Materials Science & Engineering A 644 (2015) 7984

Contents lists available at ScienceDirect

Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Inuence of interfaces on the mechanical behavior of SiC

particulate-reinforced AlZnMgCu composites
Jingya Song a, Qiang Guo a,n, Qiubao Ouyang a, Yishi Su a, Jie Zhang a, Enrique J. Lavernia b,
Julie M. Schoenung b, Di Zhang a,n
a
b

State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, 800 Dongchuan Road, Shanghai 200240, China
Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616, USA

art ic l e i nf o

a b s t r a c t

Article history:
Received 29 April 2015
Received in revised form
17 July 2015
Accepted 17 July 2015
Available online 18 July 2015

In particulate-reinforced metal matrix composites (MMCs), geometrically necessary dislocations (GNDs)

form in the vicinity of reinforcement/matrix interfaces. In this study, the hardness distribution across the
interface was studied using nanoindentation with high spatial resolution, for composites treated under
different aging conditions. The size of the GND punched zone, as determined from the hardness measurement, was found to be in agreement with that estimated by transmission electron microscopy (TEM).
Mechanical characterization of bulk composites revealed a reduction in failure strain with decreasing
punched zone size, while the strength of the composites was found to depend more on the intrinsic
strength of the matrix alloy. These observations were interpreted in terms of the load transfer capacity
between the matrix and reinforcement through the interface.
& 2015 Elsevier B.V. All rights reserved.

Keywords:
Metal matrix composites
Nanoindentation
Aging
Interface structure
Dislocation distribution

1. Introduction
Particulate-reinforced metal matrix composites (MMCs) are
ideally suited for many structural and functional applications because of their high specic strength and stiffness, isotropic properties and relatively simple processing as compared with monolithic materials and conventional ber-reinforced composites [1
4]. Among the parameters that may affect the mechanical performance of these composites, such as the reinforcement particle size
[5,6], distribution [7] and volume fraction [3,8], the properties at
and in the vicinity of particlematrix interfaces play a critical role
[9,10]. A strong interface would usually allow for effective load
transfer from the matrix to the reinforcement, leading to improved
strength, stiffness and resistance to environmental attack [11]. The
interfacial properties have also been found to determine the failure mode of the composite [1,2,4], where failure initiated by interfacial debonding is likely to occur when the interface is weak.
During the processing of particulate-reinforced MMCs, geometrically necessary dislocations (GNDs) typically form in the
metal matrix close to the particlematrix interface, as a result of
the residual stress caused by the mismatch in the coefcients of
thermal expansion (CTE) between particle and matrix [2,5]. The
n

Corresponding authors.
E-mail addresses: guoq@sjtu.edu.cn (Q. Guo), zhangdi@sjtu.edu.cn (D. Zhang).

http://dx.doi.org/10.1016/j.msea.2015.07.050
0921-5093/& 2015 Elsevier B.V. All rights reserved.

presence of GNDs, which reportedly hardens the matrix alloy in

the vicinity of the interface, has been conrmed experimentally
[1,6], as well as predicted on the basis of numerical models [5,12].
The nature of the regions populated with GNDs around the particle in the metal matrix ("dislocation punched zone") is dependent on the size, morphology, and distribution of the reinforcement particles [5,13], as well as on the processing and heat
treatment parameters [14]. The inuence of these regions on
mechanical behavior is twofold. On one hand, these regions are
considered to provide the main strengthening mechanism in
particulate-reinforced MMCs [5,14,15]. On the other hand, they
also give rise to rapid hardening saturation of the matrix at low
external strain values, resulting in the degradation in the composites' ductility and fracture toughness [10,16]. In addition to their
inuence on mechanical properties, for composites whose matrix
alloy is age-hardenable, the existence of the GNDs and the associated dislocation-punched zones have been reported to signicantly facilitate the aging kinetics of the composites during
heat treatment, where the GNDs were proposed to serve as heterogeneous nucleation sites for precipitate formation [17].
Although extensive experimental and theoretical research have
been carried out to study the size and distribution of dislocation
punched zones as a function of the conguration of the reinforcement particles, and their effect on the aging response of the
composites, inspection of the published literature show that there
are limited studies devoted to clarifying how such regions would

