Materials Science and Engineering A 480 (2008) 496–505

Aging behaviour of Al–Cu–Mg alloy–SiC composites

Sharmilee Pal a , R. Mitra a,∗ , V.V. Bhanuprasad b
aDepartment of Metallurgical and Materials Engineering, Indian Institute of Technology, Kharagpur 721302, W.B., India
b Ceramics and Composites Group, Defence Metallurgical Research Laboratory, P.O. Kanchanbagh, Hyderabad 500058, A.P., India
Received 5 April 2007; received in revised form 11 July 2007; accepted 26 July 2007

Abstract
The age-hardening kinetics of powder metallurgy processed Al–Cu–Mg alloy and composites with 5, 15 or 25 vol.% SiC reinforcements,
subjected to solution treatment at 495 ◦ C for 0.5 h or at 504 ◦ C for 4 h followed by aging at 191 ◦ C, have been studied. The Al–SiC interfaces
in composites show undissolved, coarse intermetallic precipitates rich in Cu, Fe, and Mg, with its extent varying with processing conditions.
Examination of aging kinetics indicates that the peak-age hardness values are higher, and the time taken for peak aging is an hour longer on
solutionizing at 504 ◦ C for 4 h, due to greater solute dissolution. Contrary to the accepted view, the composites have taken longer time to peak-age
than the alloy, probably due to lower vacancy concentration, large-scale interfacial segregation of alloying elements, and inadequate density of
dislocations in matrix. The composite with 5 vol.% SiC with the lowest inter-particle spacing has shown the highest hardness.
© 2007 Elsevier B.V. All rights reserved.

Keywords: Discontinuously reinforced aluminum composites; Aging; Kinetics; Interfaces; Hardness

1. Introduction have reported slower kinetics of aging in the powder metallurgy

Discontinuously reinforced aluminum (DRA) matrix com-
posites have received significant attention in recent years. The
high specific strength and stiffness make the DRA composites
attractive as candidate materials for aerospace and automo-
tive applications. It has been reported that the dislocations are
punched out at the reinforcement–matrix interfaces to relax
the stress generated owing to the mismatch in coefficients of
thermal expansion (CTE) [1,2] of Al (24 × 10−6 K−1 ) and SiC
(4 × 10−6 K−1 ). It has also been reported that the age-hardenable
Al alloy–SiC composites demonstrate accelerated kinetics of
aging [3–13], when compared to that of the unreinforced alloy
due to the much greater dislocation density in the former. The
dislocations provide sites for heterogeneous nucleation of the S
(CuMgAl2 ) precipitates [7]. Suresh et al. [6] have concluded that
the volume fraction of SiC reinforcements beyond 6% has no sig-
nificant effect on the aging kinetics of Al–3.5Cu alloy matrix in
the cast composites. However, Lin et al. [10] have shown a mono-
tonic decrease in the peak-aging time for the 2024 Al alloy matrix
with increasing volume fraction of SiC reinforcement particles.
Contrary to the results of most studies, Janowski and Pletka [14]
processed, liquid phase sintered Al–SiC composites with coarse
and widely spaced SiC particles, compared to that of similarly
processed unreinforced Al alloy, and attributed its cause to rel-
atively low dislocation density in the matrix. In general, it is
accepted that the aging behaviour depends on the reinforcement
and its volume fraction, alloy composition, heat treatment, and
other processing parameters.
The present study is aimed at examination of the role of SiC
reinforcement particles and interfaces on the aging kinetics of
the matrix in a powder metallurgy (P/M) processed Al–Cu–Mg
alloy–SiC composite, for two different conditions of solution
treatment, leading to different degrees of dissolution of matrix
precipitates.
2. Experimental procedure
The experimental procedure involves processing and heat
treatment of the composites, and characterization of microstruc-
ture and interfaces.
2.1. Processing

∗ Corresponding author. Tel.: +91 3222 283292; fax: +91 3222 282280. The Al–Cu–Mg alloy–SiC composites for the present investi-
E-mail address: rahul@metal.iitkgp.ernet.in (R. Mitra). gation were obtained from the Ceramics and Composites group,

