Surface and Coatings Technology 137 2001.

9296

Hardness, friction and wear characteristics of nickel-SiC

electroless composite deposits
A. Grosjeana , M. Rezrazi a,U , J. Takadoumb, P. Bercot a
a

Laboratoire de Chimie des Materiaux

et Interfaces, Uni ersite de Franche-Comte,

16, route de Gray, 25030 Besancon Cedex, France

b
Laboratoire de Microanalyse des Surfaces, ENSMM, 26 chemin de lepitaphe,
25030 Besanc
on Cedex, France

Received 20 June 2000; accepted in revised form 2 October 2000

Abstract
Composite coatings constitute a new class of materials which are mostly used for mechanical and tribological applications.
Among these materials, nickel deposits with incorporation of hard ceramic particles such as silicon carbide SiC., combine
anti-corrosion properties due to the presence of nickel., with mechanical and tribological performances due to the presence of
particles of SiC.. In the present study, electroless NiSiC composite deposits with various amounts of SiC have been prepared
and characterized. The first part of this paper considers the materials, the experimental conditions and the characterization of the
coatings. The second part is dedicated to the study of the mechanical hardness. and tribological friction resistance and wear.
properties of the co-deposits. Friction tests were carried out using a ball on disk tribometer. The mechanisms of wear were
analysed from observations of the wear scars and their characterization using two-dimensional and three-dimensional profilometry. The results show that increasing the size or the rate of SiC particles incorporated lead to an increase in both the hardness
of the films and friction coefficient when sliding against a steel ball. 2001 Elsevier Science B.V. All rights reserved.
Keywords: NickelSiC electroless composite deposits; Friction; Wear; Mechanical properties

1. Introduction
Composite deposits consist of solid particles incorporated in a metallic matrix. Co-deposits are made in
order to obtain the properties not only of the matrix
but also of included particles. One recalls that a composite is a polyphase solid in which two or several
components are associated in order to obtain, on a
macroscopic scale and at least in certain directions, a
completely new set of properties which the components
taken separately cannot achieve w1x.
U

Corresponding author. Tel.: q33-3-81-66-6859; fax: q33-3-8166-6858.

E-mail address: el-mustafa.rezrazi@univ-fcomte.fr M. Rezrazi..

Electrolytic deposits are the most widely used and

studied. Various metallic matrices are co-deposited with
a great variety of hard carbides, oxides, etc.. or lubricating PTFE, graphite. particles w2x.
Some electroless nickel co-deposits such as NiPTFE
have been developed in industry because of their hardness and resistance to corrosion w36x, but most codeposits are still at the experimental stage.
In this study electroless nickel composite deposits
with various kinds and amounts of particles of SiC have
been prepared. The objective of this paper is to investigate both mechanical and tribological properties of
coatings. The effect of size and rate of SiC particles
incorporated on hardness, friction coefficient and wear
resistance was particularly analysed.

0257-8972r01r$ - see front matter 2001 Elsevier Science B.V. All rights reserved.
PII: S 0 2 5 7 - 8 9 7 2 0 0 . 0 1 0 8 8 - 4

A. Grosjean et al. r Surface and Coatings Technology 137 (2001) 9296

Table 1
Characteristics of the SiC particles used
Particles

Supplier

Designation

SiC
SiC
SiC

Mattey Johnson
Norton
Norton

E110 8000
E110 10 000

Average size m.
m.
1.00
0.75
0.50

93

approximately 10 m thickness by using a Vickers

microhardness instrument. The applied load was 300 g.
Five measurements were conducted on each sample
and the results were averaged. Since the measurement
of hardness is always influenced by the substrate, we
used the Jonsson
and Hogmark method w9x, which can

dissociate the contributions of the substrate and coating of measured hardness.

2. Experimental conditions

2.2.2. Tribological beha iour

2.1. Operating conditions

2.2.2.1. Friction. Friction tests were conducted using

a ball-on-disc tribometer. A 100C6 steel ball with a
diameter of 5 mm was used. The applied load was 10 N
and the sliding speed was 3 mm sy1 . The friction
coefficient was measured continuously during the tests.
After a duration of 15 min the tests were stopped and
the wear tracks were examined.

