Defence Science Journal, Vol. 58, No. 4, July 2008 pp.

582-587
Ó 2008, DESIDOC

SHORT COMMUNICATION

Effects of Temperature on Tribological Properties of Al2O3-TiO2 Coating

V.V. Narulkar1, S. Prakash2, and K. Chandra2

1
Institute of Technology and Management, Gurgaon
2
Indian Institute of Technology, Roorkee-247 667

ABSTRACT

The Al2O3-TiO2 coating for turbine blades is being used since long. During the last decades,
a large number of papers have been published, but work on property assessment of Al2O3-TiO2
coating on rotating component from tribological point of view is very less. This paper assesses
the wear behaviour of Al2O3-TiO2 coating on inconel 601. The Al2O3-TiO2 coating on inconel 601
is deposited by plasma spray process. The SEM results show that above 300 oC, the friction
coefficient decreases due to softening of coating material. The wear rate increases with increase
in temperature. The coating showed brittle fracture at higher temperature. Other test results have
shown the drastic changes in property due to load and temperature.

Keywords: Material processing, plasma spraying, microstructures

1 . INTRODUCTION temperatures. Therefore, an interest has been shown

by the researchers in the wear of plasma sprayed
The ceramics in coatings form for applications
ceramic coatings at elevated temperatures.
involving corrosion, wear, and high temperature
are widely used due to their many inherent In the present study, the tribological behaviour
properties 1-3. The plasma spraying is an established of alumina-3 Wt per cent TiO2 coating deposited
technique to produce thick ceramic coatings. Alumina- by plasma spraying was investigated by sliding
based coatings deposited by plasma spraying are against a silicon nitride ball under unlubricated
widely used for a range of industrial applications conditions at temperatures ranging from room
due to their important mechanical properties and temperature to 600 °C. The wear mechanisms
low production costs 4-6. were discussed in terms of the observations and
analyses of the wear surfaces and the debris particles.
The tribological behaviour of ceramics is also
greatly influenced by test conditions, such as, contact
2 . EXPERIMENTAL
load, environment, and temperature7-13. The presence
of adsorbed moisture and the formation of oxide Alumina-3 Wt per cent titania coating was
films can decrease the wear of ceramics 13 . The prepared by atmosphere plasma spraying (A-2000,
wear rate of alumina-based ceramics increases Sulzer Metco AG, Switzerland). The material used
with the temperature, increasing 12 up to 600 oC. was the conventional fused and crushed powder
Tetsuya7, et al. found grain size also has an important of 10-35 mm 14. The coatings were deposited onto
effect on the wear resistance of alumina at elevated stainless steel substrates (F 25 mm x 8 mm),
Received 14 May 2007, revised 03 October 2007
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which were cleaned with acetone and grit blasted 3 . RESULTS

before plasma spraying. The coating thickness was
about 480 µm. The above experiments were described 3.1 Friction and Wear
by Lin 15, et al. From Fig. 2, it can be seen that the friction
Tribological properties of the as-sprayed coatings coefficients of conventional Al 2O 3-3 Wt per cent
against a 3 mm Si 3N4 ball were examined using a TiO2 coating ranged from 0.8 to 1.0 for the whole
pin-on-disc machine. The schematic drawing of temperature range.
the test rig is shown in Fig. 1. On the ball bearing
It is clear from Fig. 2 that the friction coefficient
a normal load was fixed and the disk sample was
decreases as the temperature increases. It is found
rotated at 199 rpm (0.1 m/s). Applied load was 5 N
and the sliding distance was 60 m. Wear tests were 0.92

FRICTION COEFFICIENT
carried out in the unlubricated condition and at 0.9
temperatures ranging from room temperature, i.e., 0.88
0.86
0.84
0.82
0.8
30 100 400 600
TEMPERATURE (° C)

Figure 2. Effect of temperature on friction coefficient of the

coating.

