about 1 μm, which is high
(SEM) with EDS mapping (Hitachi S-3400N). A cross section of the test compared to that of 0.1 μm of heat treated NiP coating. The refinement
specimen was mounted and mechanically polished using SiC papers of the grain boundary width was presumably related to the grain

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Fig. 2. a) SEM image of CSP and b) EDS mapping of CSP.

boundary diffusion phenomenon caused during the heat treatment diffusion of atoms across the grain boundary and restrict the growth of
process. During the transformation of amorphous phase to the crystal- the grain boundary width for heat treated NiP coating. Hence, this
line phase, Meta stable phases are induced in the coatings and these phenomenon caused refined grain boundaries for the heat treated NiP
phases act as impurities. These impurities certainly enhance the coatings. The role of impurities on grain boundary diffusion has also

Fig. 3. a) TEM image of CSP, b) Diffraction pattern of CSP and c) EDX pattern of CSP.

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Fig. 4. SEM images of NiP coating in a) As-plated, b) Heat treated, and c) Laser treated conditions.

been discussed in a recent article [18].
A typical sharp parabolic needle like structure was formed for Laser
treated NiP coating. This was found to be uniformly distributed
throughout its morphology (Fig. 4c). This structure, termed as a den-
drite structure is the result of the rapid solidification and cooling of the
coatings during the laser treatment process. The formation of dendrite
structure also indicates a faster growth of nickel crystal towards the
crystallographic direction. The central core of the dendrite structure
indicates the Ni phases (Ni3P, Ni12P5), which had a better interface with
the primary α-Ni. These phases are the primary reason for limiting the
growth of the dendrites in the morphology structure. This structure
almost matched with the morphology of NiCrBSi hard facings [19],
whereas, laser treated NiP coating is not reported elsewhere. To
confirm the element present in the surface of Laser treated NiP coating,
EDS analysis is shown in Fig. 5. EDS mapping clearly shown the pre-
sence of Ni, P, and Fe elements for Laser treated NiP coating. The
presence of Fe elements are due to the diffusion phenomenon caused
during the laser treatment process.
The cross section image of as-plated, heat treated and laser treated
NiP coating is shown in the Fig. 6. No cracks, voids and pores were
detected across the cross section of as-plated NiP coating and heat
treated NiP coating (Fig. 6a and b), whereas, pores were seen in the
cross section of the laser treated NiP coating (Fig. 6c). There was an
increase in the coating thickness of 54 μm for laser treated NiP coating
compared to the 18 μm of as-plated NiP coating and 20 μm of the heat
treated NiP coating. The increase in the coating thickness was related to

Fig. 5. EDS mapping image of laser treated NiP coating.

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Fig. 6. Cross section SEM images of NiP coating in a) As-plated, b) Heat treated, and c) Laser treated conditions.

the faster growth of Ni as discussed earlier for the dendrite structure. Fig. 7 shows the EDS mapping across the cross section of the laser
The growth of NiP matrix arising as a result of the rapid solidification treated NiP coating. Elemental mapping of laser treated NiP coating
caused the formation of pores. evidenced the presence of Ni, P, and Fe elements, which are the

Fig. 7. SEM and EDS mapping image of the cross section of laser treated NiP coating.

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Fig. 8. SEM images of NiP/CSP composite coating of a) As-plated (0.5 g/l), a1)As-plated (2.5 g/l), b) Heat treated (0.5 g/l), b1) Heat treated (2.5 g/l), c) Laser treated
(0.5 g/l) and c1) Laser treated (2.5 g/l).
constituents of NiP coating and the mild steel substrate. Diffusion of Fe
elements from the substrate to the upper surface of the coating was also
observed. This indicates the occurrence of effective rapid solidification
and diffusion phenomenon during the laser treatment.
A change in the morphology of as-plated NiP/CSP composite
coating was seen after the initial (0.5 g/l) dispersion of CSP in the
electroless bath (Fig. 8a). Formation of smooth spherical nickel globules
are seen on the surface of NiP/CSP (0.5 g/l) composite coating. The
reinforcement of CSP had led to two phenomena, namely, the formation
of spherical nickel globules and the increase in the coating rate. The
formation of nickel globules was presumably related to the increase in
the nucleation site created by the CSP. The tendency of CSP for in-
creasing the nucleation site has been reported in the author's previous
article [16]. Along with the spherical nickel globules, CSP reinforced
with NiP matrix was also observed in the morphology of as-plated NiP/
CSP (0.5 g/l) composite coating. There was an increase in the nickel
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Surface & Coatings Technology 357 (2019) 543–558
globules following an increase in the addition of CSP (0.5 g/l to 2.5 g/l)
in the bath. Among the various weight dispersed NiP/CSP composite
coatings, NiP/CSP (2.5 g/l) composite coating exhibited more nickel
globules due to the high weight dispersion of CSP in the NiP matrix
(Fig. 8a1). The high dispersion of CSP caused a higher catalytic nature
in the bath, generating more nickel globules in the surface of NiP/CSP
(2.5 g/l) composite coating. The increase in the catalytic nature caused
an increase in the rate of deposition of nickel and other constitution
ions of the CSP. Fig. 9 shows the cross section images of as-plated, heat
treated and laser treated NiP/CSP composite coatings. All coatings were
uniformly distributed over the mild steel surface. To discuss the coating
thickness related to the rate of deposition, coating thickness measured
across the cross section of the coatings is shown in the Table 4.
There was a considerable increase in the coating thickness for as-
plated NiP/CSP composite coating with increasing the weight disper-
sion of CSP from 0.5 g/l to 2.5 g/l in the bath. A high coating thickness
A. S. et al. Surface & Coatings Technology 357 (2019) 543–558

Fig. 9. Cross section SEM images of a) As-plated (0.5 g/l), a1) As-plated (2.5 g/l), b) Heat treated (0.5 g/l), b1) Heat treated (2.5 g/l), c) Laser treated (0.5 g/l) and c1)
Laser treated (2.5 g/l).

