Materials Today: Proceedings 22 (2020) 1038–1042

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Mechanical and tribological properties of electroless nickel phosphorous

and nickel Phosphorous-Titanium nitride coating
D. Umapathi a,⇑, A. Devaraju a, C. Rathinasuriyan b, A. Raji a
a
Department of Mechanical Engineering, Adhi College of Engineering and Technology, Kancheepuram, Chennai, India
b
Department of Mechanical Engineering, Vel Tech, Avadi, Chennai, India

a r t i c l e i n f o a b s t r a c t

Article history: Electroless coating technology is a traditional surface modification method that has wide applications in
Received 20 May 2019 various industries. In this work, nickel phosphorous and nickel phosphorous-titanium nitride coating on
Received in revised form 25 November 2019 EN8 steel using the electroless plating method. The effects of NiP and NiP–TiN on the mechanical and tri-
Accepted 27 November 2019
bological properties of EN8 steel coatings were investigated. The wear behavior was investigated through
Available online 27 December 2019
a Pin on Disc tribometer, a test carried out against the counterpart of SS-304 grade stainless steel. The
worn surface and surface hardness of the coated samples were analyzed by Trinocular microscope and
Keywords:
microhardness testing machine respectively.
Electroless coating
Friction
Ó 2019 Elsevier Ltd. All rights reserved.
Wear Selection and peer-review under responsibility of the scientific committee of the International
Micro hardness Conference on Materials Engineering and Characterization 2019.

1. Introduction
The friction is an experiential study and does not allow reaching
precise results, but only to useful approximately conclusions [1].
Wear is defined as deterioration and gradual removal or deforma-
tion of material at solid surfaces [2]. A coating is a covering that is
applied to the surface of an object, usually referred to as the sub-
strate. Various techniques like thermal spraying, friction surfacing,
electroplating, electroless plating, and epoxy spray painting are
used to deposit appropriate protection on the surface of materials.
Electroless Ni-P coating is one of the most popular in that class [3–
6]. Devaraju et al. [7–10] have investigated the friction coefficient
and wear mechanism for Plasma Nitriding on nuclear grade auste-
nitic stainless steel of AISI 316 LN. They have analyzed the
microstructural, hardness, XRD and dry sliding wear. They have
found that adhesion between two contact bodies is eliminated.
This reduces the friction as well as wear on austenitic stainless
steel from plasma nitriding treatment. Saravanan et al. [11] have
studied the wear performance of the hard TiN coated against the
Ti6Al4V alloy with different parametric conditions. They have
identified better wear resistance with minimal wear mass loss
for the applied load of 2 N and sliding velocity of 0.75 m/s respec-
tively. Jagatheeshwaran et a.l [12] have prepared pure NiP and NiP
with various amounts of Sea Shell Particles (SSP) on En8 steel using
⇑ Corresponding author.
E-mail address: umapathidr078@gmail.com (D. Umapathi).
the electroless coating process. They have found that better wear
property with high frictional force on NiP with sea shell particles
coatings when compared to the pure NiP coating, and uncoated
En8 substrate. Elayaperumal et al. [13] have deposited NiP with
weight fraction (3.0 g/l) of sea shell particles and various weight
fractions of nano ZnO particles on En8 steel using an alkaline elec-
troless process. Better wear resistance was observed in NiP/SSP/
ZnO (0.25 g/l) coatings when compared to NiP and NiP/SSP coating.
Gutsev. et al [14] have studied the effect of silicon dioxide and poly
tetra fluoro ethylene (PTFE) additives on NiP coating. Significant
improvement of friction and wear were obtained for NiP coated
samples while comparing PTFE or mixed additives. Bonin and Vitry
[15] have investigated the mechanical and wear properties of elec-
troless nickel monolayer, bilayers and duplex NiP/NiB coatings.
They have reported the hardness characteristics of duplex coatings
which are more influenced by NiB. Ramalho and Miranda et al [16].
have investigated the friction and wear characteristics of NiP and
NiP + PTFE coatings which is sliding contacts against hard chro-
mium steel. PTFE particles in the electroless NiP coatings have bet-
ter wear resistance. Arun and Satish Kumar [17] have investigated
the hardness and surface roughness of the electroless Ni-P coated
low carbon steel substrate. Electroless coating was carried out by
the bath containing of nickel chloride, ammonium chloride,
sodium hypophosphite, and Sodium hydroxide. They have identi-
fied that substrate material coated with pH 8, temperature
800 °C and 20 percent of phosphate has maximum hardness.
Zielinska et al. [18] have used the electroless deposition technique

