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Article history:
Received 5 February 2011
Accepted 24 March 2011
Available online 30 March 2011
Keywords:
A. Metal matrix composite
C. Mechanical alloying
E. Wear
a b s t r a c t
The present work deals with studies on the manufacturing and investigation of mechanical and wear
behavior of aluminum alloy matrix composites (AAMCs), produced using powder metallurgy technique
of ball milled mixing in a high energy attritor and using a blendpresssinter methodology. Matrix of
pre-mechanical alloyed Al4.5 wt.% Cu was used to which different fractions of nano and micron size
TiC reinforcing particles (ranging from 0 to 10 wt.%) were added. The powders were mixed using a planetary ball mill. Consolidation was conducted by uniaxial pressing at 650 MPa. Sintering procedure was
done at 400 C for 90 min. The results indicated that as TiC particle size is reduced to nanometre scale
and the TiC content is increased up to optimum levels, the hardness and wear resistance of the composite
increase signicantly, whereas relative density, grain size and distribution homogeneity decrease. Using
micron size reinforcing particulates from 5% to 10 wt.%, results in a signicant hardness reduction of the
composite from 174 to 98 HVN. Microstructural characterization of the as-pressed samples revealed reasonably uniform distribution of TiC reinforcing particulates and presence of minimal porosity. The wear
test disclosed that the wear resistance of all specimens increases with the addition of nano and micron
size TiC particles (up to 5 wt.%). Scanning electron microscopic observation of the worn surfaces was conducted and the dominant wear mechanism was recognized as abrasive wear accompanied by some
delamination wear mechanism.
2011 Elsevier Ltd. All rights reserved.
1. Introduction
Aluminum-based alloys are widely used as aerospace and
automotive components, because of their high specic strength,
stiffness and formability. However, both pure Al and Al alloys possess poor wear resistance. On the other hand, Al alloy matrix
composites are known to offer better wear resistance and bulk
mechanical properties. These composites are synthesized by liquid
or powder metallurgy routes. The wear performance of these composites is a subject of strong interest, especially for their potential
application in automobile components including cylinder block,
piston and brake disks [1]. The wear test is usually conducted
under sliding wear conditions using pin-on-disk or block-on-ring
tests. Though high volume fractions of hard reinforcements are
favored for wear resistance, the wear rate of the counter-body is
found to be greatly enhanced by the abrasive action of the reinforcements [2]. Carbides, oxides, nitrides and different intermetallics compounds have been used extensively as reinforcing
particulates for AMCs [3]. In specic, SiC and Al2O3 were the
Corresponding author. Tel.: +98 21 82084083; fax: +98 21 61114083.
E-mail address: emamy@ut.ac.ir (M. Emamy).
0261-3069/$ - see front matter 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2011.03.056
3719
new materials and appears further as an attractive method of synthesis in view of its potential for large scale production [16]. To obtain an absolute nanocrystalline alloy powder, materials from
initial mixtures of elemental powders in a grain size range of
micrometers with appropriate weight proportions are charged into
a high energy ball mill container. By applying the proper milling
condition such as suitable process control agent (PCA), ball to powder ratio (BPR) and time of milling, the specic alloy will be
achieved in solid state. Recently, a number of Al65Cu20TM15 or
Al50TM40Si10 (TM = early transition metals like Ti, Nb and Zr) alloys
have been developed by mechanical alloying with amorphous and/
or nanocrystalline matrix and in situ nano-intermetallic phase/
compound dispersion [6,17,18]. These composites have exhibited
nearly 23 times greater wear resistance and hardness than the
conventional microcrystalline and age hardenable Al alloys [19
21]. The general characteristics and mechanisms of mechanical
milling and alloying have been studied, but the inuence of milling
parameters on mechanical properties of composites is not yet fully
known [22]. Wear behavior of these novel mechanically alloyed Al
alloys or composites has not been investigated fully [2].