Table 4 of 29 μm was achieved for as-plated NiP/CSP (2.5 g/l) composite

Coating thickness measured across the cross section. coating among the other as-plated NiP/CSP composite coatings. The
S. no Samples As-plated (μm) Heat treated (μm) Laser treated increase in the coating thickness was due to the increase in the rate of
(μm) deposition which was the result of the catalytic effect created by the
CSP in the NiP bath. Elemental mapping across the surface of as-plated
1 NiP 18 20 54
NiP/CSP (2.5 g/l) composite coating (Fig. 10) confirmed the presence of
2 NiP/CSP (0.5 g/l) 22 23 52
3 NiP/CSP (1.0 g/l) 24 24 50
Ni, P, Ca, Mg, and Fe elements, which are the constituents of NiP ma-
4 NiP/CSP (1.5 g/l) 25 25 48 trix, CSP, and mild steel substrate. Instability of the bath was observed
5 NiP/CSP (2.0 g/l) 27 28 44 with increasing the weight dispersion of CSP to 3 g/l in the bath, which
6 NiP/CSP (2.5 g/l) 29 29 40 had an effect on the deposition process for the NiP/CSP (3 g/l) com-
7 NiP/CSP (3.0 g/l) 20 19 18
posite coating. Bath instability turning the NiP bath from green color to
black color was also observed during the deposition of NiP/CSP (3 g/l)
composite coating.
Not much change was seen in the surface morphology and coating

