653

Fretting wear of SiAlON ceramic

M F Wani
Mechanical Engineering Department, National Institute of Technology Srinagar, Jeelan Lane, Srinagar 190 006, Kashmir,
India. email: mfwnfw2002@yahoo.com

The manuscript was received on 4 September 2006 and was accepted after revision for publication on 9 May 2007.
DOI: 10.1243/13506501JET233

Abstract: Friction and wear properties of Si6−Z Alz Oz N8−Z (z = 0.5) were studied in case of fretting.
SiAlON samples were prepared by hot pressing without any externally added liquid. The effect
of running time, slip amplitude, and normal load on friction and wear were investigated. A con-
stant coefficient of 0.45 was observed during running time; however, friction coefficient increased
from 0.445 to 0.475 for normal load variation of 20 N to 60 N. Wear increased linearly with the
increase in sliding time and normal load for both SiAlON and steel; however, it decreased with
the increase in slip amplitude. Higher wear was observed at low amplitudes as compared with
wear at higher amplitudes. Transition from higher wear to lower wear occurred at fretting ampli-
tude of 100–150 μm. Wear coefficient of 7.0 × 10−4 and 18 × 10−4 was observed for SiAlON and
steel, respectively. Micrographs proved useful for understanding wear mechanism. The wear in
SiAlON/steel tribopair was caused by a combination of third body abrasion, tribofilm formation,
and minor scoring.

Keywords: tribology, ceramics, SiAlON, fretting wear

1 INTRODUCTION evident that only a few studies have been carried

SiAlON is a solid solution of silicon nitride and alumina
having the general formula Si6−Z Alz Oz N8−Z . SiAlON is
known for its low density, high strength, superior ther-
mal shock resistance, high wear resistance, fracture
toughness, and chemical inertness. SiAlON is currently
used in various applications, such as cutting tools,
induction heating, resistance welding, metal forming
tools, diesel engine valves, valve guides, roller follow-
ers, tappet shims, seals, and hybrid bearings [1]. All
these examples show that SiAlON ceramic possesses a
high potential for more applications in tribo-elements.
In view of the increasing use of SiAlON ceramic for
various applications, it is essential to understand the
friction and wear behaviour of SiAlON under various
conditions of rubbing, i.e. unidirectional and recip-
rocating sliding, and fretting. Oscillating motion at
low amplitudes can cause a considerable amount
of wear. This form of surface damage is known as
‘fretting wear’. Therefore, it is essential to study fric-
tion and wear characteristics of SiAlON under fretting
conditions; however, from the literature survey it is
out to investigate the friction and wear behaviour of
SiAlON steel tribopair under fretting conditions [2–9].
In these research studies, the influence of test param-
eters, relative humidity, and temperature was studied
on friction and wear behaviour of nitride/oxide ceram-
ics. It was observed that coefficient of friction μ was
only mildly influenced by the operational variables,
whereas the coefficient of wear showed great vari-
ations and depended strongly on the humidity of
surrounding air. It is also revealed from these stud-
ies that fretting wear investigations were carried out
under high fretting amplitudes greater than or equal
to 200 μm [6–8]. It is well known that fretting often
occurs at low amplitudes, between vibrating parts of
machines or structures that are not moveable and as
such come across fretting even at slight movement.
Moreover, increase in slip amplitude > 150 μm results
in transition from fretting wear to macroscopic wear
[9]. In order to understand friction and wear behaviour
of SiAlON under fretting conditions, experimental
studies were carried out on SiAlON/steel tribopair at
low fretting amplitudes of less than 200 μm.

