Wear 268 (2010) 12661274

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High temperature wear behavior of Al4CuTiB
2
in situ composites
S. Kumar, V. Subramanya Sarma, B.S. Murty

Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai 600 036, Tamil Nadu, India
a r t i c l e i n f o
Article history:
Received 9 June 2009
Received in revised form 7 January 2010
Accepted 13 January 2010
Available online 25 January 2010
Keywords:
Sliding wear
Thermal effects
Metal matrix composites
High temperature
a b s t r a c t
The effect of sliding temperature and load on the wear behavior of Al4Cu alloy and Al4CuTiB
2
in situ
composites was studied in this paper. The wear resistance of the Al4Cu alloy increased with increase in
wt.% of reinforcement TiB
2
particles at all temperatures and loads. The transition in the wear mode from
mild to severe wear was strongly inuenced by the addition of TiB
2
particles. The Al4Cu alloy showed
a transition from mild to severe wear at a load of 80N and at a sliding temperature of 100

C. But with
the addition of 5 and 10wt.% of in situ TiB
2
particles to the Al4Cu matrix, the transition temperatures
are increased to 200 and 300

C and the loads are increased to 100 and 120N, respectively. Analysis of
wear surfaces by scanning electron microscopy revealed the transition in wear mode. It was observed
that at elevated temperature the predominant wear mechanisms for the Al4Cu alloys are adhesion and
metal ow, whereas for Al4CuTiB
2
composites oxidation, delamination and metal ow are the most
dominant wear mechanisms.
2010 Elsevier B.V. All rights reserved.
1. Introduction
Aluminium based metal matrix composites (MMCs) has poten-
tial applications in automobile and aerospace industries, where the
components are subjected to severe surface degradation. Al based
MMCs are well knownfor their superior tribological behavior when
compared to the base alloy [1]. In recent studies, it was shown that
Al based in situ MMCs (reinforcement phases synthesis during cast-
ing) have better properties and performance when compared to ex
situ MMCs [2,3]. The superior behavior of these in situ composites
is due to good matrixreinforcement interface and smaller rein-
forcement size (<2m). It had been shown that with the addition
of in situ TiB
2
particles, it is possible to accelerate the aging kinetics,
which further subsequently increases the hardness and strength of
the Al4Cu alloy [4,5]. It was also found that when these in situ
composites were subjected to rolling (both at room and cryogenic
temperature), the aging kinetics were further accelerated resulting
in an increase in peak hardness and wear resistance [6]. It was also
noted that with the addition of TiB
2
in situ particles to the Al alloys,
the dry sliding wear, abrasive wear and erosive wear increased
signicantly [59]. Recent studies on high temperature wear have
shownthat withtheadditionof TiB
2
particles totheAl7Si alloy, the
transition of wear mode frommild to severe wear was increased to
higher the loads and temperatures [9]. The high temperature wear
resistance of these in situ MMCs are much superior to base Al7Si
alloys in all sliding conditions. Since it was found that the addition

Corresponding author. Tel.: +91 44 22574754; fax: +91 44 22570509.

E-mail address: murty@iitm.ac.in (B.S. Murty).
of TiB
2
particle to Al4Cu alloy signicantly accelerates the aging
kinetics and increases the strength, it may be worth while to study
both the ambient and elevated temperature wear behavior of these
age hardenable AlCu alloy based in situ composites.
There were few studies on high temperature wear behavior of
age hardenable MMCs, and these studies are focused on ex situ
MMCs. Martn et al. [10] noted that heat treatment did not mod-
ify the high temperature wear resistance of either the composites
(AA261815vol.% SiC) or unreinforced alloy (AA2618). Muratoglu
and Aksoy [11] also found similar results in their studies on the
effect of heat treatment on the high temperature wear behavior of
theAl4CualloyandAl4CuSiCcomposites. Therewerenoreports
on the high temperature wear studies on age harden in situ com-
posites. The paper reports the studies on high temperature wear
behavior of Al4Cu alloy reinforced with different wt.% of in situ
formed TiB
2
particles. This paper also clearly highlights the effect
of addition of TiB
2
particles on the transition in the wear mode.
2. Experimental details
Al4Cu (Al4wt.%Cu) binary alloy was cast by diluting Al33Cu
(Al33wt.%Cu) master alloy with commercial pure Al in a pit type
resistance furnace. The in situ Al4CuTiB
2
composite with 5 and
10wt.%of TiB
2
particles were preparedby mixedsalt reactionroute
in which K
2
TiF
6
and KBF
4
salts were added in proper Ti:B ratio
to the diluted liquid metal at 800