The present study has focused on the manufacturing of MMCs
using a nanocrystalline alloying matrix for the desired composite
with the composition of Al4.5 wt.% Cu, which according to the
previous study was prepared through mechanical alloying using
a high energy attritor ball mill to produce the nanostructure matrix
powder of the composites [23]. Different concentrations of nano
and micron size TiC particles as reinforcement were added to the
matrix to improve the hardness and wear resistance of the MMCs,
proper distribution of the reinforcing particles in the matrix is very
important in blending process which is measured through precise
EDX analysis [4,6], then the effect of different weight fractions of
reinforcement on the wear resistance, hardness, relative density
and microstructure of a new generation nanocrystalline matrix
composites are investigated. An effort has also been made to
understand the operative wear mechanism.
2. Experimental procedure
Pre-alloyed powder of the composite matrix produced by
mechanical alloying technique with nominal stoichiometry of
Al4.5 wt.% Cu (M) and particle size in range of 1020 lm with a
ake like morphology, typical of mechanical alloyed particles were
used. The chemical composition of the matrix is shown in Table 1,
according to previous study to produce the alloying matrix, pure Al
and Cu elemental powders with average particle size of 150 and
40 lm respectively were subjected to mechanical alloying in an
attrition ball mill. Milling was operated for 70 h at the rotational
speed of 270 rpm with 12:1 ball to powder weight ratio (BPR)
and 1.5 wt.% stearic acid was used as the milling process control
agent (PCA), using stainless steel vial (AISI 316) and hardened
chromium steel balls (6 and 10 mm diameter with the ratio of
1:2). The powder in the vial was protected with high purity argon
gas and the milling tank was cooled with a x ow of cold water
through a rotating system. Samples for analysis were removed by
interrupting the ball mill at various intervals (each 10 h). Alloying
behavior, solution and crystallite size evolution during milling
were determined by X-ray diffraction (XRD) analysis using a Philips (30 kV and 25 mA) diffractometer with Cu Ka radiation (k =
1.5405 ). All XRD experiments were done with a step size of
0.02 and a time per step of 0.1 s. Crystallite size of powders was
evaluated using the WilliamsonHall and Sherrer methods
[23,24]. Since both Al and Cu are ductile materials, the dominant
mechanism that occurs through mechanical alloying of these elements is indeed ductileductile which results in formation of
lamellar structure of repeated attened layers of aluminum and
copper in each grain of the powder particles [24].
In order to study the effect of reinforcing particulate amount
and size on the hardness, sliding wear behavior and the microstructure of the composites, different weight percent of nano-size
(0%, 0.5%, 1%, 3%, 5% and 7 wt.%) and micron size (0%, 5%, 7% and
10 wt.%) TiC particulates were added to the prepared alloy matrix
powder and blending was performed for 2 h in a planetary ball mill
at nominal room temperature and at a rotation speed (cup speed)
of 400 rpm with 12:1 ball to powder weight ratio using tungsten
carbide (WC) coated vials and hardened chromium steel balls in
four different sizes (20, 15, 10, 6 mm diameter) under Ar atmosphere and applying 1.5 wt.% stearic acid as the milling PCA [24].
The microstructure and distribution of the milled TiC powders
and the compacts were studied by CamScan MV3200 scanning
electron microscope and supplemental EDX.
The same equipment was employed to characterize the milled
powder morphology and the topology of the surfaces of compact
samples. The as-received and milled powders were consolidated
into compacts using cold and hot unidirectional pressing. First,
4 g of powders were measured and poured into in a cylindrical tool
steel die and were cold pressed. Fig. 1a shows the scheme of the die
with an inner diameter of 10 mm. Powder mixture was sustained
for 10 min in the pressure of 650 MPa then according to Fig. 1b
by adjusting an auto-controlled power of the heating system, the
compacted samples were hot pressed at 400 C under pressure of
500 MPa for 80 min. Then they are allowed to cool to room temperature and stripped off the die for characterization and mechanical
tests. Density values of compact samples were measured applying
three different methods of geometrical, Archimedes and theoretical approaches. Vickers microhardness method was used to determine the hardness of consolidates using a Mitutoyo microhardness
tester. The VHN measurements were conducted at 50 gf for 10 s of
dwell time. A minimum of ve indentations were measured per
condition.