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J. Song et al. / Materials Science & Engineering A 644 (2015) 7984

evolve upon heat treatment, and correlating their evolution with

the mechanical properties of the corresponding bulk composites.
In this study, using the widely-used silicon carbide particulate
(SiCp) reinforced Al alloy as the model system, the hardness distribution across the SiCp/Al interface with high spatial resolution
was characterized, and subsequently the size of the dislocation
punched zones was estimated, for composites treated under different aging conditions. The range that GNDs extended out from
the interface in different composite samples, as determined from
transmission electron microscopic (TEM) analysis, was found to
agree with the hardness measurements. The correlation between
bulk mechanical performance of the composites and the GNDs
punched zone size was interpreted in terms of the load transfer
capability between the matrix and reinforcement through the
interface.

2. Experimental methodology
SiCp particles with an average size of 30 m and an engineering 7A04 AlZnMgCu alloy (nominal concentration: Zn: 5.07.0,
Mg: 1.82.8, Cu: 1.42.0, Mn: 0.20.6, Cr: 0.10.25 and Al: balance,
in weight percentage) were selected as the starting raw materials.
The composite (SiC 14 vol%) was fabricated using the stir casting
technique [18], where the particles were added into the molten
aluminum alloy, and were dispersed uniformly before the mixture
was cast into ingots. Then, the composite ingots were extruded
into 12 mm-diameter bars with an extrusion ratio of 9:1 and then
10:1. Subsequently, the composite bars were solution heat-treated
at 470 C for 60 min, followed immediately by a water quench. To
prepare composite samples with different aging conditions, they
were annealed at 120 C for 12, 24, and 48 h. The tensile properties
of the bulk composites were measured using an INSTRON 8871
tensile tester at a nominally constant displacement rate of 1 mm/
min at room temperature, on specimens with 2 mm by 2 mm
square cross sectional area and 10 mm in gauge length, which
were machined from the extruded rods.
Prior to the nanoindentation tests, the specimen surface was
carefully prepared using conventional metallographic techniques
and subsequently polished with rst 2.5 mm and then 1 mm diamond abrasive [19]. Electron backscattered diffraction (EBSD)
measurements were carried out on the ion polished surfaces

(model of the ion polisher: Gatan Ilion) parallel to the extrusion

direction of the composite samples, to characterize the size and
orientation of the grains adjacent to the reinforcing SiC particles.
Then, random particles were selected, around which arrays of indentations in various directions were made across the particle/
matrix interface, as shown in Fig. 1. The objective of these measurements was to ascertain if the magnitude of hardness and/or its
evolution is dependent of the grain size, grain orientation or the
shape and dimension of the particles. Indents were also made at
various indentation depths (from 120 nm to 250 nm) and spacings
between neighboring indents (from 1 mm to 5 mm) in order to
investigate the possible effects of the roughness of the polished
surface on indentation results. Sharp particle corners were intentionally avoided in the tests, because they have been reported
to cause severe stress concentration and subsequently much
higher hardness values for the matrix near the interface, as compared with those measured from matrix alloys close to at edges
of the particles [4,20]. All indentation measurements were done
using an Agilent G200 XP Nanoindenter equipped with a Berkovich tip, in displacement-controlled mode, at a nominally constant
strain rate of 0.05 s
1. The continuous stiffness measurement
(CSM) [21] with 2 nm oscillation magnitude and 45 Hz oscillation
frequency was deployed to monitor the change in contact stiffness
during indentation. Hardness was calculated using the Oliver
Pharr method [21]. Optical microscopy (OM) and scanning electron microscopy (SEM) by an FEI Quanta SEM were used to observe the indents and their arrays, and the microstructure of the
composites was characterized by a JEOL 2100 TEM.

3. Results and discussion

3.1. Hardness variation in the vicinity of interface
The magnitude of hardness and its evolution across the particle/matrix interface were found to show little dependence on the
grain size and orientation (Fig. 1), which is consistent with the
isotropic texture of the Al matrix reported for SiCp-reinforced Al
matrix composites with a high SiCp concentration (410 vol%)
[22]. Moreover, it was found that the variation in hardness values
with varying indentation depth is within 5%, indicating that surface roughness as a result of the polishing procedures had a

Fig. 1. (a) Scanning electron microscope (SEM) image and (b) electron backscattered diffraction (EBSD) image (in the same eld of view with (a)) of indent arrays (represented by arrows) across the SiCp/Al interface in various directions.