C and stirred for 1h at regu-

lar intervals and cast in a permanent mould. The cast Al4Cu alloy
and the composites were solutionised at 540

C for 2h followed by
water quenching, and subsequent aging were carried out at 170

C
for different times to get peak hardness. Further details about the
0043-1648/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.wear.2010.01.022
S. Kumar et al. / Wear 268 (2010) 12661274 1267
synthesis and heat treatment of these composites can be found
elsewhere [57].
The high temperature dry sliding wear tests were carried out
on a high temperature pin-on-disc wear testing machine (TR-
2HT-M3, DUCOM, Bangalore, India). The pin (8mm in diameter
and 12mm in height) slides against steel (ball bearing steel) disc.
The wear tests were carried on the peak aged alloy and compos-
ites. The sliding velocity and sliding distance were kept constant
in all the experiments at 1ms
1
and 1km, respectively. The
applied load was varied from 40 to 120N and the temperature
was varied from room temperature (RT) to 300

C. The pin and

disc were heated uniformly and after the temperature is stabi-
lized the wear test was started. Further experiment details can be
found from an earlier report by the authors [9]. The wear tests
were carried out in ambient atmosphere with the humidity of
about 80% and a new disc was used for each experiment. The pin
and disc were polished and cleaned to get uniform average sur-
face roughness (Ra) of about 0.410.62m which was measured
using Perthometer (M2 Mahr GMBH, Germany). The wear rate is
dened as volume loss divided by sliding distance, and the vol-
ume loss is obtained from the ratio of weight loss to the density
of the sample. The coefcient of friction was measured continu-
ously using computer aided integration system. The worn surface
of the pin and disc were analysed using optical microscopy and
FEI Quanta 200 scanning electron microscope (SEM) with EDAX
energy dispersive spectroscopy (EDS). The subsurface of wear scar
Fig. 1. Effect of load on the wear rate of Al4Cu alloy and composites at different temperature (a) RT, (b) 100