that from room temperature to 100 oC, friction

coefficient was more or less constant but after
that, graph showed a sliding trend. Figure 3 shows
the effect of temperature on the wear rates of the
Figure 1. Experimental setup of pin-on-disc machine at IIT as-sprayed coatings.
Roorkee.

about 27 oC to 600 oC. The disc sample was mounted At room temperature, the wear rate of coatings
on a stainless steel holder and was heated to the was too small to be measured accurately, and gradually
required temperature. The relative humidity varied it increased with increase in temperature.
from 40 per cent to 60 per cent. Prior to the test, 6
WEAR RATE (x 10-5mm3N-1m-1)

the as-sprayed coatings were polished to a roughness 5

of 0.08–0.15 µm. The friction coefficient was continuously 4
recorded during the tests. Surface profiles of the 3
wear tracks on the disks were measured by a surface 2
profilometer. The wear volume of the disk specimen 1
was determined from the average cross-sectional 0
area of the wear track obtained from three points 30 100 400 600
measured perpendicular to the sliding direction. The TEMPERATURE (° C)

presented friction coefficients and wear rates were Figure 3. Effect of temperature on wear rate of the coating
the average of the three specimens. The microstructure material (x 10-5 mm3 N-1 m-1).
of as-sprayed coatings was investigated by field
3.2 SEM of Worn Surface and Wear Debris
emission scanning electron microscope (JSM-5800,
JEOL, Japan). The worn surface and wear debris Figure 4 shows the micrographs of the worn
were examined by a SEM (EPMA-8705QH2, Shimadzu, surfaces of a conventional Al 2O 3 -3 Wt percent
Japan) equipped with an EDAX attachment (Oxford TiO2 coatings sliding against a silicon nitride ball
Instruments, Model 6841, UK). at room temperature. The worn surfaces of coatings

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(a) (b)
Figure 4. SEM micrographs of worn surface of Al2O3-3 Wt Figure 5. SEM micrographs of worn surface of Al 2O3-3 Wt
per cent TiO2 coating surface at room tempreture. per cent TiO 2 coating surface at: (a) 100 0C, and
(b) 400 0C.
were covered with a discontinuous compact layer. 4 . DISCUSSIONS
The EDS analysis revealed that the compact layer
Tribochemical reaction of Al 2O 3-3 wt per cent
contained large amounts of silicon but no nitrogen,
TiO2 coating is considered to be an important factor
suggesting that silicon nitride was oxidised and
that influences the wear of ceramic materials 13,18 .
transferred to the worn surface of the coatings 7,18.
At room temperature, the worn surfaces of the
There were many cracks existing on the worn
conventional Al 2O 3 -3 Wt per cent TiO 2 coating
surface of the coatings and the compact layer was
were covered with a compact layer consisting of
in the process of delamination as flake-like debris,
silicon oxide for the tests performed in an atmosphere
due to the effect of the cyclic stress. In some
with a humidity level of 40-50 per cent. Compared
places, the delamination occurred in coatings, and
with alumina, silicon oxide is softer 17 . This softer
large craters were found. It was thought that the
layer was effective in distributing contact stress,
cracks would propagate along areas of weakness
and the shear and slipping in the soft layer could
in the underlying material under cyclic stress due
act to accommodate the velocity mismatch between
to the strong adhesion between the transferred
the two wear surfaces. Thus, the presence of the
surface layer and the underlying material, i.e., a
softer layer on the worn surface prevented the
fatigue process was involved 19 . Since the inter-
coating from undergoing brittle fracture.
splat bonding is weak in the plasma-sprayed ceramic
coating 20,21, the delamination was along the splat Consequently, the coating wear at room temperature
boundary, and accordingly, a large crater was produced. was very less but, fatigue delamination occurred
It was inferred that the wear rate of the coating along the splat boundaries in coatings under the
would increase if the sliding distance was increased. cyclic stress due to the strong adhesion between
the transferred layer and the coating. As for silicon
It can be seen that the morphology of the worn
nitride, the humidity in the atmosphere affects the
surface of the coating is strongly dependent on the
formation of oxides. The activation energies of
testing temperature. From Fig. 5, it can be seen that
reactivity of silicon nitride with wet oxygen and
at 100 oC and 400 o C, smooth areas were absent
dry oxygen are 488 ±30 kJ-mol-1 and 375 ±25 kJ-mol-1,
in the coating and the worn surface was covered
respectively, and the oxidation rate of Si 3 N4 is
with a layer of fine wear debris particles [Figs 5(a)
much more accelerated in the presence of water
and 5(b)]. At 100 o C, most of the wear debris
vapours 22 .
particles were < 1 µm and were globular, whilst
their size was up to several µm at 400 oC and their Another effect of humidity is to increase the
morphology was angular. It was found that the adhesion between the wear debris particles and
composition of the wear debris at 100 oC was similar the worn surface/wear debris particles 23-25 , which
to that at 400 oC and it was mainly alumina. is beneficial to compact the particles to form a