J. Song et al. / Materials Science & Engineering A 644 (2015) 7984

Fig. 2. SEM image of an indentation array made in the 24 h-aged composite, with
120 nm indentation depth and 1 m indentation spacing.

negligible effect on indentation hardness. In general, a shallower

indentation would inevitably result in a smaller lateral dimension
of the indents, allowing for a smaller indent spacing and subsequently a more accurate estimate on the hardness variation and
punched zone size. However, owing to the roughness of the polished sample surface, it was found that for indentation depths
smaller than 100 nm good convergence on the calculated hardness
was not achieved, and accordingly, a 1 mm spacing between
neighboring indents and a 120 nm maximum indentation depth
were used in the following experiments, to ensure a high spatial
resolution of the indents as well as the representativeness of the
trend in hardness across the interface, as illustrated in Fig. 2. For
each sample, at least 4 arrays of indentation across different SiC
particles were conducted, and more than 20 individual indents
were made for each indentation array, covering the entire range
from the SiC particle (characterized by a plateau in hardness corresponding to SiC), across the SiC/Al interface, and nally to the
matrix alloy (characterized by a plateau in hardness corresponding
to the matrix).
Fig. 3(a) shows a set of representative data corresponding to
the hardness distribution across the interface for samples treated
under 4 different processing conditions (as-extruded, aged at 12,
24, and 48 h). The origin on the horizontal axis (x 0) corresponds
to the approximate position of the interface, right of which (x 40)
corresponds to the Al matrix, and left of which (xo 0) corresponds
to the SiC particle. In the xo 0 regime (particle), the hardness
plateau has a magnitude of  40 GPa, corresponding to that of the
particle. In the x 40 regime (matrix), the magnied view as shown

81

in Fig. 3(b) demonstrates that, for the indentations made more

than 6 mm away from the SiC/Al interface, the hardness values
for all the samples reach a plateau, corresponding to the intrinsic
hardness of the matrix alloy. In this region, the sample aged for
24 h possesses the highest hardness of 2.86 70.16 GPa, followed
by the sample aged for 48 h (2.72 70.15 GPa), the sample aged for
12 h
(2.23 70.01 GPa),
and
the
as-extruded
sample
(1.96 70.04 GPa). Therefore, the samples aged for 12, 24, and 48 h
are hereafter denoted as underaged, peak-aged, and overaged
samples, respectively. Fig. 3(b) also demonstrates that, for the asextruded and underaged samples, the hardness generally shows a
gradual reduction from the interface towards the matrix, and the
width of this transition region can be estimated to be  6 mm for
both cases. For the peak-aged and overaged counterparts, in
comparison, the transition is rather sharp, and the widths are
shown to be smaller than  2 mm, i.e., comparable to the spacing
between neighboring indents. The punched zone size, together
with the hardness of the matrix under different aging treatments,
is documented in Table 1.
3.2. Microstructure evolution during aging process
It has been proposed that the width of the hardness transition
region is a measure of the dislocation punched zone size associated with the GNDs formed upon the processing of metal matrix
composites [15]. Therefore, a high density of dislocations is expected to be present in this region, which is exactly what has been
observed. Fig. 4 shows the representative TEM images on the SiC/
Al interface taken under two beam conditions, from [011] zone
axis and [002] diffraction vector, for the 4 sets of samples processed under different heat treatments. At least 3 TEM images
were used for each sample to estimate the width of its corresponding punched zone size. As demonstrated, the dislocation
punched zone extends 24 mm into the matrix alloy for composites
in the as-extruded and underaged states, and are limited to 1
2 mm for the peak-aged and overaged samples. This is in qualitative agreement with the results obtained from the hardness
measurement. However, it should be noted that the punched zone
size estimated from the TEM images only represents its lower limit
because not all dislocations are visible under this particular diffraction condition. This is especially true for the as-extruded
sample, where the size of the grains immediately adjacent to the
SiC particles was only about 2 mm (Fig. 4a), making the dislocations
in the neighboring grains unobservable, so its punched zone size
may be substantially underestimated. Also, careful examination at
the SiC/Al interfaces in Fig. 4 reveals that dislocations adjacent to

Fig. 3. (a) Variation of indentation hardness across the SiCp/Al interface for composites treated under 4 different processing conditions; (b) zoomed-in rendition of the boxed
region in Fig. (a).