C, (c) 150

C, (d) 200

C and (e) 300

C.
1268 S. Kumar et al. / Wear 268 (2010) 12661274
is analysed by cross-sectioning the worn surface along the sliding
direction,
3. Results and discussion
Fig. 1(ae) shows the sliding wear behavior of Al4Cu alloy and
Al4CuTiB
2
composites at different loads and temperatures. The
wear resistance of Al4CuTiB
2
in situ composites is found to be
superior to that of Al4Cu alloy under all sliding conditions. The
wear resistance of Al4Cu alloy increased with the addition of
TiB
2
particles and at room temperature, the wear rate of Al4Cu
alloy is reduced by 60-65% with the addition of 10wt.% of TiB
2
particles. This can be attributed to the increase in hardness due
to the change in microstructure (grain size, reinforcement and
precipitation) of Al4Cu alloy with the addition of in situ TiB
2
par-
ticles. The peak aged hardness of Al4Cu alloy, Al4Cu5TiB
2
and
Al4Cu10TiB
2
are 88, 112 and 136 HV5, respectively. It was found
that the addition of in situ TiB
2
particles to Al4Cu alloy signi-
cantly increases the aging kinetics of base alloy and the increase
in properties of these Al4CuTiB
2
composites can be attributed to
grain boundary strengthening, particulate strengthening and pre-
cipitation strengthening [4,5,7]. Similar improvement in the aging
kinetics and wear resistance was observed in the composites when
subjectedtorollingandsubsequent heat treatment [6]. Ontheother
hand, Tee et al. [12] did not observe improvement even after the
incorporationof 15vol.%of insituTiB
2
particles. This was attributed
to the presence of TiAl
3
intermetallic phase. Wu et al. [13] reported
that the presence of TiAl
3
is detrimental to the wear resistance of Al
matrix alloy and showed that the wear resistance of AlTiB
2
in situ
composites improved with decrease in TiAl
3
phase fraction. This is
because the large TiAl
3
blocky particles during sliding were sub-
jected to fracture and resulted in a particle pull out. The increase
in wear resistance observed in the present study is attributed to
the absence of TiAl
3
phase. The presence of only TiB
2
is conrmed
by XRD analysis on the extracted in situ formed particles by dis-
solving the Al4Cu matrix from the composite and this result is
reported elsewhere [5]. During wear of composites, the interaction
between the matrix and counterface will be controlled by the rein-
forcement. The interaction here refers to the adhesion phenomena
that exist between the asperities of soft matrix and hard counter-
face. Under load, the contact asperities of soft (pin) and hard (disc)
surfaces undergo deformation which results in cold welding and is
termed as adhesion. When these surfaces are subjected to sliding,
these cold welded asperities get detached and results in metal loss
and such loss of metal is termed as adhesive wear. With increas-
ing reinforcement phase, the amount of soft matrix asperities that
are in contact with hard counterface reduces and this contributes
to the increased wear resistance. In the present case the interac-
tion between steel and -Al asperities is reduced with increasing
the amount of TiB
2
particles. This can be explained based on the
microstructure [5], i.e., the area fraction of the soft -Al decreases
with increase in the amount of TiB
2
particles, thereby resulting in
the higher wear resistance of the in situ composites.
In addition to the amount of the TiB
2
particles, the wear rate is
also dependent onthe appliedload. Fig. 1(ae) also shows the effect
of applied load on the wear behavior of Al4Cu alloy with differ-
ent amounts of the reinforcement and temperatures. The wear rate
increases with increasing load at all temperatures. This is due to
increase in the deformation of the matrix with increase in applied
load. However, the extent of deformation due to applied load is
reduced with increase in the TiB
2
content. Similarly, the wear rate
is muchlower for the composites at all temperatures incomparison
to the base alloy. This improvement is attributed to the improved
strength/hardness of the composites due to grain renement, pre-
cipitationstrengthening anddispersionstrengthening. Prasada Rao
Fig. 2. Normalized wear rate as a function of TiB
2
amount at different temperatures
and at 40N load.
et al. [14] clearlydemonstratedtheimprovement inwear resistance
and load bearing capacity with grain renement. As mentioned
above, the severity of the wear damage increases with increase in
temperature (Fig. 1). In severe wear, bulk of the metal gets trans-
ferred fromthe pin to the steel counterface during sliding, whereas
in mild wear regime, the pin gets oxidized and delaminated to form
mechanically mixed layer (MML) and sliding occurs without any
bulkmetal transfer. At thetestingtemperatureof 100

C, theAl4Cu
alloy shows severe mode of wear at 80N and further increase in
slidingtemperatureto150

C(Fig. 1(c)) and200

C(Fig. 1(d)) lowers

the mild to severe wear transition load to 60 and 40N, respec-
tively. The temperature at which mild to severe wear transition
occurred shifted to higher temperatures with increasing amount
of TiB
2
particles. The transition behavior of alloy and composites is
strongly dependent on applied load and sliding temperature. Singh
and Alpas [15] also reported similar type of transition behavior in
6061 AlAl
2
O
3
composites.
To study the effect of TiB
2
particles on the wear behavior of
Al4Cu alloy the normalized wear rate (ratio of the wear rate of
composites to the wear rate of matrix alloy) was evaluated (Fig. 2).
With increase in TiB
2
content, the normalized wear rate decreased
at all temperatures usedinthe present study. It is alsointeresting to
note that the normalized wear rate decreased withincrease intem-
perature for a given amount of TiB
2
. This clearly explains that the
TiB
2
particles in the Al4Cu alloy are more effective in resisting the
wear at high temperature in comparison to the roomtemperature.
This can be attributed to the improvement in thermal stability of
Al4Cualloywiththeadditionof TiB
2
particles. It is well established
that the coefcient of thermal expansion (CTE) of Al is reduced by
the addition of hard ceramic phase [1619]. The CTEs for Al4Cu
alloy and TiB
2
are 26.910
6
and 4.610
6
C
1
, respectively,
and from rule of mixtures, the calculated CTEs for Al4Cu5TiB
2
Al4Cu10TiB
2
composites are 26.110
6
and 25.310
6
C
1
,
respectively, and these are smaller than the matrix alloy. Therefore
inthepresent case, thedimensional stabilityof matrixAl4Cualloy,
which has high CTE, is improved due to the presence of stable in
situ reinforcement, TiB
2
. With increase in sliding temperature, the
matrix alloy is softened resulting in transfer of metal to the steel
counterface, but with the addition of TiB
2
particles, the softening
tendency of the matrix alloy is reduced resulting in increased wear
resistance. It is also interesting to note that the wear resistance of
the composites is retained even after exposure to a temperature
of 300