0921-5093/$ – see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2007.07.072
 S. Pal et al. / Materials Science and Engineering A 480 (2008) 496–505
Defence Metallurgical Research Laboratory, Hyderabad, India.
Through repeated bulk EDX analyses and optical emission spec-
troscopy, the Al–Cu–Mg alloy matrix has been found to contain
5.4 Cu, 1.5 Mg, 0.3 Si, 0.02 Mn, 0.4 Fe, 0.07 Zn, 0.2 Ti, 0.2 Cr,
and balance Al (all in wt.%).
The composites were processed by vacuum hot pressing
of the intimate mixtures of inert gas atomized powders of
Al–Cu–Mg alloy (Metal Powder Company Limited, Madurai)
and commercial ␣-SiC particles (Carborundum, India), followed
by extrusion at the ratio of 25:1 after soaking at 450 ◦ C for
0.5 h. The process of extrusion helps in a more uniform dis-
tribution of SiC particles. The steps involved in processing have
been described in detail elsewhere [15]. The average size of SiC
particles was 5 ␮m in the composite reinforced with 5 vol.%
SiC, and 50 ␮m in case of those with 15 and 25 vol.% SiC.
The as-extruded Al–Cu–Mg alloy–SiC composites were solu-
tion treated either at 495 ◦ C for 30 min, or at 504 ◦ C for 4 h and
quenched in ice-cold water, following the procedures for alloys
of similar compositions mentioned elsewhere [5,16]. The tem-
perature variation during each solution treatment was ±2 ◦ C.
The conditions of solution treatment represent two extremes of
the expected degree of dissolution of solute in the matrix. For
solution treatment, the specimens were placed inside the fur-
nace, after the required temperature was reached, and time was
measured only after the temperature stabilized. The cooling rate
is expected in the range of 475–480 ◦ C/s (K/s) during quench-
ing, assuming a momentary fall of 15–20 ◦ C in the time span
between exit from the furnace and dropping into the ice-cold
water. Some of the solution-treated samples were refrigerated
(≈−15 ◦ C) inside the freezer for further characterization, while
others were subsequently subjected to artificial aging at 191 ◦ C
for various lengths of time. For the purpose of aging, the sam-
ples were inserted into the furnace after the aging temperature
was reached, and only a momentary drop of roughly 20 ◦ C was
noticed during insertion. The Al–Cu–Mg alloy matrix will be
referred to as the “Al alloy” henceforth.
2.2. Characterization
The microstructures and particle–matrix interfaces of the
as-extruded and heat-treated samples were studied using sec-
ondary (SE) and back-scattered electron (BSE) imaging modes
on a JEOL JSM-5800 scanning electron microscope (SEM).
The chemical compositions of the different phases were inves-
tigated through spot and line-scan analyses on Link AN 10/55s
Energy Dispersive X-Ray (EDX) detector, attached to the SEM.
The particle sizes were measured on an optical microscope,
and from SEM micrographs using an image analysis software
along longitudinal and transverse directions, following the pro-
cedure recommended in the ASTM E112-96 standard [17]. The
interface area was measured from the sum of perimeters of the
SiC particles, or the total interface length per unit area, using
the intercept method proposed by Underwood [18]. To iden-
tify the phases formed during the aging heat treatments, X-ray
diffraction (XRD) studies were conducted on a Philips PW1840
diffractometer using Cu K␣ radiation. Electron transparent spec-
imens were prepared, for observations on the transmission
497
electron microscope (TEM), by mechanical thinning, followed
by jet polishing using an electrolyte comprising 33 vol.% HNO3
and 67% methanol in temperature range of −20 to −30 ◦ C. Sub-
sequently, TEM observations in bright and dark field imaging
modes accompanied by energy dispersive X-ray analyses were
carried out on a JEOL 2100 HRTEM operating at an acceleration
voltage of 200 kV.
In order to study the kinetics of aging, room temperature
microhardness measurements were performed on the matrix of
the composites in as-extruded and differently aged conditions
using a Vickers diamond indenter at loads of 10, 25, 50 or 100 gf
on a computerized LECO microhardness tester. At least 10 mea-
surements were recorded at each load for every specimen and
averaged. Vickers hardness of the differently aged specimens
was also measured using the 10 kg load.
The Al alloy–15 vol.% SiC composite sample, solution
treated at 500 ◦ C (500 ◦ C is almost the average of 495 and
504 ◦ C) for 0.5 h was electropolished in an electrolytic bath
containing phosphoric acid, ethanol, and water [19] and sub-
sequently etched to reveal the dislocations using an etchant
containing a mixture of HCl, HNO3 and HF [20]. The dislo-
cation density has been measured using image analysis of etch
pits, and compared with that obtained through theoretical calcu-
lations. A large area of the specimen could be observed without
the artifacts, generally introduced by deformation during TEM
sample preparation. The method of etching is usually applicable,
when dislocation density is relatively low.
3. Results and discussion
The microstructures of the Al–Cu–Mg alloy and its compos-
ites with 5, 15, and 25 vol.% SiC reinforcements, in as-extruded,
solution treated, or aged conditions have been studied with
emphasis on the nature and location of the precipitates, and
discussed in this section.
3.1. Microstructural examination
3.1.1. As-extruded condition
Fig. 1 is a typical SEM (SE) image of the as-extruded Al
alloy–25 vol.% SiC composite, showing a uniform distribution
of SiC particles, and is representative of the other composites
as well. SEM examination has indicated that the 15 or 25 vol.%
SiC reinforced composites also show a small fraction of particles
with size in the range of 5–10 ␮m, much less than the average
of 50 ␮m. The smaller size particles owe their origin to cracking
during extrusion. The typical XRD patterns of the as-extruded
composite with 5, 15 or 25 vol.% SiC particles (Fig. 2) show the
peaks of precipitate phases, CuAl2 and CuMgAl2 (S ), besides
those of Al and SiC. Fig. 3(a) and (b) shows the typical SEM
(BSE) images depicting the microstructure of as-extruded com-
posites with 5 and 25 vol.% SiC, respectively. The precipitates
could be observed distinctly in all the composites in the SEM
(BSE) images [Figs. 3(a) and (b)], as those appear bright due
to the higher atomic number of Cu or Fe, compared to those of
Al, Si or C. Fig. 3(a) and (b) also shows that a large fraction of
the particle–matrix interfaces has precipitates. EDX analyses of
498 S. Pal et al. / Materials Science and Engineering A 480 (2008) 496–505

