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Article history: In the present work, the compressive formability of porous Al/SiC composites fabricated through
Received 26 November 2013 mechanical alloying (MA) is investigated. Aluminum matrix composites consisting of pure Al reinforced
Received in revised form 21 December 2013 with different amounts of 5, 10, 20 wt.% SiC with mean particle size of 16 lm and other composites con-
Accepted 23 December 2013
taining 10 wt.% SiC with particle sizes of 12, 16 lm were produced by a powder metallurgy route. The
Available online 3 January 2014
effect of milling time on microstructure and mechanical properties of the composites was studied. The
phased compression tests coupled with density measurement and continuous compression of the sam-
Keywords:
ples were indicative of increases in strength and decreases in ductility of the composites with increasing
Aluminum matrix composite
Powder metallurgy
milling time, increasing amount of reinforcement particles and decreasing their size. Instantaneous den-
Mechanical alloying sity coefcient and instantaneous work hardening exponent of the samples, during deformation stages,
Upsetting show decreasing trends when density increased. It was also revealed that instantaneous work hardening
Workability exponent increase with increasing milling time, increasing weight percentage of the reinforcement and
decreasing its particle size. The samples having higher initial densities, containing lower amounts of lar-
ger SiC particles show better workability.
2013 Elsevier B.V. All rights reserved.
0925-8388/$ - see front matter 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jallcom.2013.12.205
A. Hassani et al. / Journal of Alloys and Compounds 591 (2014) 132142 133
3. Experimental procedure
cold deformation is sufciently large for the elastic strain to be ne-
glected, it is frequently convenient to employ the Ludwik power To fabricate the composites, various nominal portions of 5 wt%,
law [21]: 10 wt% and 20 wt% of the SiC powders having the particle sizes of
12 and 16 lm, were added to the atomized Al powders of 65 lm
reff K eneff 12
(Table 1). Those mixtures were ball-milled for 4, 8, and 12 h in a
Fig. 1. SEM images of (a) as-received Al powder, (b) 12 lm SiC powder, (c) 16 lm SiC powder and the Al10%SiC12 lm powder mechanically alloyed for (d) 4 h and (e) 8 h
(lamellar structure of one of powder particles is shown in higher magnication) and (f) 12 h.
A. Hassani et al. / Journal of Alloys and Compounds 591 (2014) 132142 135
Fig. 2. SEM images of (a) Al5%SiC16 lm, (b) Al10%SiC16 lm and (c) Al20%SiC16 lm, after 12 h of milling time (the right column is same as the left but in higher
magnication).
planetary ball mill at speed of 270 rpm using chromium steel balls diffractometer equipped with a graphite monochromator using
of 10 mm diameter. The ball-to powder mass ratio was 12:1 zinc Cu Ka operated at 40 kV and 30 mA. The XRD patterns were re-
stearate (2 wt%) was used as the process control agent (PCA) to corded in the range of 080 for 2h by the step size of 0.02 /s. After
prevent excessive cold welding of powder particles. Mechanical background subtraction, all the proles are t with Lorentzian
alloying conducted under argon atmosphere for a variety of milling function [22] by Fityk software and full-width at half maximum
times (4, 8, 12 h). The mixed powders were die-pressed at room (FWHM) for all peaks was measured. The results were analyzed
temperature under a pressure of 315325 MPa in a 15 mm diame- using WilliamsonHall [23] to calculate the crystallite size of the
ter cylindrical steel die to produce the compacts with densities of samples.
0.87, 0.9 and 0.95. The specimens which consisted of eight pre- For compression tests, cylindrical specimens with 14.9 mm
forms of the composites with different initial conditions (Table 2) diameter and 8.4 mm length were used. Compression tests were
were then compressed using Dartec compression testing machine carried out at room temperature using an Instron machine operat-
at a constant cross-head velocity of 0.1 mm/s. After degassing the ing at a constant strain rate of 0.1 mm/s. To reduce the friction,
specimens at 200 C for 15 min, they were sintered for 1 h in an samples were wrapped with Teon tape. The test was carried out
electrical furnace protected by Ar atmosphere with a heating rate until the rst surface cracks was seen.