C (which is much higher than the peak aging temperature

of 170

C), whereas the peak aged Al4Cu alloy undergoes severe

wear at 100

Cat anappliedloadof 80N. It canbeconcludedthat the

S. Kumar et al. / Wear 268 (2010) 12661274 1269
Fig. 3. Average coefcient of friction () of Al4Cu and composites as the function of load at different temperatures (a) RT, (b) 100

C, (c) 150

C, (d) 200

C and (e) 300

C.
presence of hard ceramic particles (TiB
2
) in Al4Cu matrix resists
metal ow at higher temperature and results in improved wear
resistance at high temperatures. Huang et al. [20] clearly demon-
strated the presence of TiB
2
in situ particles improves the creep
resistance of the matrix Al alloy.
The effects of load and temperature on the average coefcient of
friction () of Al4Cu alloy and composites were plotted in Fig. 3.
The coefcient of friction () of the Al4Cu alloy and composites
increased with increase in load and temperature. In all the cases, in
situ composites showed lower values when compared to matrix
alloy. Similar behavior was also observed in Al7Si alloy based in
situ composites [8,9]. This clearly shows that the formationof ultra-
ne in situ particles lowers the coefcient of friction of Al4Cu
alloy matrix andthis is attributedtothe goodparticlematrix inter-
face, improved dispersion and smaller particle size [21]. Min et al.
[22] compared the of AlTiB
2
composites with AlSiC compos-
ites and found that AlTiB
2
composites showed lower coefcient
of friction (0.160.17) when compared to AlSiC composites
(0.70). It was observed that of Al4Cu alloy increases with
increase in temperature due to the severe transfer of metal to the
counterface. However, Al4Cu composites show a drop in with
increase intemperature up to 200

C. This drop in for the Al4Cu

composites can be attributed to the improved thermal stability of
composites (due to the presence of TiB
2
particles) and formation of
iron oxide layer between the mating surfaces.
Fig. 4 shows the wear surface of Al4Cu alloy at 40Nload tested
at room temperature. The wear surface shows (Fig. 4(a)) distinct
parallel grooves throughout the worn surface. These grooves were
formed due to the ploughing tendency of steel asperities. The
aggressiveness of the ploughing increased with increase in the
applied load. The wear surface of the Al4Cu alloy did not show
grooves, when the sliding temperature was increased to 100

C
(Fig. 4(b)). Grooves are formed over the soft material (Al4Cu
alloy) by the ploughing of sliding hard asperities (steel disc).
During ploughing, the metal from the grooves are displaced by the
sliding asperities along the side of the grooves, but at high sliding
1270 S. Kumar et al. / Wear 268 (2010) 12661274
Fig. 4. Wear surface of Al4Cu alloy after sliding at (a) RT and (b) 100

C with the load of 40N. The arrow mark shows the sliding direction.
temperature, the displaced soft metal has the tendency to ow
back. This result in the worn surface to have shallowgrooves when
compared to the sample subjected to wear at room temperature.
Therefore, the wear scars of the Al4Cu alloy worn at 100

C do
not show steep grooves. When the temperature is increased to
200

C, there is a bulk transfer of metal from the Al4Cu alloy to

the steel surface. This process of bulk metal transfer is termed as
severe mode of wear and is the reason for the observed increase in
the . Fig. 5(a) clearly shows the metal owon the worn surface of
Al4Cu alloy and Fig. 5(c) shows the deposition of Al4Cu alloy on
Fig. 5. (a) SEMmicrograph, (b) EDS analysis on the worn surface of Al4Cu alloy, (c) SEMmicrograph and (d) EDS analysis of steel disc at temperature of 200

C with the load

of 40N.
S. Kumar et al. / Wear 268 (2010) 12661274 1271
Fig. 6. Longitudinal cross-section (parallel to the sliding direction) of the wear scar of Al4Cu alloy tested at 200

C (a) low and (b) high magnication.