The dry wear tests were performed according to ASTM standard
G99 [25] on a unidirectional pin-on-disk aperture wear tester with
a counter face of AISI 52100 steel which was hardened to 62 HRC at
ambient temperature, the cylindrical shape pins with the dimensions of 10 mm in diameter and 15 mm in length were prepared
by machining the consolidated samples for the tests. Prior to wear
tests, the pins and disks were polished/grinded with 800 grit SiC
paper to a 1 lm nish. Samples were cleaned thoroughly using
an ultrasonic device with acetone and dried prior and after the
tests and then weighed to determine the wear loss using an electronic balance (GR200-AND) with an accuracy of 0.1 mg. All data
on wear were measured from the pins. The volume loss of samples,
according to Eq. (1), was calculated through the mass loss divided
by the Archimedes density of the materials and the friction coefcient (l) values were measured by a load cell equipped with the
pin-on-disk apparatus and the wear rate values of the samples
were calculated for all samples according to Eq. (2).
The morphology of the worn surfaces was analyzed using similar SEM, the same test parameters were used for all samples: 10
Table 1
Chemical composition of the alloying matrix.
Materials
Si
Fe
Cu
Mn
Mg
Cr
Ni
Zn
Ti
Al
0.01
0.012
4.542
0.003
0.002
0.02
0.001
0.01
0.004
Base
3720
Fig. 1. (a) Schematic of cylindrical tool steel die and its dimensions used for cold and hot press and (b) auto-controlled power of the heating system used for compacts to be
hot pressed.
and 20 N for the normal load, 200 rpm for the sliding speed,
1500 m for the sliding distance and 25 C for the ambient
temperature.
Weight loss g
1000
Density g=mm3
Fig. 2. SEM micrographs of: (a) as-received Al powder and (b) Al4.5 wt.% Cu (M) powders mixture after 10 h milling time.
3721
Fig. 3. XRD patterns of: (a) Cu/Al powder mixture produced and (b) most intensive Al peak positions produced at different intervals of milling.
creases, the grain size decreases to some extent. The point to bear
in mind is the homogeneity of the composites is reduced in specimens containing more than 5 wt.% TiC nano and micron size particles. The reason for this phenomenon can be due to their higher
specic surface of ner particles in comparison with coarse particulates [27]. An increase in the specic surface leads to higher interparticle friction and thus leading to decreased particle distribution
and so weakening of grain junctions occurs [28]. It should be stated
that the addition of hard reinforcing particles affects both compressibility and sinterability of compacts. So, the relative density
of the compacts decreases and porosities are formed [26]. The
experimental, theoretical and relative density values of the compacts are shown in Table 2.
The relative density of the consolidated samples, measured by
Archimedes water immersion method, is demonstrated in Table
2. By increasing nano-size particulates portion, in comparison with
same portion of micron sized particulates, density rst increases
slightly and then decreases (10 wt.% TiCl). The reinforcing particles
which are smaller than the matrix particles situate among the matrix particles, lling pores. This causes an increase in the density of
the nano-particle reinforced composites compared with the matrix
and micron size particle reinforced composites. However, the increase in agglomeration of the particles by increasing the nanosized TiC particulates may lead to the decrease of the density, in
case of further TiC addition (>7 wt.%). It would be worth mentioning that nano-particles are prone to agglomerate and pores retained in the agglomerated zones, which may result in
decreasing the density [29].
Moreover, according to Fig. 5, XRD patterns reveal that no
detectable interaction layer is observed between TiC and Al alloy
matrix during different mixing intervals. Unequivocally, formation
of interaction layer between TiC and the matrix is very likely to occur especially after long mixing periods, the products (different
carbide or intermetallics) are so small, which is undetectable by
X-ray diffraction technique. Besides the production of this interaction will make mechanical properties to decline signicantly, so
the shortest time of mixing (2 h with planetary ball mill) was selected to ensure the minimum interaction and well distribution
to avoid the drawbacks.