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Fig. 10. SEM and EDS mapping image of as-plated NiP/CSP (2.5 g/l) composite coating.
thickness of heat treated NiP/CSP composite coating when compared to
the as-plated NiP/CSP composite coating in respect to the various dis-
persions of CSP in the bath (Fig. 8b). However, laser treated NiP/CSP
composite coating exhibited a structural change in the surface mor-
phology (Fig. 8c). There was a formation of dendrites structure, which
is similar to the laser treated NiP coating. However, there was the oc-
currence of a greater reduction in the growth of dendrites due to the
reinforcement of CSP. The restriction in dendrites growth could be due
to two reasons: one was the formation of Meta stable phases and other
was the co-mixture of the inter-dendrite liquids (Ca, Mg, and Si) during
the melting and solidification. Dissolving nature of CSP constitutes like
Ca, Mg, and Si in the NiP matrix during the coating process is discussed
in the previous article [16]. These reinforced elements tend to melt
during the laser treatment and increase the density of the nickel liquid.
Hence, the high density created by the constituent elements of CSP
restricts the growth of the Ni dendrites during the solidification. On
increasing the weight dispersion of CSP, there was a continuous de-
crease in the growth of Ni dendrites. Low dendrite growth was seen for
laser treated NiP/CSP (2.5 g/l) composite coating as a result of the in-
crease in both Meta stable phases and density of intermetallic liquid
created by the high dispersion of CSP (Fig. 8c1). The restriction in
dendrite growth resulted in a decrease in the coating thickness for laser
treated NiP/CSP composite coatings. Hence, a low coating thickness of
36 μm was obtained for laser treated NiP/CSP (2.5 g/l) composite
coating compared to the other laser treated NiP/CSP (0.5 g/l) compo-
site coatings.
The cross section of laser treated NiP/CSP (0.5 g/l) composite
coating and NiP/CSP (2.5 g/l) composite coating are shown in Fig. 9c
and c1. Numerous pores and voids formed around the dendrites are
seen across the cross section of the laser treated NiP/CSP (0.5 g/l)
composite coating. On increasing the weight dispersion of CSP, there
was an increase in the pores due to the decreased hardness of the NiP/
CSP composite coating prior to the laser processing. NiP/CSP (2.5 g/l)
composite coating exhibited many pores, voids, and cracks across the
cross section of the coatings. The formation of pores and voids was the
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Surface & Coatings Technology 357 (2019) 543–558
result of the inter-metallic shrinkage that occurred around the dendrites
during the growth of the Ni. The low hardness values of NiP/CSP
(2.5 g/l) composite coating caused crack formation in the coatings.
However, the depth of the crack did not reach the substrate material.
Elemental mapping of laser treated NiP/CSP (2.5 g/l) composite coating
clearly showed the presence of elements Ni, P, Mg, Fe, and Ca elements
across the cross section and porosity around the dendrites (Fig. 11).
3.3. Phase structure characterization
NiP is a eutectic alloy which induces phase changes during the
application of thermal stress. Hence, it is important to study the effect
of phase changes before and after the heat treatment and the laser
treatment process. The XRD pattern obtained for NiP and NiP/CSP (as-
plated, heat treated and laser treated) composite coatings are shown in
Fig. 12.
As-plated NiP coating exhibited a typical amorphous structure
presented as one broad diffraction peak NiP (111) at angle 2θ = 45.5°,
indicating the solid solution of phosphorus in Ni matrix [20]. There was
a phase structure change in the NiP coating following the heat treat-
ment and laser treatment process. Heat treated NiP coating exhibited a
micro-crystalline structure with various Meta stable phases (Fig. 12a).
The pattern of heat treated NiP coating showed several sharp peaks at
angle 2θ = 45°, 37°, 50°, and 62° evidencing the formation of phases
like Ni (111), Ni12P5 (112), and Ni3P (103) respectively. These phases
had led to precipitation hardening in the coating, which was the pri-
mary reason for the increase in the hardness of heat treated NiP coat-
ings. The XRD pattern obtained for the laser treated NiP coating evi-
denced the formation of both amorphous and crystalline phase
structures. The peak at angle 2θ = 42° indicated the existences of
amorphous Ni12P5 phase. The formation of amorphous Ni12P5 phase
was due to the re-calescence effect caused during the rapid solidifica-
tion. Various peaks at angle 2θ = 32°, 36.5°, and 43° represents mi-
crocrystalline Ni3P (111) and Ni (111) phases. The formation of Ni3P
(111) confirmed the effective solid solution of nickel and phosphorus
A. S. et al.
Fig. 11. SEM and EDS mapping image of laser treated NiP/CSP (2.5 g/l) composite coating.
elements. Additional peaks were formed for laser treated NiP coating at
various angle of 2θ = 36.5° and 67.5° in contrast to heat treated coat-
ings. These peaks indicated the presence of FeNi2P phase. The forma-
tion of FeNi2P phase was due to the inter-diffusion phenomenon that
took place between the two liquids (Ni and P) and Fe constitutions of
the substrate during the laser processing. The diffusion of Fe solute in
two alloying liquid (Ni and P) could have led to the weaker atomic
interaction, thus decreasing the crystallization process. This induced an
amorphous structure for the laser treated NiP coating.
The patterns of as-plated NiP/CSP composite coatings shown in
Fig. 12b and c are almost similar to the amorphous structure of as-
plated NiP coating. The initial dispersion of crab shell particles (0.50 g/
l) had no effect on the crystallographic structure of as-plated NiP/CSP
(0.50 g/l) composite coatings. However, with increasing the weight
dispersion of CSP to 2.5 g/l in the bath, there was a slight shift in the
peak of NiP (111) for as-plated NiP/CSP (2.5 g/l) composite coating.
The peak shift from angle 45.5° of NiP coating to 42.5° of as-plated NiP/
CSP (2.5 g/l) composite coating indicates the increase in the internal
stress created by the CSP in the NiP matrix. Peaks obtained at angle
26.8°, 62.5°, and 42.5° also confirm the existence of element Ca, Mg,
and NiP, which are the constituents of NiP matrix and CSP. On com-
parison with as-plated and heat treatment, laser treatment had greatly
influenced the change in crystallographic structure of NiP/CSP com-
posite coatings. Heat treated NiP/CSP composite coating exhibited a
microcrystalline structure, which is in sharp contrast to the amorphous
structure of as-plated NiP/CSP composite coating. The sharp diffraction
peak at an angle 44° evidenced the existence of face center cubic Ni
(111) and microcrystalline structure. Dispersion of CSP (0.50 g/l) in the
NiP matrix has led to the formation of more Meta stable phases and
peak shift phenomenon (Fig. 12b). Meta stable phases like Ni12P5 (112)
and Ni3P (103) formulated at various angle of 2θ = 64° and 22.5° are
due to the heat treatment process. The shift in the peak of Ni (111)
plane to the lower angle was also evidenced for heat treated NiP/CSP
(0.5 g/l) composite coatings with the initial dispersion of CSP (0.5 g/l)
in the bath, when compared to the heat treated NiP coating. Gradual
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Surface & Coatings Technology 357 (2019) 543–558
increase in the peak shift was seen with increasing the weight disper-
sion from 0.5 g/l to 2.5 g/l of CSP in the bath. This was the result of the
maximum replacement of nickel ions by the constituent's elements (Mg
and Ca) of CSP, which increases internal stress and precipitate forma-
tion [16]. The peak around an angle 2θ = 56° of heat treated NiP/CSP
(2.5 g/l) composite coatings indicated the presence of Mg, while the
peak at an angle 2θ = 24° represented the existence of Ca elements
(Fig. 12c). The presence of peaks Mg and Ca evidences the effective
solid solution of elements of CSP with the NiP matrix.
The XRD pattern of laser treated NiP/CSP composite coatings
showed a typical peak of Ni3P and FeNi2P formed at an angle of 36.5°,
45°, and 47.8°. This was similar to the laser treated NiP coating.
However, there was a slight shift in the angle for Ni3P and FeNi2P
phases from a higher angle to a lower angle for laser treated NiP/CSP
composite coatings. The presence of Mg and Ca was seen at angle of
57.5° and 24° respectively. The existence of these peaks confirmed the
solid solution strengthening of CSP elements in the NiP matrix. Apart
from the peak shift, the presence of Ca and Mg elements played a major
role in the formation of the FeNi2P phase. As discussed earlier, the
formation of FeNi2P phase was the result of the diffusion of Fe elements
from the substrate to the coating surface. The diffusion is depended on
the hardness of the coatings, on account of which, the maximum
hardness of NiP coating resulted in a low diffusion of Fe elements. This
caused a low distribution of FeNi2P phases in the laser treated NiP
coating compared to the laser treated NiP/CSP composite coatings. The
formation and distribution of FeNi2P phase increased with the initial
dispersion of CSP (0.5 g/l) in the coating. This was due to the decrease
in the hardness of as-plated NiP/CSP composite coating. On comparison
with various weight dispersion, laser treated NiP/CSP (2.5 g/l) com-
posite coating presented more FeNi2P peaks. This was due to the lower
hardness of as-plated NiP/CSP (2.5 g/l) composite coating, which al-
lowed the diffusion of more Fe elements from the substrate to the
surface.
A. S. et al. Surface & Coatings Technology 357 (2019) 543–558