Fig. 7. Wear surface on Al4Cu10TiB
2
in situ composite after sliding at (a) RT and (b) 200

C with the load of 40N and (c) EDS analysis on 200

C sample.
1272 S. Kumar et al. / Wear 268 (2010) 12661274
the counterface. The EDS analysis on the worn surface of Al4Cu
alloy (Fig. 5(b)) does not show Fe, further conrming the absence
of mechanical mixed layer. Elemental analysis on steel surface
(Fig. 5(d)) shows the presence of Al and Cu without any Fe peak,
which indicates that Al alloy is coated as a thick layer on the wear
track of the steel surface. Further, the cross-section of worn surface
(Fig. 6(a)) shows that Al4Cu alloy has undergone extrusion at
elevated temperature and the high magnication image (Fig. 6(b))
shows no macroscopic evidence for mechanically mixed layer. This
is consistent with SEM (Fig. 5(a)) and EDS (Fig. 5(b)) analysis on
wear scars of worn surface. This conforms that, due to instability of
the alloy at high temperature, the bulk of metal starts to owalong
Fig. 8. (a and b) SEM micrographs and (c) EDS analysis on the worn surface of Al4Cu10TiB
2
composites at 200

C with 120N.
Fig. 9. (a) SEM micrograph and (b) EDS analysis on the worn surface of steel counterface with Al4Cu10TiB
2
composites at 200

C with 120N.
S. Kumar et al. / Wear 268 (2010) 12661274 1273
the sliding direction, as a result (a) part of the metal adheres to the
steel counterface and (b) part of the metal is extruded to the rear
end of the sliding surface (pin). Further, due to repeated sliding of
the pin on the same wear track of steel counterface, the adhered
matrix alloy on steel counterface starts to pile-up on the front of
sliding surface (Fig. 6(a)). From the analysis of wear surface it can
be concluded that at roomtemperature, the observed wear mecha-
nismof Al4Cu alloy is abrasion whereas at higher temperature the
predominant wear mechanismis adhesion followed by metal ow.
The wear surface of Al4Cu10TiB
2
insitucomposites are shown
in Fig. 7. At room temperature and at load of 40N, the wear sur-
face of Al4Cu10TiB
2
composite shows shallow grooves running
parallel to the sliding direction (Fig. 7(a)). The wear surface of the
Al4Cu10TiB
2
composites after sliding at anelevatedtemperature
of 200

C still shows the grooves (Fig. 7(b)), which is in contrast to

that observed in Al4Cu alloy (Fig. 5(a)). This is attributed to the
dimensional stability of matrix due to the presence of TiB
2
parti-
cles. Further, the EDS analysis (Fig. 7(c)) on the worn surface shows
Fig. 10. Longitudinal cross-section (parallel to the sliding direction) of the wear scar of Al4Cu10TiB
2
in situ composites tested at 200

C with 120N: (a) low, (b) high

magnication and (c) trace diagram from (b) to show various regions below the worn surface.
Fig. 11. (a) SEM micrograph and (b) EDS analysis on the worn surface of Al4Cu10TiB
2
in situ composites at 300

C with 100N.
1274 S. Kumar et al. / Wear 268 (2010) 12661274
the evidence of Fe and O. When the load and temperature of the
testing were increased to 120N and 200