In order to investigate the morphology and analysis of TiC nanoparticles, SEM image with high resolution and high magnication
3722
Fig. 4. Optical micrographs of the microstructure of the compacts with different contents of TiC nano-particles: (a) Al + 4.5 wt.% Cu(M), (b) M + 3 wt.% TiC, (c) M + 5 wt.% TiC
and (d) M + 7 wt.% TiC.
Table 2
Experimental and theoretical density values of consolidated samples.
Sample
name
Theoretical
density
(0.001 g/cm3)
Geometrical
density
(0.001 g/cm3)
Archimedes
density
(0.001 g/cm3)
Relative
density
Pure Al
Al + 4.5 wt.%
Cu (M)
M + 0.5% TiC
M + 1% TiC
M + 3% TiC
M + 5% TiC
M + 7% TiC
M + 5% TiCl
M + 7% TiCl
M + 10%
TiCl
2.701
2.982
2.601
2.752
2.601
2.833
0.97
0.95
2.991
3.001
3.041
3.081
3.121
3.081
3.121
3.176
2.706
2.680
2.672
2.671
2.692
2.758
2.743
2.688
2.841
2.880
2.888
2.895
2.803
2.772
2.746
2.763
0.95
0.96
0.95
0.94
0.90
0.90
0.88
0.87
3723
effect of Orowan strengthening mechanism decreases [33]. According to the literature, the optimum levels of Al2O3 and SiC also had
been detected to be effective in enhancing mechanical properties
of composites [2,5]. In case of micron size TiC particulates, by
increasing its content from 5% to 10 wt.% the hardness decreases
slightly.
3.3. Investigation of wear behavior
Fig. 5. XRD patterns of TiC particulates and alloying matrix (M) mixture in different
intervals of mixing via ball milling.
To investigate the size effect of reinforcing particulates a comparison is made between the composites reinforced with nano
and micron size TiC. Figs. 10 and 11 show the weight loss values
for all specimens under 10 and 20 N applied loads. It is generally
believed that contribution of hard particles to aluminum alloys results in an improvement of the wear resistance of the base alloy to
a great extent [34,35]. Based on the results, under both loads the
amount of weight loss of the all nano-particle reinforced composites is less than that of micron size TiC reinforced condition. The
main reason for this fact is clearly related to the hardness enhancement of nano-size TiC reinforced samples and according to Archad
equation:
Q K
W
H
Fig. 6. (a) SEM image of TiC nano powders, (b) high magnication SEM image of TiC nano-particles indicating the formation of agglomerated powders and (c) corresponding
EDX point analysis of TiC powders coated with Au.
3724
Fig. 7. SEM micrographs of the surfaces of consolidated: (a) M + 7 wt.% TiC and (b) M + 3 wt.% TiC nanocomposites.
Fig. 8. (a) SEM image, (b) corresponding line scan EDX spectra and EDX elemental maps of (c) Al, (d) Cu and (e) Ti of the surface of M + 5 wt.% TiC nanocomposite.
3725
Fig. 9. Microhardness test results of bulk aluminum, Al4.5 wt.% Cu (M) and
composites along the diameter of consolidated samples.
Fig. 11. Weight loss values under 20 N applied load for: (a) bulk Al, alloying matrix
(M) and TiC nano-particle reinforced specimens and (b) micron size TiC reinforced
specimens.
Fig. 10. Weight loss values under 10 N applied load for: (a) bulk Al, alloying matrix
(M) and TiC nano-particle reinforced specimens and (b) micron size TiC reinforced
specimens.
3726
Fig. 12. Variation of wear rate values of the composites, Al and matrix under 10 and
20 N applied loads.
Fig. 14. Variation of the friction coefcient (l) of: (a) M + 5 wt.% TiC and (b) M
samples via sliding distance under 20 N applied load.
Fig. 13. Variation of the friction coefcient (l) of: (a) M + 5 wt.% TiC and (b) M
samples via sliding distance under 10 N applied load.
nano-size TiC particles) is the main reason for the increased wear
rates, the fragmentation of coarse and brittle TiC particles during
wear test may contribute to the increased wear rates of the composite containing micron size TiC particles. As a result lower hardness and wear resistance will be achieved.