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654
2 EXPERIMENTAL
2.1 Materials
The samples of Si6−Z Alz Oz N8−Z (z = 0.5) were made
by hot pressing: (a) appropriate mixture of silicon
nitride powder containing 2.2 atom per cent oxygen,
(b) aluminum nitride, and (c) optical grade silicon
oxide. The excess silicon oxide used over the stoi-
chiometric composition was 1.5 per cent for SiAlON.
Hot pressing was carried out in boron nitride (BN)
coated graphite punch and die, under a pressure of
30 MPa at a temperature of 1700 ◦ C, until all shrink-
age ceased. No external sintering aid was used in this
process. Sintering was achieved by excessive silicon
oxide, which was attained by shifting the composi-
tion of SiAlON towards the silicon oxide corner of
the phase diagram [10]. The microstructure of SiAlON
samples shows elongated β- SiAlON grains. Scanning
electron microscopy (SEM) of etched SiAlON surface
showing microstructure details is given in reference
[11]. Moreover, SiAlON phase diagram details are also
provided in reference [11]. The exact value of z was
ascertained by X-ray diffraction. Composition of sili-
con nitride, aluminum nitride, and silicon oxide and
their source is shown in Table 1. The samples were
polished and finished with 4 and 2 μm diamond grit in
an automatic polisher and average surface roughness
value attained for SiAlON samples was 0.13 μm Ra. The
physical and mechanical properties of SiAlON were
measured using a microhardness tester, three-point
bending machine, digital balance, etc. The details of
measurement of the physical and mechanical prop-
erties are mentioned elsewhere [10–12]. The values
of physical and mechanical properties are: density =
3.2 × 103 kg m−3 , hardness = 1750 Hk , fracture tough-
ness K1c = 6.2 MPa.m1/2 , thermal conductivity = 24 W
m−1 K−1 , and elastic modulus = 365 GPa. A ball 10 mm
diameter of SAE 52100 steel (HRc 59-63) was used as
counter body tribomaterial.
2.2 Tribotesting
Initially, all the samples of SiAlON and steel were
cleaned and de-greased in an ultrasonic bath with
benzene for 20 min. Then the samples were dried in
Table 1 Composition of materials used for making of SiAlON ceramic
Silicon nitride
Material 86% α phase with a specific surface
composition area of 8.78 m2 g−1 . 0.538%
(wt.%) calcium, 0.01% magnesium,
0.084% sodium, 0.13% iron, 38.6%
nitrogen, 2.2% oxygen.
Source H. C. Starck, Goslar (Germany)
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M F Wani
an automatic oven at room temperature. The disc sam-
ples of SiAlON were weighed repeatedly on a balance,
accurate to 10 μg. The details of the balance are given
in references [10] and [11] After the test, the process
was repeated to measure the weight loss of the disc.
The wear scar diameter at the ball was measured on
a travelling microscope accurate to 0.1 mm. Wear vol-
ume (Wv ) of SiAlON was obtained from weight loss,
and wear volume of the steel ball was calculated using
the following equation [10, 11]

Wv = h2 (r − h/3), where

h = (d/2)2 /r + r 2 − (d/2)2
r is the radius of the ball, h is the wear scar depth, and
d is the wear scar diameter of the ball.
The specific wear rate ( Kw ) was determined by the
ratio of the volume lost (mm3 ) per unit, sliding dis-
tance (m) per unit, normal load (Fn ) and is given in
equation as
Kw = Wv /(Sd × Fn ) = mm3 /(m × N )
where Wv is the volume lost mm3 , Sd is the sliding
distance (m), and Fn is the laod applied (N ).
Friction and wear tests were carried out on an SRV
test rig using a ball on disc configuration under fret-
ting conditions. The details of the test rig are also given
in reference [10]. Fretting tests were conducted to
study the influence of running time (t), fretting ampli-
tude (x ), and normal load (Fn ) on friction and wear
behaviour of SiAlON ceramic. Operating parameters
adopted for fretting tests are as follows:
Fn = 20, 40, 50, and 60 N; running time = 4, 8, 12,
and 16 h; frequency f = 20 and 50 HZ; ambient room
temperature T = 50 ◦ C; and slip amplitude x = 50,
100, 150, and 200 μm. The friction tests were carried
out in ambient air (relative humidity of approximately
65–70 per cent) at a constant temperature of 50 ◦ C.
Morphology of worn ceramic surfaces as well as
SAE 52100 steel surfaces were studied using SEM and
optical microscopy. The transfer of material on sur-
faces of SiAlON and steel were examined with energy
dispersion spectroscopy (EDS).
Aluminum nitride Silicon oxide
65.0% aluminum, 99.9% pure with
32.5% nitrogen, 0.004% iron
0.05% carbon,
0.019% iron, 1.1%
oxygen
H. C. Starck, Goslar Hesal Minerals Ranchi
(Germany) (India)
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3 RESULTS AND DISCUSSIONS

Friction coefficient μ as a function of running time,

fretting amplitude, and normal load is shown in
Figs 1 to 3, respectively. As shown in Figs 1 and 3,
μ remains stable during running time and fretting
amplitude tests; however, μ increases from 0.445 to
0.475 with the increase in normal load as shown
in Fig. 2. During running time μ equal to 0.45 was
observed, as shown in Fig. 1. In the case of fretting
amplitude test, μ equal to 0.445, 0.47, and 0.475 was
observed under normal load of 20, 50, and 60 N as
shown in Fig. 3; a marginal decrease in μ from 0.47 Fig. 3 Friction coefficient (μ) as a function of fretting
to 0.465 is also observed under normal load of 40 N. amplitude
It is evident from these experimental studies that
friction coefficient μ remained stable during running
time and fretting amplitude tests of SiAlON/steel tri-
bopair. Predominant increase by μ = 0.445–0.475
was exhibited in μ within the increase in normal
load (20–60 N). The value μ 0.445–0.475 observed in
this research study conforms with the value of μ 0.46
observed in unidirectional sliding of SiAlON/steel cou-
ple by the researchers [8]. The value of μ observed in
this research study is lower than μ (0.55–0.6) reported
in references [10] and [13] for SiAlON/steel tribopair.