The electroless depositions were carried out in a cell,

where an agitation induced by the fluid circulation with
a centrifugal pump and a cascade system was used w7x.
Thus, the circulation of the bath from top to bottom
created a laminar flow of the fluid on the surface of the
sample. The average linear velocity of fluid past the
working electrode was 0.45 cm sy1 . A 750 cm3 circulation overflowing cell with two compartments s 10
cm., one regulating the temperature of 85C w8x and the
other doing the plating, was chosen. This type of cell,
with upward circulation, provided the agitation and had
the advantage of keeping the particles suspended in the
solution.
A brass substrate UZ 36 62 - Cu - 65.5 wt.%, 34.1
- Zn - 37.6 wt.%, impurities: Fe - 0.2 wt.%, Pb - 0.2
wt.%. was used to realize these deposits: the samples
75 = 35 = 0.5 mm. underwent a range of pre-treatment in order to eliminate all types of dirt mainly just
oils..
The bath contained the main constituents, i.e. nickel
sulfate 26 g ly1 ., sodium hypophosphite 30 g ly1 .,
acids, cadmium salt w8x. The deposit contained approximately 12% phosphorus.
The pH of bath was adjusted to 4.5 with a diluted
ammoniacal solution. To this initial bath were added
variable quantities of pre-treated SiC powder. The particles were immersed in hydrochloric acid to eliminate
possible impurities, then rinsed to remove Cly ions
which could contaminate the electroless bath, filtered
on a microfilter 0.2 m. and finally dried.
The characteristics of the various particles of SiC are
described in Table 1.
The percentage of embedded particles in the deposits for the same deposition time was determined by
an image analysis technique w4x. A data processing
software coupled with an optical microscope LEICA
metallux 3 was allowed to quantify the proportion of
particles in the deposit.
2.2. Mechanical characterization of the coatings
2.2.1. Measurements of Vickers hardness
These measurements were taken on samples from

2.2.2.2. Wear. Microscopic observations and profilometric analysis of the wear scars have been conducted
in order to qualify and quantify the wear of material.

3. Experimental results
3.1. Vickers hardness
The results of Vickers hardness determined with a
precision of "25 Hv, for the SiC Mattey Johnson, SiC
Norton 8000 and SiC Norton 10 000 particles according
to the inclusion rate v of the particles in the deposit
are presented in Fig. 1.
The curves have the same profile; hardness is increased gradually with increasing the rate of SiC in the
deposits until approximately:

15% for SiC Mattey Johnson;

20% for SiC Norton 8000;
16% for SiC Norton 10 000.

After the ascending phase hardness was remained

stationary with:

825 Hv for the particles of SiC Mattey Johnson;

875 Hv for the particles of SiC Norton 8000;
approximately 700 Hv for the particles of SiC Norton 10 000.

If we look at the curve showing the volume rate of

incorporation of particles in the deposit v according
to the concentration of particles in the bath C v for the
various particles of SiC Fig. 2., we notice that this
phase of stability of hardness correspond to a saturation of the deposit in particles of SiC dotted line in
Fig. 2..

94

A. Grosjean et al. r Surface and Coatings Technology 137 (2001) 9296

Fig. 1. Hardness of electroless nickelSiC incorporating various types

of SiC particles according to the rate of particles in the deposits.

The comparison of the crystallographic structure and

average size of the particles could explain the higher
values of hardness for the particles of SiC Mattey
Johnson for the same concentration of particles in the
deposit. The hardness of the metal matrix was increased with the size of particles. Indeed the particles
of SiC Norton 10 000, SiC Norton 8000 and SiC Mattey
Johnson had an average size of 0.5 m, 0.75 m and 1
m, respectively. The hardness properties involved with
the Mattey Johnson particles were higher. This was due
to the crystallographic characteristics. Mattey Johnson
particles crystallize in the system whereas the Norton
particles crystallize in the system.
For nickel without particles, the value of hardness
525 Hv. is in agreement with those obtained by many
authors. Hubbell w10x, Ebdon w11x, and Honma w12x
found a hardness for the chemical nickel of 500 Hv,
Changgeng et al. w13x of 509 Hv, Tulsi w14x of 600 Hv,
Sale w15x of 500600 Hv and finally Hussain and Such
w16x of 480 Hv.
On the contrary, in the case of chemical NiSiC
deposits, different values have been reported 1300 Hv
w10x, 1090 Hv w17x, 650 Hv100 w13x, 900 Hv100 w12x, 724
Hv100 w18x and 700 Hv50 w16x. Therefore, comparison of