Fig. 12. XRD diffraction pattern of As-plated, Heat treated and laser treated of a) NiP coating, b) NiP/CSP (0.50 g/l) composite coating, and c) NiP/CSP (0.50 g/l)
composite coating.

Fig. 13. Micro hardness of mild steel, NiP, and NiP/CSP composite coatings (As-plated, Heat treated and laser treated).

3.4. Microhardness analysis
The surface hardness of mild steel, NiP, and NiP/CSP composite
coating (as-plated, heat treated, and Laser treated) measured using a
Vickers hardness tester is shown in Fig. 13.
It was clearly evident that the surface hardness of mild steel is in-
creased after NiP and NiP/CSP coating in the as-plated condition itself.
As for the as-plated NiP/CSP composite coating, there was a decrease in
the hardness with the incorporation of CSP (0.50 g/l) into the NiP
matrix. There was a continuous decline in the hardness of as-plated
NiP/CSP composite coating due to the increase in the weight dispersion
(0.50 g/l to 2.5 g/l) of CSP in the electroless NiP bath. This was due to
the defect substitutional solid solution strengthening mechanism, which
has been discussed in the author's previous articles [16]. In electroless

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A. S. et al.
Fig. 14. Friction coefficient of mild steel, NiP, and NiP/CSP composite coatings (As-plated, Heat treated and laser treated).
coating process, the solution state of Ni and P elements forms the solid
NiP matrix on the substrate. Hence, the solubility of reinforcement
particles plays a significant role in defining the hardness of the coatings.
Similar to this, the dissolved Ca, Mg, and Si elements in the NiP bath
tend to replace several Ni atoms in certain positions of the lattice,
making the NiP matrix softer. This phenomenon leads to a decrease in
the hardness of as-plated NiP/CSP composite coatings in respect to the
various weight dispersion of CSP in the bath. The solubility nature of
CSP has been discussed in the author's previous article [11]. Due to this
feature, the presence of Ca, Mg, and Si is increased in the NiP bath due
to increase in the weight dispersion of CSP. This caused a decrease in
the hardness of as-plated NiP/CSP composite coating with increasing
the weight dispersion of CSP from 0.50 g/l to 2.5 g/l. The decrease or
increase in the hardness of the coatings owing to the hardness of re-
inforcement particles has been referred in many articles [21,22].
There was an increase in the hardness of NiP and NiP/CSP com-
posite coating (0.50 g/l, 1.0 g/l, 1.5 g/l, 2.0 g/l and 2.5 g/l) following
the heat treatment process, when compared to the as-plated coatings.
However, there was no change in the decreasing sequence of hardness
values of heat treated NiP/CSP composite coating with increasing the
weight dispersion of CSP from 0.5 g/l to 2.5 g/l similar to the as-plated
NiP/CSP composite coating. Among the various weight dispersions of
CSP, heat treated NiP/CSP (0.5 g/l) composite coating presented a
higher hardness value. An increase in the weight dispersion from 0.5 g/l
to 2.5 g/l caused a considerable decrease in the hardness of the coatings
due to the reinforcement of soft CSP in the matrix as discussed earlier
for the as-plated NiP/CSP composite coating. Heat treatment caused a
phase transformation of coatings from amorphous to crystalline struc-
ture, which played a huge role in the hardness of the coatings [23].
During the phase transformation, there was a formation of Meta stable
Ni3P precipitates, which was considered as the reason for the increase
in the hardness for heat treated NiP/CSP composite coating when
compared to the as-plated NiP/CSP composite coating. These pre-
cipitates are generally formed as Ni–Ni3P interfaces, generally in-
creasing the interfacial free energy of Ni3P as discussed in the previous
article [16]. The inclusion of Ca and Mg atoms could cause a decrease in
the interface strength of Ni and Ni3P as the result with a decrease in the
hardness for heat treated NiP/CSP composite coatings. The inclusion of
CSP constituent between Ni and Ni3P was intensified on increasing the
CSP in the bath. Hence, the maximum dispersion of CSP (2.5 g/l)
achieved a low hardness compared to the minimum dispersion of CSP in
the bath.
Hardness of laser treated NiP coating increased to 966 HV0.05 from
507 HV0.05 of as-plated NiP coating. The increase in hardness was
caused by the formation of hard dendrites phases Ni3P and FeNi2P in
the coating. The rapid growth of dendrite was the result of rapid soli-
dification, which caused microstructural changes in the laser treated
coatings. This dendrites caused a fine crystalline structure by restricting
the growth of the grains of Ni matrix, thereby, increasing the hardness
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Surface & Coatings Technology 357 (2019) 543–558
of the coatings.
A comparison with as-plated and heat treated, laser treated NiP/CSP
(0.5 g/l) composite coating presented a high surface hardness of
662 HV0.05 with the initial dispersion of CSP (0.5 g/l) in the NiP. There
was an increasing trend in the hardness value for laser treated NiP/CSP
composite coatings following an increase in the weight dispersion of