https://doi.org/10.1016/j.matpr.2019.11.283
2214-7853/Ó 2019 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Conference on Materials Engineering and Characterization 2019.
 D. Umapathi et al. / Materials Today: Proceedings 22 (2020) 1038–1042 1039

for fabricating Ni–P–nano-ZrO2 composite coatings. Composition

and surface morphology of the Ni–P–nano-ZrO2 composite coat-
ings were analyzed by energy-dispersive X-ray (EDX) spectroscopy
and scanning electron microscopy (SEM) respectively. Dadvand
et al. [19] have reported electrodeposition of Ni-P from a citrate
bath whaich was containing citric acid, sodium chloride, nickel sul-
fate, sodium hypophosphite and ammonia. They have found that
cathode current efficiency twice higher when compared to the
modified Watts bath. Bredael et al. [20] was fabricated Ni-P elec-
trodeposits with various contents of phosphorus which was rang-
ing from 0 to 18.0 wt% respectively. They have found that the
plated Ni-P coatings, which possess phosphorus content of above
12 wt%. are amorphous. Saravanan et al. [21,22] have evaluated
the surface roughness, mechanical properties, tribological behav-
iors on thin nano tungsten carbide coated and Low Temperature
Carburized stainless steel. Susmit Datta et al. [23] developed TiN Fig. 2. Electroless Coating setup.
coatings on Ti6Al4V alloy and evaluated their corrosion, tribologi-
cal, mechanical and biological properties for implant applications.
They have found that the TiN coatings can be achieved by minimiz- from electroplating by not using external electrical power. The
ing coating defects. experimental setup of this works is shown in Fig. 2.
From the literature, the mechanical and tribological behavior of Electroless plating has been defined as a controlled autocat-
nickel phosphorous-titanium nitride coating on EN8 steel has not alytic deposition of a continuous layer on a catalytic surface by
been exposed clearly. The present work aims to study the mechan- the reaction of a complex compound and a chemical reducing
ical and tribological behavior of NiP-Ti coatings on EN8 steel with agent.
different surface patterns using electroless plating method. The electroless Ni-p and Ni-P/TiO2 composite coatings are
deposited on EN8 steel substrate of a size of 40 mm diametre
and 5 mm thick using an acidic hypophosphite reduced electroless
2. Materials and methods nickel–phosphorus bath. The substrate is prepared with a well-
polished surface. The electroless bath setup is shown in Table 1.
2.1. Base material All the composite coatings are post-annealed at 400 °C for an hour
in a muffle furnace in order to improve the surface properties.
In this work, EN8 steel was selected as base material. EN8 is an
unalloyed medium carbon steel which is used in applications of
2.3. Chemical composition test-OES
automotive parts like connecting rods, studs, spindles, axle, etc.
For activating the surface, pretreatment is necessary before coat-
Optical Emission Spectroscopy, or OES, is a well trusted and
ing. Pretreatment of the coating process is shown in Fig. 1.
widely used analytical technique used to determine the elemental
composition of a broad range of metals.
2.2. Electroless deposition
2.4. Micro hardness test
Electroless plating, also known as chemical or auto-catalytic
plating, is a non-galvanic plating method that involves several The basic principle of hardness, is to observe a materials ability
instantaneous reactions. Electroless plating is mainly different to resist plastic deformation from a typical source. Micro-hardness

Fig. 1. Steps involved in pretreatment of the coating process.