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J. Song et al. / Materials Science & Engineering A 644 (2015) 7984

Table 1
Tensile properties, indentation properties, and structural parameters of the SiCp/Al composite samples treated under different processing conditions.
Condition

Punched zone size (m)

Matrix hardness (GPa)

Strength (MPa)a
sy
smatrix

sL-T (MPa)

Failure strain (%)

Average grain size (m)

sL-T/sy (%)

As-extruded
Underaged
Peak-aged
Overaged

6
6
o 2
o 2

1.96 7 0.04
2.23 7 0.01
2.86 7 0.16
2.727 0.15

370
480
520
496

25
87
17
18

6.2
4.3
2.6
1.9

4
 51
 27
 65

6.8
18.1
3.3
3.6

345
393
503
478

sy: 0.2% offset yield strength of the composite; smatrix: 0.2% offset yield strength of the Al matrix.

the interface are not uniformly distributed, and regions of slightly

different diffraction contrast can be observed. In general, microstructural features, such as grain boundaries, interfaces, precipitates and stacking faults, can all affect the distribution of dislocations, and subsequently the formation and morphology of
substructures. On the other hand, as mentioned previously, dislocations have been reported to serve as heterogeneous nucleation
sites for precipitate formation in age-hardenable alloys [17].
Therefore, the presence of SiC/Al interfaces as well as the precipitates introduced by aging, may have given rise to substructure
formation (i.e., the different diffraction contrast) in the vicinity of
the interface, as observed in Fig. 4. Moreover, it is important to
point out that the indentation depth (120 nm) and the associated
lateral radius of the indents (  500 nm [23]) is signicantly (at
least a factor of 8) smaller than the average grain size of the Al
matrix in all samples (465 m, see Table 1, Column 8). Yang and
Vehoff [24] reported that if the grain size of pure Ni is more than
3.5 times the lateral radius of the indents, the plastic zone caused
by the indentation conducted at the center of the grain would be
limited inside the grain and would not interact with the grain
boundaries. This is generally the case in the present experiments.

Therefore, on the whole, the hardness evolution in the vicinity of

the SiC/Al interface was unlikely to be caused by the variation in
the Al grain size, and should solely be the result of the GNDs.
During cooling from the high temperature processing of stir
casting and extrusion deformation, the CTE mismatch between the
particle and the matrix alloy is likely to cause residual stress in the
vicinity of the interface [1], and subsequently a considerable increase in the dislocation punched zone size in the as-extruded and
underaged samples. On the other hand, the reduction in the
punched zone size along with the progression of precipitation, in
the peak-aged and overaged samples, can be explained in terms of
the aging kinetics affected by the presence of GNDs. It is well
known that, in an AlZnMgCu alloy, the precipitation sequence
upon articial aging can be generally listed as GuinierPreston
(GP) zones- and (MgZn2)-S (Al2CuMg) phases [25]. In related studies, Cantrell et al. [26] argues that the nucleation and
growth of precipitates near matrix dislocations may cause the
dislocations to bow under the action of local precipitatematrix
coherency stresses; it has also been reported that when the precipitates become larger in size with increasing aging time, they
may promote the rearrangement of dislocations and the

Fig. 4. Transmission electron microscopy (TEM) images of the reinforcement/matrix interface, from SiCp/Al composite samples treated under different processing conditions: (a) as-extruded state; (b) underaged state; (c) peak-aged state; and (d) overaged state.