CSP from 0.5 g/l to 2.5 g/l in the bath, which is in contrast to the as-
plated NiP/CSP composite coating. The increase in the hardness after
laser treatment is due to the formation of Ni3P and FeNi2P phases as
discussed earlier for the laser treated NiP coating. The formation of
these phases was increased considerably with increasing the addition of
CSP with NiP matrix. Among the various weight dispersions, NiP/CSP
(2.5 g/l) composite coating presented a high hardness value. This was
due to the increase in the formation and refinement of Ni3P and FeNi2P
dendrites phases in the coating. The low hardness of as-plated NiP/CSP
(2.5 g/l) composite coating was the primary cause for the diffusion of
more Fe elements to the surface of the coatings during the laser pro-
cessing. These Fe elements tend to solidify with the NiP matrix and
form as a FeNi2P phase in the coatings which resulted in the increase in
hardness value. Hence, the distribution of more FeNi2P phase had been
the reason for the higher hardness of laser treated NiP/CSP (2.5 g/l)
composite coating.
3.5. Friction-wear study
Fig. 14 shows the average friction coefficient measured for mild
steel, NiP and NiP/CSP (as-plated, heat treated, and Laser treated)
composite coatings. High friction coefficient was exhibited for mild
steel on sliding against hardened EN-31 steel in comparison with NiP
and NiP/CSP composite coatings. A decrease in the friction coefficient
after NiP and NiP/CSP composite coatings on mild steel was evident.
The increase in the friction coefficient of mild steel indicated the high
wearing out of material from the mild steel. The wear rate calculated
using the mass loss is presented in Fig. 15. From the Figure, it is clear
that mild steel exhibited a high wear rate when compared to the NiP
and NiP/CSP composite coatings. Hence, modification of the surface of
mild steel was seen as important for controlling friction and wear rate.
As plated NiP coating exhibits a friction coefficient of 0.31 which is
comparatively less than the uncoated mild steel. The low friction
coefficients of as-plated NiP coating are due to the lubrication created
by the nickel during the sliding against EN-31 steel and as a result of
which, wear rate of the NiP coating was also reduced.
To discuss the wear mechanism, SEM image of the wear track of NiP
and NiP/CSP composite coating was taken and shown in Fig. 16. Ad-
hesive and abrasive wear as the dominant wear mechanism for as
plated NiP coating (Fig. 16a). Ploughing furrows, abrasive grooves, and
scratches are visible in the wear track of as-plated NiP coating, which
indicates the characteristic of abrasive wear. This could be due to third
body particles called wear debris removed during the sliding. Along
A. S. et al.
Fig. 15. Wear rate of mild steel, NiP, and NiP/CSP composite coatings (As-plated, Heat treated and laser treated).
with grooves, there was a shallow region in the wear track which in-
dicated the existence of adhesive wear. Generally, NiP coatings are
subjected to severe adhesive wear on sliding against the carbon steel.
This is due to the high force of attraction between the nickel atoms from
NiP coating and iron from the counterface. Hence, in the as-plated
condition or at a high load condition, NiP coatings fail to sustain the
adhesive wear. As a result, the wear rate of as-plated NiP coating is high
when compared to the heat treated and laser treated NiP coating.
Heat treated NiP coating and laser treated NiP coating have shown a
low friction coefficient of 0.24 and 0.37 when compared to as-plated
NiP coating. The low friction coefficient of heat treated NiP coating was
due to improved hardness created by the Ni3P precipitates. The pre-
sence of Ni3P phase in the soft Ni matrix could act as a hard precipitate
and reduce the material (Ni) transfer from the coating to the EN-31
counterface. In general, nickel and iron have a high mutual solubility
[24] indicating the substantial attractive forces between atoms of nickel
and iron, as a result of which, adhesive wear was severe in the case of
as-plated NiP coating. However, in the case of heat treated NiP coating,
mutual solubility of nickel and iron obtained through the formation
Ni3P precipitates was low. Hence, the interaction of Ni3P precipitates
Fig. 16. SEM image of the wear track of (a–c) As-plated, Heat treated and laser treated NiP coating and (d–e) As-plated, Heat treated and laser treated NiP/CSP
(2.5 g/l) composite coating.
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Surface & Coatings Technology 357 (2019) 543–558
with the iron in EN-31 resulted in an incompatible sliding surface,
thereby causing a slight reduction in the adhesive wear and friction
coefficient of heat treated NiP coating. Typical characteristics of abra-
sive wear were also seen in the wear track of heat treated NiP coating
(Fig. 16b). Along with the abrasive wear, adhesive wear marks were
spotted in the wear track but were very low compared to the as-plated
NiP coating. Primary cracks started generating on the wear track of heat
treated NiP coating due to the existence of crystalline nature in the
coatings.
Laser treated NiP coating presented a lower wear rate and a slight