of 10 C/min to a temperature of 500 C. Cold upset test were conducted at room temperature in a com-
Phase analysis of milled powder at different stages of milling puter controlled Dartec compression testing machine at a constant
was conducted by X-ray diffraction using a Philips X-ray cross-head speed of 0.1 mm/s. In general, each preform was sub-
136 A. Hassani et al. / Journal of Alloys and Compounds 591 (2014) 132142
jected to compressive incremental loading in steps of 3 kN until platelet or pancake shapes as it is shown in Fig. 1d. It can be seen
ne cracks appeared on its free surface. After each interval of load- that the initial irregular shape of the powder has changed to ake
ing dimensional changes in the specimen such as height after like after mechanical alloying, and the small irregular particles
deformation (hf), top contact diameter (D1), bottom contact diam- have attened and attached to the large particle (Fig. 1d). Fig. 1e
eter (D2), bulged diameter (Db) and density of the preform (q) were shows after 8 h of milling a composite lamellar structure is formed
measured. The density of forged preforms was determined using by cold welding of the attened particles; so, it seems that the cold
the Archimedes principle. The above measurements were made be- welding is the dominant mechanism during milling before 8 h of
fore and after deformation. The instantaneous density coefcient process due to the ductility of aluminum powders. Strain harden-
(Ai), instantaneous strain-hardening exponent (ni) and formability ing of powder particles by increasing the MA time results in brittle-
stress index (b) under triaxial stress state condition was measured ness of particles cause the fragmentation; thus more equiaxed and
according to relations which have been discussed in Section 2 ner particles is seen in powders after 12 h of milling (Fig. 1f).
using owcharts describes in Narayanasamy et al. [14]. Fig. 2 shows the SEM images of composite powders reinforced
Density measurements of the forged samples were carried out, by 16 lm SiC particles milled for 12 h with various amount of rein-
using the Archimedes method using pure water according to the forcements (SiC particles). Results show that increase in percent-
standard ASTM B 328-96 [24]. Also porosity in term of percentage age of SiC, will cause to reduction of the size of composite
calculated by: powder. The reason can be referred to this point that with increas-
qc q ing SiC particles, as the harder part, severe deformation will be
Porosity% 100 happened in softer part (Al particles). As a result, the crystalline de-
qc
fects such as dislocations are generated. Hence the dislocations
where qc is theoretical density of composite and q is the calculated density is increased and hardening of particles is accelerated. Frac-
density of samples. ture of harder particles leads to reduce the size of particles.
Microstructural characteristics of the consuming powders, the Results in Table 2 show that with increasing amount of SiC rein-
milled composite powders and sintered preforms were investi- forcement, the amount of porosity in sintered performs was ob-
gated by scanning electron microscope (SEM, Philips XL30, Nether- served to be reduced. Also, Compare materials number 3 and 5 in
lands). An automatic image analyzer system is used to calculate Table 2, it is clear that at the same milling time and percentage
the average grain size of particles using SEM images. of reinforcement, decrease in the particle size of SiC particles had
signicant effect on reducing the porosity due to a higher rate of
4. Results and discussion load transfer. In the composites with higher amount of reinforce-
ments or lo with arrows in SEM images of Fig. 3, show some of
4.1. Microstructural studies these porosities in the sintered samples. By decrease the particle
size from 16 to 12 lm, the extent of porosity was reduced by about
Fig. 1 shows SEM micrographs of the as-received Al and SiCp 3.7%. In the composites with higher amount of reinforcements or
and the evolution of morphologies of milled powders by increasing lower particle size of them, the total matrixreinforcement inter-
the time of mechanical alloying. It can be seen that Al particles ex- faces is longer. Therefore the paths for diffusion, as one of the
hibit an irregular shape (Fig. 1a). Fig. 1(b and c) show that SiC par- mechanisms of pore elimination during sintering, are much more
ticles have irregular shape with sharp angles. After 4 h of milling Al in these composites. As a result the elimination of pores is acceler-
particles which are the more ductile component get attened to ated. On the other hand at the same amount of reinforcements, the
Fig. 3. SEM images of sintered composites which is mechanically alloyed for 12 h; (a) Al10%SiC12 lm and (b) Al10%SiC16 lm. Some porosities are indicated by the
arrows.