Fig. 4 Wear volume for SiAlON and steel as a function of

running time

However, the value of μ is higher than the value

reported in the literature for both unidirectional and
reciprocating sliding [12–14]. In the case of fretting
wear of silicon nitride/steel tribopair, the highest
value, μ 0.2–0.6, has also been reported in references
[5] and [7]. The coefficient of friction μ decreases pre-
dominantly under lubricating conditions, as reported
in references [12] and [13]. The lowest value, μ 0.05,
has been observed in these research studies. Higher
values of μ and increase of μ with the increase in nor-
Fig. 1 Friction coefficient (μ) as a function of running mal load fretting is due to the presence of continuing
time fracture and hard debris particle layer entrapped at the
point of contact. The value of μ did not change with the
variation of contact pressure from 2.8 G Pa to 2.8 MPa
for a normal load of 20 N.
Wear volume (mm3 ) as a function of running time of
SiAlON and counter surface steel ball is shown in Fig. 4.
Wear increases linearly, with the increase in running
time for both SiAlON and steel. Wear volume as a func-
tion of fretting amplitude under normal contact load
Fn = 40 N and Fn = 60 N is plotted (in Fig. 5), whereas,
wear volume as a function of normal load at fret-
ting amplitude x = 50, 100, and 150 μm is shown in
Fig. 6. Higher wear is observed at lower fretting ampli-
tude (x = 50 and 100 μm), as compared with wear
Fig. 2 Friction coefficient (μ) as a function of normal at higher fretting amplitudes (x = 150 μm) for both
load (N) SiAlON and steel. The specific wear rate of SiAlON and

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Fig. 5 Wear volume of SiAlON and steel as a function of
fretting amplitude
Fig. 6 Wear volume of SiAlON and steel as a function of
load
steel in fretting wear test is shown in Fig. 7. Wear rates
of 7.0 × 10−4 mm3 N−1 m−1 and 18 × 10−4 mm3 N−1 m−1
were observed for SiAlON and steel respectively, as
shown in Fig. 7.
It is evident, from the wear studies that wear
of SiAlON and steel increases with the increase
in running time under normal load whereas wear
decreases with the increase in fretting amplitude. In
case of SiAlON, severe wear was observed at low
fretting amplitude of 50 μm, whereas transition in
wear behaviour was observed after fretting ampli-
tude was increased beyond 100 μm. At lower fretting
Fig. 7 Wear rate of SiAlON and steel in fretting wear test
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M F Wani
amplitude and higher loads, wear of SiAlON was higher
as compared with wear of SiAlON at higher ampli-
tudes and higher loads, as shown in Figs 5 and 6.
It is also revealed from these fretting wear studies
that at lower fretting amplitudes, the wear particles
remain entrapped at the point of contact for longer
duration. For example, at lower fretting amplitude
(50 μm) wear debris was visible after fretting dura-
tion of 1 h, whereas at higher fretting amplitudes
(>150 μm) wear debris was visible only after 20 min.
Therefore, the presence of continuing fracture and
hard debris particle layer at the point of contact at
lower fretting amplitudes resulted in higher wear of
ceramics as compared with wear at higher amplitude
fretting. It is also observed that wear of fretting is influ-
enced by operational parameters such as normal load
and fretting amplitude. Specific wear rate of SiAlON
and steel increases with the increase in sliding dis-
tance and normal load; however, it decreases with
the increases in fretting amplitude. Specific wear rate
or 7.0 × 10−4 mm3 N−1 m−1 was observed for SiAlON
under normal load of 20 N and fretting amplitude
of 150 μm. Higher wear of SiAlON was observed
in this research study, as compared with wear of
SiAlON results reported in references [6] and [8] for
SiAlON/steel tribopair. In addition to this, wear of
SiAlON is also higher than the wear of silicon nitride
reported in reference [7]. It is important to note that
fretting wear is more severe than reciprocating slid-
ing and unidirectional sliding wear as reported in
references [8], [11], [12], and [14] to [16].
After testing, worn specimen surfaces of SiAlON and
steel were observed under SEM and optical micro-
scope. Typical micrographs of the surfaces are shown
in Figs 8 and 9. Figure 8(a) was obtained from the
surface of an SiAlON specimen after a fretting test of
15 h, and higher magnification view of this wear scar is
shown in Fig. 8(b). Highly magnified view of the wear
scar indicates the presence of dark and bright regions
on the SiAlON wear track. X-ray dot mapping of the
bright region of the worn surface is shown in Fig. 8(c).
The EDS spectrum of a spot in the bright region of
a worn SiAlON surface is shown in Fig. 8(e), whereas
in Fig. 8(f ) the EDS spectrum of SiAlON in the dark
region is shown. It is clear that metallic elements are
seen on the worn surface of SiAlON in the bright region
whereas no metallic element is present in the dark
region. Figure 8(d) shows the worn surface of steel after
a sliding distance test of 15 h. The EDS spectrum of a
spot in dark region of the steel ball is shown in Fig. 8(g).
It is clear from the EDS spectrum that silicon is present
on the surface of worn steel. Surface morphological
studies on SiAlON/steel tribopair under dry condi-
tions revealed that frictional and wear behaviour of
SiAlON ceramic/steel couples is a function of mutual
transfer of material and subsequent removal of these
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Fig. 8 SEM micrographs of the worn surfaces of SiAlON (a) an overview of wear track (b) Higher
magnification of wear track (×1200) (c) X-ray dot mapping showing distribution of ferrous
particles (×1200) (d) Wear scar on steel ball (e) EDS spectrum of a spot in bright region of
worn surface of SiAlON (f) EDS spectrum of a spot in dark region of worn surface of SiAlON
(g) EDS spectrum of a spot in dark region of steel ball