Fig. 1. SEM SE image of Al alloy–25 vol.% SiC composite, showing a uniform

distribution of particles.

the spots on interfacial precipitates have shown the peaks of Cu,

Mg and Fe, as is obvious from the typical spectrum depicted in
Fig. 3(c). Of course, there are several particle–matrix interfaces
without any precipitate.

3.1.2. Solution-treated condition

Studies on the composites with the matrix solution treated
at 495 ◦ C have shown undissolved precipitates at some of the
particle–matrix interfaces, as is evident from the SEM (BSE)
image in Fig. 4(a). Quantitative analysis considering about 50
SiC particles has shown that almost 50% of the SiC parti-
cles exhibits undissolved precipitates at their interfaces with
the matrix. EDX spot analyses, with spectra resembling that
in Fig. 3(c), have confirmed the enrichment of solute, particu-
larly Mg, Cu or Fe at many of the Al–SiC interfaces shown in
the SEM (BSE) image of Fig. 4(a). Magnified view of the XRD
pattern from the sample solution treated at 495 ◦ C is shown in
Fig. 4(b), and depicts very tiny peaks of undissolved CuAl2 or
CuMgAl2 precipitates. Thus the presence of precipitates at the

Fig. 3. As-extruded Al alloy–SiC composites: SEM (BSE) images with: (a)

5 vol.%, and (b) 25 vol.% reinforcements, showing precipitates present in
the matrix and at interfaces, and (c) EDX spectrum of a precipitate at the
particle–matrix interface, showing the peaks of Al, Cu, and Fe.