1040 D. Umapathi et al. / Materials Today: Proceedings 22 (2020) 1038–1042

Table 1 Table 3
Bath requirement. Microhardness of coated and uncoated material.

S. No Description Quantity Sample Micro hardness @ 0.5 N Average

NiP NiP + TiO2 Point-1 Point-2 Point-3 Point-4 Point-5
1 Nickel Sulphate 18 g/L 18 g/L Uncoated EN-8 145.3 152.6 156.4 160.2 151.3 153.6
2 Sodium Hypophosphate 23 g/L 23 g/L NiP 221.4 229.4 218.7 238.1 264.5 234.48
3 Sodium Citrate 11 g/L 11 g/L NiP + TiN 289.4 277.3 310.7 264.8 255.6 276.58
4 Acetic Acid 2–5 ml/L 2–5 ml/L
5 Titanium di-oxide – 2 g/L
6 Temperature 90 ± 20c 90 ± 20c
7 pH Value 4–5 4–5
pared to nickel phosphorous coated material. The hardness value
8 Coating timing 1h 1h
of nickel phosphorous coating is higher than uncoated sample. In
all cases, the micro hardness of the electroless work, nickel
phosphorous-titanium nitride coatings and nickel phosphorous
was measured at the centre region of coated sample using a Vick-
has improved significantly when compared to the uncoated EN-8
ers microhardness testing machine (Shimadzu HMV–2 T). The test
steel.
was performed on the coated plates with a load of 4.9 N for 20 sec
[24].
3.3. Friction and wear analysis
2.5. Wear and friction analysis
Friction and wear analysis of the substrate has been done by
using the pin on disc tribometer. The results are discussed below.
Wear and friction tests were performed in a pin-on-disc
machine (DUCOM) for uncoated, nickel phosphorous and nickel
phosphorous-titanium nitride coatings under the various loading 3.3.1. Co-efficient of friction
condtions 3–5 N under dry sliding condition. The track diameter The frictional force was measured using pin on disc tribometer
and sliding velocity of 32 mm, 0.5 m/sec were kept constant at constant sliding velocity of 0.5 m/s and sliding distance of 500 m
throughout the test respectively. from which co-efficient of friction is calculated. Co-efficient of fric-
tion for nickel phosphorous and nickel phosphorous-titanium
nitride coatings with various loading conditions are shown in
2.6. Microstructural analysis
Table 4. It is shows that, the value of coefficient of friction is
decreased when increased the load for both conditions. Coefficient
The surface morphology of coated samples is characterized
of friction for coated nickel phosphorous-titanium nitride has con-
using optical Trinocular Microscope. The crosssection which is
siderably high when compared to the coated nickel phosphorous.
taken as coated samples is polished using various grids and etched
for metallographic analysis.
3.3.2. Wear mass loss
The mass losses for both disc and pin are analyzed, and the
3. Results and discussion
results are discussed in this section. The mass of a substrate is
obtained before and after the wear test by using electronic balance.
3.1. Chemical composition test
The Fig. 3 shows that mass loss of the disc material at various load-
ing conditions with the constant sliding velocity of 0.5 m/s. It is
In this work, the coating material was selected as EN8 steel. The
noted that the mass loss of the disc gradually increases while
chemical composition of the EN8 steel was tested by the Optical
Emission Spectroscopy. The test results are presented in Table 2.
Table 4
It is confirmed that the substrate is EN8 grade steel, because that COF for NiP and NiP + TiN coated materials.
the observed readings are satisfy the standard values.
Sample ID Load (N) COF

3.2. Micro hardness evaluation NiP-1 3 0.63

NiP-2 4 0.68
NiP-3 5 0.71
After the completion of electroless deposition of Nickel Phos- NiP + TiN-1 3 0.52
phorous and Titanium coatings over the polished EN-8 substrate, NiP + TiN-2 4 0.57
the micro hardness of the material has been evaluated at the load- NiP + TiN-3 5 0.61
ing condition of 0.5 N. The microhardness was measured at five dif-
ferent locations on the substrate, and then taken as average. The
value of microhardness is presented in Table 3.
It has been noted that the hardness of the nickel phosphorous-
titanium nitride coated sample is increased by 16% when com-

Table 2
Chemical composition of substrate material.