J. Song et al. / Materials Science & Engineering A 644 (2015) 7984

movement of subgrain boundaries [27]. Furthermore, GNDs have

been proposed to signicantly facilitate the aging kinetics by serving as heterogeneous nucleation sites for precipitate formation
[2]. All these effects may lead to a decrease in the GND density and
the associated punched zone size, as has been observed here in the
TEM images.
EBSD measurements show that the average grain size of the
matrix alloy changes from 51 m for the underaged sample, down
to 27 m for the peak-aged sample, and again up to 65 m for the
overaged sample (Table 1). This evolution was mostly likely the
result of recrystallization upon aging treatment. Recrystallization
of deformed alloys at aging temperatures has been reported, but
the kinetics can be quite slow. For example, Jones and Hymphreys
[28] reported the complex interaction between precipitate formation and recrystallization in AlSc alloys, where precipitation
was found to precede, follow or occur concurrently with recrystallization, depending on the deformation processing conditions of the alloy. It was also found that it takes over 20 h for the
Al0.02 Sc wt% alloy to get fully recrystallized at 280 C. Liu et al.
[27] reported recrystallization during aging for a rapidly solidied
CuCrZrMg alloy, and the dispersed precipitates were reported
to retard recrystallization. In the solution heat-treated Mg9Al
1Zn alloy, which was later subject to severe plastic deformation,
recrystallization was observed with sufcient aging time ( 410 h)
at 180 C [29].
Considering the evolution of the average grain size of the Al
matrix as demonstrated in Table 1, we propose that the nucleation
and growth of recrystallized grains started to take place at some
point between the underaging and peak-aging processes, i.e., between 12 h and 24 h aging treatment. During aging towards the
overaged state, further growth of recrystallized grains occurred,
leading to an even larger average grain size of 65 m. On the other
hand, the observation that the average grain size changed from
4 m in the as-extruded state to 51 m in the underaged state is
likely the result of signicant grain growth caused by solution
heat-treatment [30,31].
Since recrystallization (which softens the matrix) was likely to
occur concurrently with aging-induced precipitation (which
hardens the matrix) in this study, the resulting hardness evolution
in the Al matrix in the vicinity of the interface would be determined by the competition between these two processes. Results
of hardness measurements as well as macroscopic tensile tests
indicate that precipitation-strengthening played the dominant
role, making the 24 h-aged (peak-aged) sample stronger and
harder than the 12 h-aged (underaged) sample.
3.3. Mechanical properties of the bulk composites
Fig. 5 shows the engineering stress vs. engineering strain response of the composites as obtained from uniaxial tensile tests.
Consistent with the hardness measurements, the sample subjected
to the 24 h aging treatment ("peak-aged") has the highest 0.2%
yield strength (520 MPa), followed by the overaged (496 MPa),
underaged (480 MPa), and as-extruded (370 MPa) samples. In the
case of ductility, the failure strain shows a decrease with increasing aging time, changing from 6.2% for the as-extruded
composite, to 4.3% (underaged), 2.6% (peak-aged), and nally to
1.9% (overaged). The yield strength and failure strain data are listed in Table 1, along with the estimated dislocation punched zone
size and the intrinsic hardness of the matrix alloy obtained from
hardness measurements, and the average grain size of the matrix
alloy for each sample, measured by EBSD characterization.
3.4. Strengthening mechanisms of the composites
To explore the mechanisms that may be responsible for the

83

Fig. 5. Tensile stress vs. strain curves of the composite samples treated under
4 different processing conditions.

evolution of the composites strength and failure strain for different heat treatments, the yield strength of the composites, sy, is
decomposed and expressed as [7,10]

y = 0 + aging + SiC
0 + aging + dis + L T
matrix + L T

(1)