Fig. 2. XRD pattern of as-extruded Al alloy–25 vol.% SiC composite, showing

the peaks of CuAl2 and CuMgAl2 precipitates.
 S. Pal et al. / Materials Science and Engineering A 480 (2008) 496–505
Fig. 4. Al alloy–25 vol.% SiC composite solution treated at 495 ◦ C for 0.5 h: (a)
SEM (BSE) image of the microstructure showing precipitates at the interface
and in the matrix; and (b) XRD pattern showing peaks of precipitates.
interfaces, and small peaks of CuAl2 or CuMgAl2 , appearing in
the XRD patterns is suggestive of incomplete dissolution dur-
ing solution treatment. EDX spot analysis from matrix of the
composite solution treated at 495 ◦ C for 0.5 h has also shown
Cu concentration as low as 2–3 wt.%, which is much less than
that in the bulk.
On the other hand, the concentration of Cu in the alloy matrix
on solution treatment at 504 ◦ C has been found to be almost
similar to the bulk composition. Fig. 5 is an SEM (BSE) image
of the composite with 15 vol.% SiC particles solution treated at
504 ◦ C for 4 h, showing undissolved precipitates at a very limited
number of particle–matrix interfaces. EDX spot analyses have
confirmed the enrichment of Mg and Fe in the coarse precipitates
at the SiC–matrix interfaces in the alloy solutionized at 504 ◦ C
for 4 h. Quantitative analysis considering about 50 SiC particles
in the SEM (BSE) images, has shown precipitates at about 10%
of the interfaces. Thus a comparison of the SEM (BSE) images
in Figs. 4(a) and 5 shows that the undissolved precipitates occur
less frequently in the matrix and at interfaces, compared to that in
samples solution treated at 495 ◦ C for 0.5 h, confirming a much
larger extent of solute dissolution in case of the former. The
499
Fig. 5. SEM (BSE) image showing the microstructure of the Al alloy–25 vol.%
SiC composite solution treated at 504 ◦ C for 4 h.
dissolution of precipitates in the composites solution treated at
504 ◦ C for 4 h is closer to its completion than in those solution
treated at 495 ◦ C for 0.5 h. It is imperative that both the time and
temperature of solution treatment have an effect on the degree of
dissolution. The root mean square diffusion distance of a given
solute atom under non-steady state condition is proportional to
Dt, where D is the diffusion coefficient and t is the time [21]. The
term, D is related to the absolute temperature by an Arrhenius
type relation. In the present study, the difference in temperature
is only 9 ◦ C, but time of solution treatment at the 504 ◦ C is eight
times that at 495 ◦ C. The effects of temperature and time could be
distinguished from one another, only through further systematic
studies on solution treatment, keeping one of those unchanged
and the other varying.
Negligible solubility of Fe in Al does not allow dissolution
at either of the solution treatment temperatures. In addition, the
atoms of Mg have a strong tendency to segregate at interfaces, as
confirmed through EDX spot analyses. The solute atoms tend to
segregate at the interfaces in the composites in solution-treated
condition, since the free energy is reduced by Gibbs adsorp-
tion. In certain other studies, the surfaces of SiC particles have
also provided preferred sites for the nucleation of intermediate
precipitates [22,23]. At high cooling rates used in this study,
the possibility of formation of intermediate precipitates is also
unlikely [24].
The density of dislocations appearing as etch-pits in the
microstructure of the Al alloy–15 vol.% SiC composite (Fig. 6)
with matrix in solution-treated condition has been found to be
7 × 1011 m/m3 .
3.1.3. Aged condition
Fig. 7(a–c) shows the SEM (BSE) images of the Al alloy–5,
15, and 25 vol.% SiC composites, over-aged after solution treat-
ment at 495 ◦ C for 0.5 h. A large number of the SiC–matrix
interfaces show precipitates enriched in Cu, Mg or Fe. Since the
Al alloy–SiC interfaces also have a higher density of dislocations
compared to that in the matrix, in addition to a higher degree of
interfacial solute enrichment, the nucleation and growth of pre-
500 S. Pal et al. / Materials Science and Engineering A 480 (2008) 496–505

Fig. 6. SEM (SE) image of the Al alloy–15 vol.% SiC composite, showing etch-
pits for dislocations present.

cipitates at and near interfaces is usually preferred during aging.

The XRD patterns from the underaged or overaged Al-alloy–SiC
composite have shown the peaks of CuAl2 and CuMgAl2 phases
as expected. The ternary Al–Cu–Mg phase diagram [25] shows
equilibrium between ␣-Al, ␪ (CuAl2 ), and S (CuMgAl2 ) phases.
Fig. 8(a) and (b) is the typical bright and dark field TEM
images of the Al alloy in under-aged condition, showing rod-
shaped precipitates of the CuMgAl2 phase. The selected area
diffraction (SAD) pattern from the area with the precipitates, is
shown as inset in the dark field TEM image of Fig. 8(b). The
diffraction spots are streaked perpendicular to the rod-shaped
precipitates. On examination of the bright and dark field TEM
images with reference to the diffraction pattern, it is obvious
that the axis of the CuMgAl2 rods are aligned in the orthogonal
1 0 0 direction of the matrix. The 1 0 0 orientation of the
rod-shaped CuMgAl2 precipitates in the TEM images [Fig. 8(a)
and (b)] agree with the observations previously reported in the
literature [26–29]. Fig. 8(c) is a typical diffraction pattern from
a larger area confirming the presence of CuMgAl2 as well as
CuAl2 precipitates in under-aged samples.