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dense layer. The adsorption tendency of water is such as porosity and grain size. A high hardness,
reduced as the temperature is increased. As a low porosity, and small grain size are desirable to
result, the worn surfaces of conventional Al2O3-3 Wt improve the wear resistance of polycrystalline
per cent TiO2 coating were not covered with the ceramics 5,29,30 . On the worn surfaces of the coating,
compact layer at 100 o C and the friction stress the existence of pits indicate that brittle fracture
could not be distributed. Brittle fracture occurred mostly occurs along the grain boundary, which is
on the worn surface of the coating, and alumina directly related to the strength of grain boundaries 8.
wear debris particles were produced. However, The strength of grain boundaries is weakened by
adsorbed water on the surface cannot be completely the residual stresses from the thermal expansion/
removed 26 100 o C. Therefore, the wear debris still elastic anisotropy. According to the Hall-Petch
remained a part of its adhesive capability and was relationship, the stresses increase with the grain
trapped on the wear track. size, resulting in higher stress in the grain
boundaries of coarser grain size materials and an
During the subsequent sliding, the wear debris increasing tendency for intercrystalline fracture 29 .
that remained on the wear track was subjected to Below 700 oC, the increase in the wear rate of
continuous fracture and was composed of fine particles. alumina with grain size was interpreted in term of
For temperatures up to 400 oC, the adhesion capability decrease in strength of grain boundaries with grain
of the wear debris further decreased. Under the size 8.
effect of centrifugal force, the wear debris particles
could be swept away from the contact zone after
5 . CONCLUSIONS
these were produced, and further fracture of the
wear debris could not happen. Thus, wear debris I n t h i s s t u d y, w e a r t e s t s a t e l e v a t e d
consisted of coarse particles at 400 o C. temperatures have been conducted for both
conventional Al 2O 3-3 Wt per cent TiO2 coatings.
It is generally assumed that the presence of The wear rates of coating sliding against a silicon
wear debris in the contact zone increases wear. But, nitride ball increased with an increase of temperature
this is far from truth in dry friction, especially for in the range room temperature to 600 oC. At room
ceramic materials27,28. Fretting experiments have clearly temperature, the wear of coating was too low to
shown that wear debris decreases the wear of materials 27. be measure of using the test condition because a
Compared with ceramic materials, wear debris is layer consisting of oxidation products of silicon
looser and can also respond kinematically to the velocity nitride appeared on the worn surface of both the
mismatch, and accordingly, causes less damage than coatings. When the temperature was increased up
that occasioned by locked asperities of the mated to 100 o C, brittle fracture occurred on the worn
material with identical hardness28 . In this study, the surface of the coating, which was enhanced with
hardness of the Si3N4 ball was about 1600 HV 0.2 , the increase in temperature due to the desorption
which is much higher than that of the coating (830 of the moisture on the worn surface.
HV 0.2 ). Thus, the wear of the coatings from the
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