A. Hassani et al. / Journal of Alloys and Compounds 591 (2014) 132142 137
Fig. 6. Axial, hoop, effective and mean stress vs. axial stress for Al10%SiC12 lm mechanically alloyed for (a) 4 h, (b) 8 h and (c) 12 h.
Fig. 7. Variation of instantaneous density coefcient (Ai) with relative density for samples milled in different times at (a) axial stress state and (b) triaxial stress state.
slightly. This is caused by the fact that the pores no more enhance in Fig. 8. For all milling times the exponent have the descending
the capacity of deformation of the material, but they lower the trend by increasing the relative density. Also, the increase in mill-
strength by acting as crack initiation sites. The rate of decrease in ing time leads to achieve higher instantaneous strain-hardening
instantaneous density coefcient (Ai) with respect to relative den- exponent. In porous materials, geometrical work hardening is
sity (R) is higher for 12 h milled sample compared to others be- added to the conventional work hardening resulting in a higher
cause of geometric hardening in 12 h milled composite. work hardening compared with non-porous materials [26]. By
Using Eq. (14) instantaneous strain-hardening exponent (ni) is increasing the milling time, domination of geometrical work hard-
calculated for Al10%SiC12 lm at different milling times. The ening, compared to the work hardening resulted from dislocation
variations between the instantaneous strain-hardening index va- mechanisms, causes the work hardening exponent to be higher
lue (ni) and the relative density (R) for these composites is shown and its fall with relative density increase to be steeper. As seen
A. Hassani et al. / Journal of Alloys and Compounds 591 (2014) 132142 139
Fig. 8. Variation of instantaneous strain-hardening exponent (ni) with relative density for samples milled in different times at (a) axial stress state and (b) triaxial stress state.
Fig. 10. True stressstrain curves of composites reinforced with different amount of
16 lm SiC and milled for 12 h.
Fig. 9. Variation of formability stress index (b) with relative density for samples
milled in different times. different milling times. Increase in formability stress parameter,
b, with increasing relative density during the process is evident.
Higher strengthening of the material due to closure of pores, which
in the gure, the nal value of n for a sample milled for 12 h is leads to a higher density, is the cause of this change [10]. The less
more than that for the other samples, because here the closure of the time of milling, the higher is the strain to failure.
pores occurs late, and even geometrical work hardening occurs at
nal stages of deformation. In the other samples, faster elimination 4.2.2. Effect of the amount of SiC particles
of pores leads to a nearly ineffective geometrical work hardening, True stresstrue axial strain curves of composites reinforced
and to domination of conventional work hardening, which results with different amount of 16 lm SiC particles and milled for 12 h
in lowering n value and expansion of its change range (the lower are shown in Fig. 10. By increasing the amount of SiC particles
decline rate). the strength is increased while the strain to fracture is decreased.
Formability stress index (b) is calculated by Eq. (7) to determine SiC particles as the harder part in the composites can prevent the
the fracture limit as discussed in Section 2.1. Fig. 9 shows the var- dislocations glide. The lower ductility of the composites contain
iation of this index with relative density for Al10%SiC12 lm at more SiC particles may come from the fact that large volume frac-
140 A. Hassani et al. / Journal of Alloys and Compounds 591 (2014) 132142
Fig. 11. Axial, hoop, effective and mean stress vs. axial stress for (a) Al5%SiC16 lm, (b) Al10%SiC.16 lm and (c) Al20%SiC16 lm.
Fig. 12. Variation of instantaneous density coefcient (Ai) with relative density for different amount of SiC particles at (a) axial stress state and (b) triaxial stress state.
tions usually lead to a non-homogenous distribution and clustering amount of SiC, strain to fracture is reduced and the strength is in-
of the particles, degrading the mechanical properties of the com- creased. Using results in Fig. 11 in equations in Section 2, the work-
posite [27,28]. ability parameters including instantaneous density coefcient (Ai),
Data extract from upset tests of composites contain different instantaneous strain-hardening exponent (ni) and Formability
volume fraction of SiC is shown in Fig. 11. By increasing the stress index (b) are calculated.
A. Hassani et al. / Journal of Alloys and Compounds 591 (2014) 132142 141
Fig. 13. Variation of instantaneous strain-hardening exponent (ni) with relative density for different amount of SiC particles at (a) axial stress state and (b) triaxial stress state.
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