3.2. Theoretical analysis of interface area and

inter-particle spacing

The integrity of SiC–matrix interfaces and inter-particle spac-

ing strongly affect the dislocation density, which is known to
affect the aging behaviour in turn, as has been mentioned in
Section 1. Assuming the particles to be equiaxed or sphrerical,
the net particle–matrix interface area per unit volume, AI (ignor-
ing the intermetallic precipitates in the alloy matrix) has been
calculated using the relation [30]:
6Vp
AI =
d a function of volume fraction and particle size. Assuming the
where Vp is the volume fraction of particles and d is the particle
size. Since the SiC particles are irregularly shaped, the calcu-
lated area of interfaces per unit volume is only approximate.
The average spacing between the dispersed SiC particles is also
Fig. 7. SEM (BSE) images showing interfacial segregation: (a) Al alloy–5 vol.%
SiC composite after solution treatment and artificial aging for 16 h; (b) Al
alloy–15 vol.% SiC composite after solution treatment and artificial aging for
48 h; and (c) Al alloy–25 vol.% SiC composite after solution treatment and
artificial aging for 16 h.
(1)
particles to be equiaxed, the inter-particle spacing is calculated
using the following relationship [31]:
λ = 0.77d(Vp )−0.5 (2)
 S. Pal et al. / Materials Science and Engineering A 480 (2008) 496–505 501

Fig. 8. TEM micrographs of underaged alloy: (a) bright and (b) dark field images showing lath-shaped precipitates of CuMgAl2 with the SAD pattern shown as the
inset; and (c) SAD pattern from a larger area showing rings representing polycrystalline Al, CuAl2 , and CuMgAl2 phases. The dark field image has been recorded
using the reflection, g = [2 0 0].

Table 1
The measured and calculated values of the particle-size, particle–matrix interface area, inter-particle spacing, and calculated value of the dislocation density in the
matrices of as-extruded Al alloy–SiC composites
Volume fraction of SiC (%) Particle size (␮m) Interface area (m2 /m3 ) Inter-particle spacing (␮m) Dislocation density, B (m/m3 )