increase in the friction coefficient when compared to the heat treated
NiP coating. The increase in the friction coefficient arose as a result of
the phase transformation of the coatings and formation of dendrites
structure. The sliding interaction of FeNi2P phase in the NiP coating and
iron from the counterface resulted in an increase in the friction coef-
ficient. The distribution of Ni3P, Ni12P5, and FeNi2P phase in the
crystallographic structure played a vital role on decreasing the wear
rate of laser treated NiP coating. The formation of these phases de-
creases the mutual solubility of nickel with the iron of the counterface
during the sliding, thereby reducing the compatibility of two sliding
A. S. et al.
surface (nickel and iron) as discussed earlier. The increase in the in-
compatibility of two surfaces caused a substantial reduction in the wear
rate of laser treated NiP coating. No cracks were seen in the wear track
of laser treated NiP coating in contrast to the heat treated NiP coatings
(Fig. 16c). The existence of the crystalline and amorphous phase tran-
sition across grain-matrix interfaces of laser treated NiP coating limits
the formation of cracks during their interaction with the counterface.
Wear track also evidenced the initiation of material removal due to the
soft matrix components (alpha nickel). Partial damage was also seen for
the dendrite structure (Ni3P, Ni12P5 and FeNi2P), as a result of the re-
moval of soft nickel matrix during their interaction with the counter-
face. However, dendrites did exist on the wear track, playing a vital role
on the decrease in the wear rate of laser treated NiP coating. Therefore,
the increase in the amount of hardening phase and dendrites formation
had been the primary reason for a better wear resistance for laser
treated NiP coating.
There was a reduction in the friction coefficient and wear rate for
as-plated NiP/CSP composite coatings after the reinforcement of CSP in
the NiP matrix. Friction coefficient decreased considerably with in-
creasing the weight dispersion of CSP from 0.5 g/l to 2.5 g/l in the NiP
bath and found increasing for the 3.0 g/l dispersion. The decrease in the
friction coefficient was due to the lubricity created by the constituent's
elements of CSP (Ca, Mg, and O) and matrix elements (Ni) in the surface
of the NiP coating. The constituent elements of CSP were dissolved in
the NiP matrix during the solid solution strengthening process, as a
result of which, lubricity is increased for the NiP/CSP coatings [17].
Among the various weight dispersions of CSP, NiP/CSP (2.5 g/l) com-
posite coating presented a low friction coefficient of 0.06. This was due
to the reinforcement of more constituent elements of CSP in NiP matrix.
The presence of these elements in the coatings generally leaves a way
for two factors; one is the increase in the lubrication during the sliding
against the EN-31 counterface and other is decrease in the compatibility
of the two sliding surfaces. The decrease in the compatibility of two
surfaces certainly reduced the adhesive wear. Hence, these two factors
resulted in a low friction coefficient and improved wear behavior.
Tribolayer formation was seen in the wear track of as-plated NiP/CSP
(2.5 g/l) composite coatings (Fig. 16d). However, its distribution was
only partial. The poor adhesion of the tribolayer in the wear track fa-
cilitated the material removal by the counter face during the sliding.
The poor adhesion of tribolayer was primarily due to the amorphous
nature of the as-plated NiP/CSP composite coating.
Heat treated NiP/CSP composite coatings had shown a low friction
coefficient and wear rate compared to the as-plated NiP/CSP composite
coating. There was a considerable decrease in the friction coefficient
with increasing the weight dispersion from 0.50 g/l to 2.5 g/l similar to
the as-plated NiP/CSP composite coatings. Heat treated NiP/CSP
(2.5 g/l) composite coating exhibited a low friction coefficient of 0.01
and a low wear rate, which was comparatively lower than the as-plated
NiP/CSP (2.5 g/l) composite coating. This was due to the sustainment
of tribolayer formation in the wear track during the sliding. The phase
transformation of NiP/CSP composite coating from the amorphous
phase to the crystalline phase certainly improved the adhesion of tri-
bolayer in the wear track. As a result, the formed tribolayer tend to
adhere more efficiently than in the as-plated NiP/CSP composite
coating, thereby reducing the friction coefficient and wear rate. The
formation of tribolayer was clearly seen in the wear track of heat
treated NiP/CSP (2.5 g/l) composite coatings (Fig. 16e), indicating the
smooth sliding of the counterface. This smooth sliding evidenced the
decrease in the friction coefficient and wear rate. In addition to the
tribolayer, the formation of Ni3P precipitates and reinforcement of CSP
in the NiP matrix had increased the strength of the matrix while de-
creasing the compatibility of two sliding surfaces. These two factors
could also constitute the reason for the low friction and wear rate of
heat treated NiP/CSP composite coatings.
There was an increase in the friction coefficient for laser treated