Sl. No Elements BS-970 standard (%) Observed (%)

1 Carbon 0.36–0.44 0.365
2 Manganese 0.6 – 1.00 0.774
3 Silicon 0.10–0.40 0.224
4 Sulphur Min. 0.005 0.012
5 Phosphorous Min. 0.005 0.038
6 Iron Max. 99.0 Balance
Fig. 3. Comparison of Wear mass loss of disc.
 D. Umapathi et al. / Materials Today: Proceedings 22 (2020) 1038–1042
Fig. 4. Comparison of Wear Mass Loss of pin.
increasing the load, for both nickel phosphorous and nickel
phosphorous-titanium nitride coatings. It was found that the wear
mass loss for nickel phosphorous-titanium nitride coating is higher
when compared to the nickel phosphorous.
This is due to the higher hardness was obtained in nickel
phosphorous-titanium nitride than nickel phosphorous coatings.
It is concluded that the value of hardness is important factor which
affects the mass loss of the substrate. Wear mass loss for pin mate-
rial is shown in Fig. 4. It is noted that the mass loss of the pin is
increased while increasing the load, for both coated material. The
mass loss of pin for nickel phosphorous-titanium nitride coatings
is lesser when compared to the nickel phosphorous coating.
3.4. Microstructure analysis
The worn surfaces of the nickel phosphorous coating sample at
different loading conditions are shown in Fig. 5(a–c), which are
Fig. 5. OM images of worn surfaces of the nickel phosphorous a) 3 N b) 4 N and c) 5 N.
1041
analyzed using Trinocular microscope. The analysis of the worn
surfaces are supports the result in the wear behaviour of the coated
sample. Normally, combination of two or three wear mechanism
will exist for many tribo pairs [25]. In the present work, it was
observed that the delamination and patches formed in the nickel
phosphorous coated sample at 3 N, 4 N and 5 N respectively.
Therefore, the wear mechanism exhibits for the current study is
the combination of an abrasion and delamination.
The worn surfaces of the nickel phosphorous-titanium nitride
coating sample at different loading conditions are shown in Fig. 6
(a–c), which are analyzed using Trinocular microscope.
From these images it is observed that only a small patches were
seen on the wear track of nickel phosphorous-titanium nitride
coated specimen at the loading conditons of 3 N. There is no
delamination and patches formed at loading conditons of 3 N and
5 N respectively. Though the electroless nickel phosphorous coat-
ings have lesser hardness, and also adhesive wear that take place
to some extent on the counterpart which is tends to decrease coef-
ficient of friction. In case of nickel phosphorous-titanium nitride
coating has considerably high coefficient of friction when com-
pared to the coated nickel phosphorous.
4. Conclusion
In this work, nickel phosphorous and nickel phosphorous-
titanium nitride have successfully coated on EN8 steel using the
electroless plating method. The following conclusion are drawn
from the experimental and analyses,
 NiP-Ti coatings have better mechanical and tribological proper-
ties when compared to the Ni-P coating.The hardness of the
nickel phosphorous-titanium nitride coated sample is increased
by 16% than nickel phosphorous coated material.
 Coefficient of friction for coated nickel phosphorous-titanium
nitride has considerably high when compared to the coated
1042 D. Umapathi et al. / Materials Today: Proceedings 22 (2020) 1038–1042
Fig. 6. OM images of worn surfaces of the nickel phosphorous-titanium nitride coatings a) 3 N b) 4 N and c) 5 N.
nickel phosphorous. This is due to the higher hardness was
obtained in nickel phosphorous-titanium nitride than nickel
phosphorous coatings. The mass loss of pin and disc for nickel
phosphorous-titanium nitride coatings is lesser when compared
to the nickel phosphorous coating. It is concluded that the value
of hardness is important factor which affects the mass loss of
the substrate.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
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