Calculated Measured Calculated Measured

5 05 6.0 × 104 1.1 × 103 17.2 14.2 3.7 × 1011

15 50 1.8 × 104 4 × 104 99.4 95.7 1.2 × 1011
25 50 3.0 × 104 7 × 104 77.0 75.5 2.3 × 1011
502 S. Pal et al. / Materials Science and Engineering A 480 (2008) 496–505
Fig. 9. Plots showing the variation of matrix microhardness with time of aging for indentation loads of 10, 25, 50, and 100 gf in case of the (a) Al alloy, and composites
with (b) 5 vol.%, (c) 15 vol.%, and (d) 25 vol.% SiC particles. The solution treatment was carried out at 495 ◦ C for 0.5 h.
Table 1 shows the calculated and experimentally measured
values of interface area per unit volume and the average inter-
particle spacing, obtained for composites with the different SiC
particle sizes. The values of experimentally measured interface
area are similar to those calculated from Eq. (1), except in case
of the composites reinforced with 5 vol.% SiC particles with
5 ␮m average size. It may be noted that Eq. (1) was derived,
considering spherical particles, while the SiC particles are irreg-
ular in shape. Smaller the particle size, larger is the surface
area to volume ratio. As a result, the deviation of experimen-
tally determined value of surface area from that evaluated using
Eq. (1) is maximum for the smallest particle size of 5 ␮m. On
the other hand, the experimentally determined values of inter-
particle spacing have the same order of magnitude and are very
close to those obtained through calculations using the relation-
ship (2). The composite with 5 vol.% SiC particles having the
average size of 5 ␮m has shown the smallest inter-particle spac-
ing, which is close to the 1/5th of that between the particles in
the other two composites.
The density of dislocations with Burgers vector, b, generated
as a result of quenching from solution treatment temperature
(500 ◦ C) to 0 ◦ C (ice-cold water) has been calculated using the
following Eq. [2]:
(BVp ε)
ρ=
bt(1 − Vp )
where B is a constant having value between 4 and 12, ε is the
strain due to mismatch in CTE = (T) (CTE), and t is the small-
est dimension of the reinforcement. The calculated dislocation
densities in the Al alloy–SiC composites, shown in the last col-
umn of Table 1, have the same order of magnitude in spite of the
different sizes and volume fractions of reinforcement particles,
and increase with decreasing inter-particle spacing. The order
of magnitude of the theoretically evaluated dislocation densities
agrees well with that of experimental measurement, mentioned
in Section 3.1.2.
3.3. Isothermal ageing kinetics
Fig. 9(a–d) shows the plots depicting the variation of matrix
microhardness with time of aging obtained using indentation
loads ranging between 10 and 100 gf, for the composites hav-
ing 5, 15, and 25 vol.% SiC particles, respectively, after solution
treatment at 495 ◦ C for 0.5 h. It is clear from the microhard-
ness data, that the time taken for peak aging of the Al alloy
and all the composites solution treated at 495 ◦ C are 3 and 5 h,
respectively. Fig. 10(a) and (b) shows the plots depicting the
aging kinetics (based on microhardness measurements at load
of 100 gf) of the matrix in Al alloy and its composites with 5,
15, or 25 vol.% SiC particles, previously subjected to solution
treatment at 495 ◦ C for 0.5 h and 504 ◦ C for 4 h, respectively.
The peak-aging condition could be reached in the monolithic
alloy and the composites solution treated at 504 ◦ C for 4 h after
4 and 6 h of aging, respectively. There is a very large scatter in
(3)
the microhardness of the matrix, which could be due to contact
of the indenter with SiC particles in the sub-surface locations,
and a locally inhomogeneous distribution of reinforcements and
precipitates. Different loads have been used to determine the
microhardness for better statistics and reliability, and the time
 S. Pal et al. / Materials Science and Engineering A 480 (2008) 496–505 503

Fig. 11. Plots showing the variation of hardness of the Al alloy and its com-
posites, with duration of aging after solution treatment at 504 ◦ C for 4 h. The
hardness tests were carried out using a load of 10 kgf.

reduced kinetics of aging observed in the Al alloy–SiC compos-

ites is in contrast to what has been reported for most of the times
in the past [3–13].
The slower kinetics of aging in the Al alloy–SiC composites
compared to that in the alloy, could be due to one or more of the
following mechanisms:

(I) The presence of SiC particles leads to a reduction in the

Fig. 10. Plots showing variation of matrix microhardness with time of aging,
after solution treatments at: (a) 495 ◦ C for 0.5 h, and (b) 504 ◦ C for 4 h, for the Al
alloy and its composites with 5, 15, 25 vol.% SiC particles. The microhardness
tests were carried out using a load of 100 gf.
for reaching peak hardness has been found to be the same for
all. A smaller load gives a more localized microhardness with-
out interference from the neighbouring or sub-surface regions.
On the other hand, a larger load would cause a larger indenta-
tion covering a wider area. The variation of Vickers hardness of
the Al alloy and the composites, solution treated at 504 ◦ C for
4 h with time of aging is shown in Fig. 11. The aging kinetics
and time for peak aging determined through measurement of the
microhardness [Fig. 10(b)] and Vickers hardness (Fig. 11) agree
well.
It is obvious that the aging kinetics of the Al alloy is faster
than that of the composites for both the temperatures of solution
treatment [Fig. 9(a–d), 10(a and b), and 11]. Fig. 10(a) shows
that for solution treatment at 495 ◦ C for 0.5 h, the rate of increase
in hardness with time of aging of the alloy is the highest, fol-
lowed by that of composite with 5 vol.% SiC particles, while
the composites with 15 and 25 vol.% SiC particles show a more
gradual increase in hardness. The rise to peak hardness in less
time is suggestive of the faster kinetics in the initial stages. The
volume fraction of GP zones, which follows from the lower
vacancy concentration in the composite, compared to that
in the unreinforced alloy [4,11,14,32]. The vacancy con-
centration is lower in the composites due to the large area
of particle–matrix interfaces, acting as vacancy sinks. It is
intuitive that the lower vacancy concentration in the matrix
of the composite compared to that in the Al alloy is respon-
sible for retarding the formation of GP zones. It has been
argued in a previous study [11], that the initial retardation
of aging kinetics due to lower density of GP zones may
affect the remaining steps of the aging sequence [14]. On
the other hand, a higher concentration of vacancies in the
Al alloy leads to a greater density of GP zones, enhancing
the aging kinetics in the initial stages. In a related study
on the aging kinetics of the 2024 Al–9 or 14 vol.% Al2 O3
fiber composites, Cen and Chao [32] have shown negligi-
ble effect of the reinforcement phase on the aging kinetics,
and explained it on the basis of reduced vacancy concen-
tration, and lower GP zone density restricting the S phase
formation as well.
(II) Excessive segregation of alloying elements at the Al–SiC
interfaces and presence of undissolved, coarse precipi-
tates causing depletion of solute inside the matrix, found
particularly on solutionizing at 495 ◦ C for 0.5 h, leads to
lower supersaturation of solute. A lower degree of super-
saturation would reduce the chemical driving force for
precipitation in the composites. Previously, Hunt et al. [33]
have reported retardation of S precipitation in matrix of
the composite, attributing its cause to higher intermetallic
504 S. Pal et al. / Materials Science and Engineering A 480 (2008) 496–505
content in the composite compared to that in the alloy, and
incomplete solutionizing, which makes solute unavailable
for S formation.
(III) The difference in kinetics of aging is caused by S pre-
cipitation at dislocations, density of which plays a critical
role. The dislocation density in the composites may be
insufficient for enhancement of kinetics of aging:
(a) The experimentally determined and calculated dislo-
cation density of the order of 1011 m/m3 (Table 1)
is dictated by the inter-particle spacing, and is simi-
lar to those (calculated) in some of the liquid phase
sintered Al alloy–SiC composites [14], with coarse
particle sizes and low volume fraction, which have
also shown retarded or unaltered aging kinetics, with
respect to that of the Al alloy. The low dislocation
density generated by the smaller thermal expansion
mismatch between Al and Al2 O3 has been cited as
one of the reasons for the little effect of reinforcement
on aging kinetics of the composite [32].
(b) Static recovery through the annihilation of dislocations
of opposite sign is likely to set in and reduce the dislo-
cation density inside the composites at the temperature
of aging, which is about half the absolute melting point
of pure Al. Unlike precipitation, annihilation of dislo-
cations of opposite sign in a dense network reduces the
strain energy of the system, and does not face an acti-
vation barrier. There must be a competition between
the recovery process and precipitation, with the faster
process affecting the hardness more.
The present study shows that aging kinetics of the composite
with respect to that of the unreinforced alloy may not be always
faster. At the same time, average microhardness of the matrix
in the composite with 5 vol.% SiC is the highest for both the
solution treatments, which can be best explained on the basis
of the much smaller inter-particle spacing, finer particle size,
and greater dislocation density (Table 1), compared to others.
Smaller distance between the SiC particles and higher density
of dislocations is expected to reduce spacing between the precip-
itates, and increase the microhardness of the matrix. In addition,