NiP/CSP composite coatings when compared to the as-plated and heat
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Surface & Coatings Technology 357 (2019) 543–558
treated NiP/CSP composite coatings. There was a considerable increase
in the friction coefficient with increase in the weight dispersion of CSP
from 0.50 g/l to 2.5 g/l in the bath. The interaction of iron phase with
the iron elements of the counterface had increased the friction force
during the sliding as discussed earlier. Hence, the formation of FeNi2P
phase in the NiP/CSP composite coatings had a great influence on the
increase in the friction coefficient. Among the various weight disper-
sions of CSP, NiP/CSP (2.5 g/l) composite coatings presented a high
friction coefficient of 0.65. This is because, the formation of FeNi2P
phase increases with increasing the weight percentage as discussed in
the XRD analysis. Hence the interaction of FeNi2P phase against the
counterface was found more for the laser treated NiP/CSP (2.5 g/l)
composite coating. As result, there was an increase in the friction
coefficient for laser treated NiP/CSP (2.5 g/l) composite coatings when
compared to the other heat treated and as-plated NiP/CSP composite
coatings. Despite an increase in the friction coefficient, there was a
decrease in the wear rate for laser treated NiP/CSP composite coating
when compared to the other coatings. The decrease in the wear rate was
related to the presence of hard crystalline Ni3P, Ni, FeNi2P phases and
amorphous Ni12P5 phase. The presence of these phases caused restric-
tions on the material removal during the sliding with the counter face.
The reduction in the growth of dendrites structure also played a major
role in decreasing the wear rate for laser treated NiP/CSP composite
coating. No deformation in the dendrites was observed in the wear
track of laser treated NiP/CSP (2.5 g/l) composite coating after the
sliding with the counter face (Fig. 16f). This was due to the better in-
terface strength of dendrites (Ni3P and FeNi2P) with the Ni matrix.
Though cracks were seen in the morphology of laser treated NiP/CSP
composite coating, its influence in the wear performance is very low, as
the cracks were seen overlapped with the formation of tribolayer. A
tribolayer was also seen in the wear track strongly adhered to the
surface. EDS confirms the presence of Ni, P, Ca, Mg and O elements in
the wear track of laser treated NiP/CSP (2.5 g/l) composite coating
(Fig. 17). This indicated the existence of coatings in the wear track. In
addition to the constituent's elements of NiP matrix and CSP, presence
of O is evidenced in the wear track. The presence of O indicates the
occurrence of oxidation during the sliding.
In case of laser treated NiP coating, wear was initiated by the re-
moval of soft Ni matrix. However, it was restricted in the laser treated
NiP/CSP composite coating due to the strengthening of alpha nickel
with the constituents (Ca, Mg and O) of CSP and presences of hard
FeNi2P phase. These constituents increased the strength of Ni matrix in
such way that it produced enough lubrication and toughness to the
coatings during the sliding with the counterface. Therefore, laser
treated NiP/CSP composite coating presented a lower wear rate than
the as-plated and heat treated NiP/CSP composite coatings.
4. Conclusions
Electroless NiP and NiP/CSP composite coatings were prepared with
various weight dispersions of CSP. The following conclusions have been
drawn from a comparative study of heat treatment and laser treatment
with as-plated NiP and NiP/CSP composite coatings:
• A spherical nickel globule was formed for as-plated and heat treated
NiP/CSP (0.5 g/l) composite coating with the initial dispersion of
CSP (0.5 g/l) and found increasing with the increase in CSP dis-
persion. Laser treated NiP and NiP/CSP composite coatings ex-
hibited a morphological change with the formation of dendrite
structure. Laser treated NiP/CSP (2.5 g/l) composite coating showed
a reduction in the dendrite structure with maximum porosity as a
result of the high weight dispersion of CSP in the NiP matrix.
• Formation of Meta stable phases was seen for heat treated NiP and
NiP/CSP composite coatings. In addition to the Meta stable phases,
there was a formation of FeNi2P phase for laser treated coatings.
More FeNi2P phase was formed for NiP/CSP (2.5 g/l) composite
A. S. et al.
Fig. 17. EDS mapping of the wear track of laser treated NiP/CSP (2.5 g/l) composite coating.
coating, which was due to the low hardness of the coating prior to
the laser treatment.
•
Both as-plated and heat treated NiP/CSP composite coating pre-
sented a low hardness with increasing the dispersion of CSP in NiP
matrix. However, hardness increased for Laser treated NiP/CSP
composite coating with increasing the dispersion of CSP. Higher
hardness was achieved for laser treated NiP/CSP (2.5 g/l) composite
coating due to the formation of FeNi2P phase.
• On a comparison of friction and wear property, as-plated and heat
treated NiP and NiP/CSP composite coatings presented a low fric-
tion coefficient and a moderate wear rate. Friction coefficient was
high for the laser treated NiP and NiP/CSP composite coatings.