where s0 stands for the initial strength of 7A04 alloy without reinforcement and aging treatment, saging and sSiC are the
strengthening contributions from articial aging and SiC reinforcement, respectively. sSiC primarily comes from a dislocation strengthening part sdis and a load-transfer (L-T) strengthening part sL-T, where the former is usually negligible for micron-sized reinforcements [7]. matrix = 0 + aging is the strength
of the matrix alloy, which can be estimated from the hardness
plateau corresponding to the matrix alloy by nanoindentation
measurement (Fig. 3 and Column 3 in Table 1).
A Tabor factor value of 3 is usually used to estimate the yield
strength from hardness data [32], i.e., y /3, where H is the
hardness measured by nanoindentation. However, in the present
work, dividing the hardness of 2.86 GPa for the peak-aged composite (Table 1) by 3 gives a stress value of about 950 MPa, which
is almost a factor of 2 higher than the yield strength of monolithic
7A04 Al alloy fabricated and heat treated under nominally the
same conditions as those used in this study (503 MPa) [33]. A similar discrepancy has previously been reported for 6xxx Al alloys
[13,34], and is likely the result of strong dislocation pile-up at the
indents. Bolshakov and Pharr [35] reported that, for materials
showing a strong pile-up effect (a high hf/hmax, where hf is the nal
contact depth and hmax is the maximum contact depth during the
nanoindentation test [21,35]), because of a signicant underestimation of the indentation contact area, the hardness calculated
using the OliverPharr method [21] can be greatly overestimated.
When hf/hmax 40.7, the underestimate of contact area can reach as
high as 60% [35]. In this study, hf/hmax is found to be systematically
higher than 0.9, indicating a strong pile-up and subsequently a
substantial overestimation of the hardness values. To accommodate this effect, here we dene an effective Tabor factor,
calculated using the apparent hardness of 7A04 alloy matrix
(2.86 GPa, see Table 1), divided by the yield strength of peak-aged
7A04 alloy (503 MPa) [33], which gives a value of 5.68. The yield
strength of the matrix alloy in the composites, smatrix, can then be
estimated from the hardness data, and the load-transfer

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J. Song et al. / Materials Science & Engineering A 644 (2015) 7984

strengthening contribution from the SiC particles, sL-T, can be

calculated from Eq. (1) as 0 matrix .
Column 9 in Table 1 lists the percentage of sL-T in sy for the
samples heat treated under different conditions. It is clearly shown
that samples with larger dislocation punched zones (the as-extruded and underaged states) have relatively more effective load
transfer between the reinforcement and the matrix, while for the
ones with narrower punched zones (the peak-aged and overaged
states), the load carried by the reinforcement is very limited,
which would more easily cause stress concentration and subsequent necking upon deformation, leading to early failure of the
composite [20]. This argument is supported by our results, which
show a decreasing failure strain from the as-extruded and underaged samples relative to the peakaged and overaged ones. The
reduction in ductility may also be associated with different types
and contents of the precipitates in the samples, whose interface
with the matrix alloy may serve as nucleation sites and easy paths
for crack growth [36]. In the case of the composites strength, on
the other hand, it seems that the intrinsic strength of the matrix
alloy plays a dominant role over the interfacial properties, and the
composite with the strongest matrix (peak-aged) has the highest
yield strength. This is actually a natural result of the low load
transfer in the interface region for this sample.

4. Conclusions
This work studied the hardness distribution across the reinforcement/matrix interface in SiCp/Al composites treated at
different aging conditions, with high spatial resolution. It has been
found that the dislocation punched zone size determined from the
hardness measurements is in qualitative agreement with the range
that GNDs extended out from the interface measured in TEM microstructural analysis. The evolution of the width of the punched
zone over different heat treatment conditions can be rationalized
by the effect of GNDs on aging kinetics. Moreover, mechanical
characterization of bulk composites revealed a reduction in failure
strain with decreasing punched zone size, most likely due to the
effect of less effective load transfer between the reinforcement and
the matrix in composites with smaller punched zone sizes. In the
case of composite strength, it has been found that the strength is
more dependent on the intrinsic strength of the matrix alloy then
on the nature of the interface. This study indicates that the
hardness measurement combined with microstructural analysis
may have important implications on the bulk properties of particulate-reinforced MMCs, and thus be a useful way to help sort out
composites with specic properties, leading to improved modeling
and design of MMCs.

Acknowledgment
The work is supported by the National Basic Research Program
of China (973 Program, No. 2012CB619600), the National High-

Tech R&D Program of China (863 Program, No. 2013AA031201), the

National Natural Science Foundation of China (Program No.
51471190), the Science and Technology Commission of Shanghai
Municipality (STCSM) (Nos. 13PJ1404000 and 14DZ2261200), and
the Ofce of Naval Research (ONR) under the guidance of Dr.
Lawrence Kabacoff (ONR N00014-12-1-0237). QG and JS would
like to acknowledge C. Xie from Keysight Technologies (China),
and Dr. L. Jiang from the University of California, Davis for useful
discussions.

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