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658 M F Wani

Fig. 9 Optical micrographs of worn surfaces in fretting (a) Highest fretting amplitude
(x = 200 μm, Fn = 60 N, f = 50 Hz) (b) High fretting amplitude (x = 150 μm, Fn = 60 N,
f = 50 Hz) (c) low fretting amplitude (x = 100 μm, Fn = 60 N, f = 50 Hz) (d) lowest fretting
amplitude (x = 50 μm, Fn = 60 N, f = 50 Hz)

adhered fragments [8, 10–12]. In these research stud-
ies, it was also revealed that dominant wear mecha-
nism in SiAlON/steel tribopair is adhesion and micro
abrasion.
Optical micrographs obtained on worn surfaces of
SiAlON after fretting wear tests are shown (in Fig. 9).
Figures 9(a) and (b) were obtained on the surface of
SiAlON after high fretting amplitude tests (>100 μm),
whereas Figs 9(c) and (d) were obtained after low fret-
ting amplitude tests. It is evident from these figures
that at high fretting amplitude (200 and 150 μm) minor
scoring marks are observed on the surface of harder
SiAlON material, and the worn surface of SiAlON is
covered with adhered fragments of the tribolayer as
shown in Figs 9(a) and (b). At low fretting amplitudes
(50 and 100 μm) severe scoring marks were observed
on the surface of SiAlON and the wear track was rough,
covered with adhered fragments of tribolayer. The sur-
face morphological and optical microscopy studies
conform with the results of research studies reported
in references [8] and [10] to [12].
From these observations it is seen that the friction
coefficient (μ) in SiAlON/steel tribopair depends upon
contact load and is independent of sliding time and
slip amplitude. It increases with an increase in normal
load. However, μ is not influenced either by mutual
transfer of material or by the formation tribofilm at
the point of contact in dry rubbing. Similar friction
behaviour was observed for SiAlON/steel tribopair
in unidirectional sliding, as is reported in reference
[8]. It is also known from research studies that the
coefficient of friction is predominantly decreased for
SiAlON/steel tribopair with lubrication in references
[12] and [13].
From these observations it is also seen that fret-
ting wear in SiAlON/steel tribopair is caused by a
combination of wear mechanisms, which includes
third body abrasion, tribofilm formation, and minor
scoring leading to the conclusion that adhesion and
micro abrasion is the dominant wear mechanism in
SiAlON/steel couple. The wear debris emanating from
the contact zone appears to be ferrous oxide, given
to its brown colour. These wear particles are likely
to be a combination of SiAlON and steel material.
The wear debris that remains in the wear track is
subjected to continued chemical reaction. The debris
remaining in the contact area constitutes a third
body in the fretting, particularly at very low ampli-
tudes, which generate scoring marks on the surface
of SiAlON.
4 CONCLUSIONS
The fretting tests on SiAlON/steel tribopair were con-
ducted to assess friction and wear behaviour of SiAlON
ceramic. The effect of various parameters on friction
and wear of SiAlON/steel tribopair were studied in
fretting. The friction coefficient is found independent
of running time and fretting amplitude. However, the
friction coefficient depends on normal contact load.
The friction coefficient is not influenced by the forma-
tion of tribofilm at the point of contact. The fretting

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 Fretting wear of SiAlON ceramic
wear is highly influenced by fretting amplitude, fret-
ting load, and by the formation of tribofilm (third
body) at the point of contact. It is caused by the com-
bination of third body abrasion, tribofilm formation,
and minor scoring. Fretting wear is more severe at
lower fretting amplitudes. Further studies on SiAlON
and steel tribopair are required to be carried out to
substantiate the result of tribofilm formation and also
to understand fully the wear mechanism observed in
this research study.
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