its lower total area of the particle–matrix interfaces per unit vol-
ume probably reduces the effect of interfacial segregation of the
alloying elements, increasing the volume fraction of precipitates.
Among the samples solution treated at 495 ◦ C for 0.5 h, the
alloy has shown higher average and peak hardness compared to
the composites with 15 or 25 vol.% SiC, which is contrary to
the expectation. In contrast, on aging after solution treatment at
504 ◦ C for 4 h, the alloy has shown lower hardness compared
to the composites, which is usually expected. The much higher
hardness of the alloy, besides faster kinetics of aging in compari-
son to composites with 15 or 25 vol.% SiC for solution treatment
at 495 ◦ C, implies that volume fraction of precipitates is less
in the latter. Solutionizing at 495 ◦ C was insufficient for com-
plete dissolution of alloying elements segregated at the Al–SiC
interfaces.
Again the less time required for peak aging in case of the
alloys and composites solution treated at 495 ◦ C for 0.5 h com-
pared to that at 504 ◦ C for 4 h is probably because the difference
in the Cu concentration of the matrix between its solution treated
and equilibrium condition is less in case of the former. In addi-
tion, the peak hardness of the alloy and composites on aging
after solution treatment at 504 ◦ C for 4 h is more than those of the
samples aged after solutionizing at 495 ◦ C for 0.5 h [Fig. 10(a)
and (b)], which again can be explained on the basis of the lower
volume fraction of precipitates in case of the latter caused by
incomplete dissolution of alloying elements. It is thus obvi-
ous that both the microhardness under the condition of peak
aging and time required for reaching that depend on the time
and temperature of solution treatment.
Although the rate of increase in hardness with aging time
varies, yet the time required for peak aging of the composites
appears to be independent of size or volume fraction of SiC
particles, which is in agreement with the observations of Pan
and Cheng [16], and Suresh et al. [6]. Suresh et al. have shown
that once a threshold density of dislocations is reached, further
increase in the SiC volume fraction has little effect on the aging
kinetics.
4. Conclusions
The artificial aging behaviour of the powder metallurgy
processed Al–Cu–Mg alloy and the matrix in its composites rein-
forced with 5, 15, or 25 vol.% SiC particles has been studied after
incomplete or complete solutionizing treatments at 495 ◦ C for
0.5 h, or 504 ◦ C for 4 h, respectively. The following conclusions
may be drawn from the present study:
Precipitates of CuAl2 , CuMgAl2 and those enriched in Fe
have been observed in the alloy matrix as well as at SiC–matrix
interfaces in the composites in as-extruded and aged conditions.
The CuMgAl2 precipitates appear rod shaped, and aligned along
the orthogonal 1 0 0 directions. The composite samples solu-
tion treated at 495 ◦ C for 0.5 h have a larger fraction of the
Al–SiC interfaces with undissolved precipitates and enrichment
of alloying elements, than those solutionized at 504 ◦ C for 4 h.
The time for peak aging of the Al alloy and its composites
with 5, 15 or 25 vol.% SiC particles, solution treated at 495 ◦ C
for 0.5 h and aged at 191 ◦ C has been found to be 3 and 5 h,
respectively. On the other hand, hardness of the alloy and com-
posites solution treated at 504 ◦ C for 4 h has peaked on artificial
aging for 4 and 6 h, respectively. Again higher peak hardness has
been observed on aging of samples after solution treatment at
504 ◦ C for 4 h, than those aged after solutionizing at 495 ◦ C for
0.5 h. The difference in age-hardening behaviour based on the
time and temperature of solution treatment has been attributed to
the larger concentration of Cu atoms in solid solution available
after solution treatment at 504 ◦ C for 4 h, giving rise to a higher
volume fraction of precipitates.
The composite with 5 vol.% SiC particles has shown the high-
est hardness, irrespective of the solution treatment condition,
probably due to the lowest inter-particle spacing, and a higher
volume fraction of precipitates among the composites studied.
For solution treatment at 495 ◦ C for 0.5 h, the peak-age hardness
of the Al alloy is greater than that of the composites with 15 or
25 vol.% SiC particles, due to the lower volume fraction of pre-
 S. Pal et al. / Materials Science and Engineering A 480 (2008) 496–505
cipitates in case of the latter. On the other hand, the peak-age
hardness of the alloy is less than that of the composites on aging
after solutionizing at 504 ◦ C for 4 h.
The slower kinetics of aging in the matrix of composites is
attributed to the lower concentration of vacancies, inadequate
dislocation density, as well as extensive interfacial segregation
of alloying elements, such as Cu, Al and Fe, and undissolved
precipitates at the particle–matrix interfaces causing the deple-
tion of Cu or Mg in the matrix, and reduction in degree of solute
supersaturation inside the matrix.
Acknowledgement
The technical assistance rendered by Mr. B.P. Mirdya and
Mr. Bijon Das with XRD, Mr. D.N. Mahato and Mr. A.K. Jha
with heat treatment, Dr. R. Maiti and Mr. Sana of SEM, Mr.
Ranadhir Bose with TEM, and Mr. B.C. Jena and Mr. B. Deb in
Metallography Laboratory is gratefully acknowledged.
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