Fig. 2. Volume rate of SiC particles in electroless nickelSiC incorporating various types of SiC particles according to the concentration
of particles in the bath.

results was difficult. The hardness variations could be

explained according to size and structure of powder,
quantity of particles included in the deposits, load of
indentation and the thickness of the coatings tested.
3.2. Friction and wear
3.2.1. Friction coefficient
Deposits with two different thicknesses 3.5" 0.5 g
and 9.5" 1 g. had been tested Table 2..
The deposit of nickel alone has a friction coefficient
of 0.16, regardless of the thickness. While the addition
of SiC particles has led to a gradual increase in friction
due to the high hardness and abrasive properties of the
carbide particle.
3.2.2. Wear
Fig. 3 presents some two-dimensional and threedimensional profiles as well as the volume of matter
removed of the coatings.
It is clear that the wear resistance of nickel without
particles was comparable with those of NiSiC Norton
10 000. and NiSiC Mattey Johnson.. In contrast, the
deposit of SiC Norton 8000 had shown the lowest
resistance to wear. The volume of matter removed was
higher in this last case.

Table 2
Friction coefficients of nickel-SiC electroless deposits according to their thickness
Thickness of the
deposit m.

Deposit

Inclusion rate of particles

in the deposit %.

Friction
coefficient

3.5" 0.5

Nickel
Ni-SiC Norton 8000
Ni-SiC Norton 10 000
Ni-SiC Mattey Johnson

0
20
17
15

0.16
0.41
0.31
0.29

9.5" 1

Nickel
Ni-SiC Norton 8000
Ni-SiC Norton 10 000
Ni-SiC Mattey Johnson

0
10
9
7

0.16
0.35
0.28
0.25

A. Grosjean et al. r Surface and Coatings Technology 137 (2001) 9296

95

Fig. 3. Rugosimetric profiles two-dimensional and three-dimensional . and volume of matter removed for few electroless nickel samples. Deposit
without particles a. and composites deposit realized with different kinds and concentrations of SiC particles in the deposit for thicknesses of
3.5" 0.5 m b. and 9.5" 1 m c..

Fig. 4 represents optical microscope observations of

the wear scars on various chemical nickel deposits.
The scars on the deposits carried out with the particles of SiC Norton 8000 were more visible that those
on the deposits carried out with the other particles.
The wear scar of the deposits of SiC Norton 8000 was
so deep that the substrate brass. appears.

4. Conclusions
Nickel deposits incorporating various types and
amounts of SiC particles have been carried out. The
results show that hardness of nickel increases with

increasing the rate of incorporation of particles until a

maximal value. In addition it has been found that
hardness increases with increasing SiC particle size.
Regardless of the rate of inclusion of particles, the
friction coefficients of co-deposits were always higher
compared with that obtained for nickel deposits. The
SiC particles in general appeared to increase friction
due to their abrasive properties.
The profilometric and microscopic analysis of the
wear scars revealed that nickel incorporating SiC Norton 8000 particles average size 0.75 m. shows poor
wear resistance compared with deposits incorporating
SiC Norton 10 000 average size 0.5 m. or SiC Mattey
Johnson average size 1 m..

A. Grosjean et al. r Surface and Coatings Technology 137 (2001) 9296

96

Fig. 4. Photographs realized with an optical microscope of the wear

scars of the electroless nickel composite deposits realized with different particles of SiC. Thickness of the deposits between 3.5" 0.5
m a. and 9.5" 1 m b. with different concentrations of particles
in the deposit.

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