However, there was a decrease in the wear rate. Wear resistance of
laser treated NiP/CSP (2.5 g/l) composite coating was better than
that of the other post treated coatings. Thus, the overall conclusion
is that laser treatment to the surface of NiP and NiP/CSP a com-
posite coating tends to increase the friction coefficient and decrease
the wear rate.
Acknowledgement
Sincere thanks to the UGC (NFST scheme) (Grant No: 201516-NFST-
2015-17-ST-TAM-2123), India for providing stipend for doing the re-
search and also to the Engineering Design Division, Anna University,
Chennai, Tamilnadu, India, for providing facilities needed for this re-
search. The authors also thank Meera laser solutions, Ambattur,
Chennai, Tamilnadu, India for providing Nd:YAG laser processing fa-
cility.
References
[1] Engineering tribology, Prasanta Sahoo, Eastern Economy Edition, (2005).
[2] Prasanta Sahoo, SumanKalyan Das, Tribology of electroless nickel coatings – a re-
view, Mater. Des. 32 (2011) 1760–1775.
[3] I. Apachitei, F.D. Tichelaar, J. Duszczyk, L. Katgerman, The effect of heat treatment
557
Surface & Coatings Technology 357 (2019) 543–558
on their structure and abrasive resistance of autocatalytic NiP and NiP–SiC coatings,
Surf. Coat. Technol. 149 (2002) 263–278.
[4] Hong Luo, Michael Leitch, Yashar Behnamian, Yongsheng Ma, Hongbo Zeng, Jing-
Li Luo, Development of electroless Ni–P/nano-WC composite coatings and in-
vestigation on its properties, Surf. Coat. Technol. 277 (2015) 99–106.
[5] Ankita Sharma, A.K. Singh, Electroless Ni-P and Ni-P-Al2O3 nanocomposite coatings
and their corrosion and wear resistance, J. Mater. Eng. Perform. 22 (2013)
176–183.
[6] D. Gutsev, M. Antonov, I. Hussainova, A.Y. Grigoriev, Effect of SiO2 and PTFE
additives on dry sliding of NiP electroless coating, Tribol. Int. 65 (2013) 295–302.
[7] Y. Wu, H. Liu, B. Shen, L. Liu, W. Hu, The friction and wear of electroless Ni–P
matrix with PTFE and/or SiC particles composite, Tribol. Int. 39 (2006) 553–559.
[8] Y. Wu, B. Shen, L. Liu, W. Hu, The tribological behaviour of electroless Ni–P–Gr–SiC
composite, Wear 261 (2006) 201–207.
[9] M.S. Jagatheeshwaran, A. Elayaperumal, S. Arulvel, Impact of nanozinc oxide on
the friction – wear property of electroless nickel-phosphorus sea shell composite
coatings, Mater. Sci. Eng. B 225 (2017) 160–172.
[10] A. Akyol, H. Algul, M. Uysal, H. Akbulut, A. Alp, A novel approach for wear and
corrosion resistance in the electroless Ni-P-W alloy with CNFs co-depositions, Appl.
Surf. Sci. 453 (2018) 482–492.
[11] S. Arulvel, A. Elayaperumal, M.S. Jagatheeshwaran, Discussion on the feasibility of
using proteinized/deproteinized crab shell particles for coating applications:
synthesis and characterization, J. Environ. Chem. Eng. 4 (2016) 3891–3899.
[12] Jothi Sudagar, Jianshe Lian, Wei Sha, Electroless nickel, alloy, composite and na-
nocoatings – a critical review, J. Alloys Compd. 571 (2013) 183–204.
[13] M.S. Jagatheeshwaran, A. Elayaperumal, S. Arulvel, Wear characteristics of elec-
troless NiP/bio-composite coatings on En8 steel, J. Manuf. Process. 20 (2015)
206–214.
[14] J.N. Balaraju, K.S. Rajam, Electroless deposition and characterization of high
phosphorus Ni-P-Si3N4 composite coatings, Int. J. Electrochem. Sci. 2 (2007)
747–761.
[15] H. Liu, Y.Y. Lv, Z. Liu, H. Liu, G.E. Thompson, Dry sliding wear behaviour and
structural characteristics of laser-annealed electroless Ni–P/Ni–Mo–P duplex coat-
ings, Tribol. Int. 103 (2016) 343–351.
[16] S. Arulvel, A. Elayaperumal, M.S. Jagatheeshwaran, Controlling adhesive wear
failure of nickel-phosphorus coating at high load condition using crab shell particle
as reinforcement, Eng. Fail. Anal. 90 (2018) 310–323.
[17] M. Franco, W. Sha, S. Malinov, R. Rajendran, Phase composition, microstructure
and microhardness of electroless nickel composite coating co-deposited with SiC on
cast aluminium LM24 alloy substrate, Surf. Coat. Technol. 235 (2013) 755–763.
[18] D. Prokoshkina, V.A. Esin, G. Wilde, S.V. Divinski, Grain boundary width, energy
and self-diffusion in nickel: effect of material purity, Acta Mater. 61 (2013)
5188–5197.
[19] Rastislav Mikuš, Ivan Kováč, Jozef Žarnovský, Effect of microstructure on properties
A. S. et al.
of NiCrBSi alloys applied by flame-powder deposition, Adv. Mater. Res. 1059
(2014) 1–9.
[20] Felipe Samuel Goettems, Jane Zoppas Ferreira, Wear behaviour of electroless heat
treated Ni-P coatings as alternative to electroplated hard chromium deposits, Mater.
Res. 20 (2017) 1300–1308.
[21] M. Ebrahimian-Hosseinabadi, K. Azari-Dorcheh, S.M. MoonirVaghefi, Wear beha-
vior of electroless Ni–P–B4C composite coatings, Wear 260 (2006) 123–127.
558
Surface & Coatings Technology 357 (2019) 543–558
[22] Q. Zhao, Y. Liu, H. Muller-Steinhagen, G. Liu, Graded Ni–P–PTFE coatings and their
potential applications, Surf. Coat. Technol. 155 (2002) 279–284.
[23] M.S. Jagatheeshwaran, A. Elayaperumal, S. Arulvel, The role of calcinated sea shell
particles on friction-wear behavior of electroless NiP coating: fabrication and
characterization, Surf. Coat. Technol. 304 (2016) 492–501.
[24] M. Hansen, Constitution of Binary Alloys, McGraw Hill, New York, 1958, p. 29.