As expected, the weight loss and wear rate values for all samples under 20 N applied load is more for 10 N load. It can be explained that at higher load the separation of surface asperities
and hence the number of contact asperities increase and consequently the worn surface material increases [37]. Based on the
weight loss data, specimens with 5 wt.% TiC and without reinforcement have the highest wear resistance among the all tested samples, also unreinforced pure aluminum give the lowest wear
resistance.
Figs. 13 and 14 show the variation of the friction coefcient (l)
of samples via sliding distance under the both applied loads. The
average friction coefcient of Al4.5 wt.% Cu + 5 wt.% TiC sample
was 0.31 under 10 N applied load which is much smaller than that
for the matrix sample (0.575) in the same condition. This is mainly
due to the high hardness of the nanostructured composite. The
reinforcement particles support the load, so as to lessen the touch
area between the pin and counter disk surface, decrease the friction coefcient and can prevent the scratch and cut from the surface [38]. Also, a comparison between Figs. 13 and 14 reveals
that increasing the normal load from 10 to 20 N has no signicant
effect on the variation trend of l values, but in case of matrix specimen the friction coefcient is higher in 20 N applied load. Similar
results for aluminum alloy matrix composites have been reported
by Bermudez et al. [39]. For all specimens, initially friction coefcients have a quick increase with sliding distance to an approximately steady range after about 50 m. This increase in l
3727
Fig. 15. SEM micrographs of worn surfaces of: (a) bulk pure Al, (b) alloying matrix (M), (c) M + 3 wt.% TiC, (d) M + 5 wt.% TiC and (e) M + 7 wt.%TiC nanocomposites under
10 N applied load.
corresponds to an increase in apparent contact area, until full contact occurs across the full diameter of the pin.
Results of SEM revealed complex wear mechanisms on the sliding surface of the composites and the aluminum alloy matrix, as
seen in Figs. 15 and 16. Three different wear mechanisms were observed to coexist, namely abrasion, delamination and adhesion.
Surface coverage of impression for each of the mechanisms depends on the load applied normal to the worn surface. Identication of the type of wear mechanisms involved depends on
surface morphology of the worn specimen. SEM results were performed after completion of the wear experiments. Fig. 15 shows
the wear surfaces of samples under 10 N applied load which reveals great details of the contributed wear mechanisms. As it is
clear, the worn surface of the aluminum consists of large delaminated areas and no sign of grooves are observed (solid arrows indicate abrasive wear and bald arrows indicate delaminating or
adhesive ones in these gures), in contrast as can be seen in other
worn surfaces micrographs, as TiC nano-particle reinforcement
fraction is increased through the matrix the surface coverage
impression alters gradually and grooves parallel to the sliding vector are observed.
Distinct ner grooves and the abrasive zones have become
more, especially for the unreinforced alloying matrix. The worn
surface observation suggests that the dominant wear mechanism
for samples containing different levels of TiC nano-particles is
abrasive wear accompanied by some delaminating wear mechanism under both loads, regarding to the fact that for the composite,
because of the hard reinforcement presence and higher hardness,
the portion of adhesive mechanism is less or ignorable, the worn
surface is smoother and grooves are ner and also the total depth
of deformation is smaller than for the aluminum alloy matrix. The
depth of deformation should be linearly related to the true contact
area and the asperity contact radius. In case of micron size TiC reinforced samples, as can be seen in Fig. 16 there is no sign of grooves
and mainly adhesive wear mechanism is present in the surface of
the samples with 7% and 10 wt.% TiC. This is due to lower hardness
of these samples and also excessive delaminated areas are formed
due to particle decohesion during wear test, as hard micron size
3728
Fig. 16. SEM micrographs of worn surfaces of micron size TiC reinforced composites: (a) M + 7 wt.% TiC and (b) M + 10 wt.% TiC, under 10 N applied load.
Acknowledgements
The authors would like to thank University of Tehran and Sahand University of Technology for nancial supports of this
research.
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