C, respectively, the worn

surface in the composite clearly shows delamination (Fig. 8(a)). A
higher magnication view of the delaminated region shows the
presence of small particles (Fig. 8(b)) and EDS analysis (Fig. 8(c))
conrms the presence of Fe and O
2
. The presence of iron oxide
particles on the worn surface resembles the delamination of MML,
which is formed during continuous sliding of the pin over the steel
disc in which the mating surfaces were exposed to the elevated
temperature and high load. The worn surface on the steel coun-
terface (Fig. 9(a)) also shows the presence of Fe, Ti, Cu, Al and O
(Fig. 9(b)) on the wear track, which also conrms the formation of
MML. Formation of iron oxide layer on worn surface was also found
by Singh and Alpas [23] and they reported that iron oxide layer
will reduce the coefcient of friction and wear rate of the com-
posites by acting as in situ lubricant. To understand this further,
the subsurface analysis was carried out on the worn pin speci-
men by cross-sectioning it vertically along the sliding direction.
Thecross-sectionedmicrostructureof Al4Cu10TiB
2
wornsurface
(Fig. 10(a)) shows very ne extruded portion at rear (compared to
the Al4Cumatrix alloy, Fig. 6(a)) andthe highmagnicationimage
(Fig. 10(b)) reveal the existence of MML and deformed region. The
ne extruded part in composites is attributed to the presence of
TiB
2
particles, which reduces the softening tendency of the matrix
when subjected to elevated temperature wear process. The obser-
vance of MML only in composite is attributed to the presence of
hard ne TiB
2
particles, which abrade the steel counterface and the
resultant debris (generally of Fe and Fe-oxide) get in between the
mating surfaces where it is mixed with soft matrix during subse-
quent sliding toformMML. Fig. 10(c) shows a schematic of different
regions on the worn subsurface microstructure of Fig. 10(b). Bellow
MML, there is a region, where the TiB
2
particles are well distributed
within the matrix and this is due to the high shear strain experi-
enced locally during the deformation and termed as shear mixed
layer. In this region, most of the ex situ composites reinforcements
fractured to ne particles and get distributed uniformly [23,24]. On
the other hand, inthe present case since the in situ formed TiB
2
par-
ticles are less than 1.5min size, the particles did not fracture and
are distributed uniformly beneath the MML region. Further below
the shear mixed region, plastic ow line can be clearly observed
(deformed layer) where the TiB
2
particles are aligned in such a way
that ow lines progressively bend towards the sliding direction as
moving towards the worn surface. The alignment of TiB
2
particles
alongtheowlinerepresents theplastic deformationundergoneby
subsurface along the shear strain direction. Near the un-deformed
region of the composite pin, the shear strain is minimum, but as it
approaches the worn surface, the shear stain increases and even-
tually reaches maximum near to the worn surface. Such ow lines
are not observed in the Al4Cu alloy because of the absence of TiB
2
particles. Thereforefromthepresent wear scar analysis onthecom-
posites it can be summarised that at high temperature, oxidation
and delamination were the dominant wear mechanisms, whereas
at room temperature the predominant wear mechanism for the
composites (up to 10wt.% TiB
2
) is adhesion and abrasion. When
the temperature is increased to 300

C and at a load of 120N, the

Al4Cu10TiB
2
in situ composites undergo transition from mild to
severe wear and the wear surface (Fig. 11(a)) is similar to type of
metal ow observed in Al4Cu alloy at 100

C (Fig. 5(a)) and EDS

analysis (Fig. 11(b)) conrms the absence of Fe on the worn surface.
4. Conclusions
The room temperature and elevated temperature wear resis-
tance of Al4Cu alloy is increased with the addition of TiB
2
in situ
particles. Coefcient of frictionof these in situ composites are lower
thanthe base alloy. The wear rate of alloy andcomposites increased
with increase in applied load and sliding temperature. The mild to
severe wear mode transition in Al4Cu alloy is dependent on the
applied load, temperature and TiB
2
content. Normalized wear rate
decreases with increase in temperature for the given amount of
TiB
2
, which clearly indicates that the TiB
2
particles in the Al4Cu
alloy are more effective in resisting the wear at high temperature
than at room temperature. At elevated temperature, the predom-
inant wear mechanisms in Al4Cu alloy are adhesion and metal
ow, whereas in Al4CuTiB
2
composites oxidation, delamination
and metal ow are the dominant wear mechanisms.
Acknowledgement
The authors are thankful to Naval Research Board, Government
of India, for funding this research work.
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