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Enhanced combination of strength and ductility in ultrafine-grained

aluminum composites reinforced with high content intragranular
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Article  in  Materials Science and Engineering A · December 2018

DOI: 10.1016/j.msea.2018.12.090

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 Materials Science & Engineering A 745 (2019) 10–19

Contents lists available at ScienceDirect

Materials Science & Engineering A

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

Enhanced combination of strength and ductility in ultrafine-grained T

aluminum composites reinforced with high content intragranular
nanoparticles
⁎ ⁎
A.B. Li, G.S. Wang, X.X. Zhang , Y.Q. Li, X. Gao, H. Sun, M.F. Qian, X.P. Cui, L. Geng, G.H. Fan
National Key Laboratory of Materials Behavior and Evaluation Technology in Space Environment, School of Materials Science and Engineering, Harbin Institute of
Technology, Harbin 150001, China

A R T I C LE I N FO A B S T R A C T

Keywords: Simultaneous enhancement of the strength and ductility in metal-matrix nanocomposites with high content
Metal-matrix nanocomposites (MMNCs) nano-reinforcements is crucial for the development of novel composite materials. Here SiC/Al nanocomposites
Mechanical alloying with ultrafine Al grains and intragranular 10 vol% SiC nanoparticle were prepared by mechanical alloying and
Hot extrusion hot pressure sintering followed by hot extrusion. The results show that nanocrystalline Al grains and uniformly
Mechanical properties
distributed SiC nanoparticles (SiCnp) in the composite powders are obtained after ball-milling. The prior particle
Strengthening mechanisms
boundary (PPB) in the composite powders cannot be fully removed by sintering at 580 °C under 20 MPa, but can
be eliminated by subsequent hot extrusion at 450 °C with a ratio 25:1. The extruded nanocomposites possess
ultrafine Al grains with diameter 320 nm and intragranular SiCnp created by the dynamic recrystallizations
(DRX). Such optimal microstructure favors a significant improvement of 284% in yield strength (YS) and 259%
in ultimate tensile strength (UTS) compared with monolithic Al, and more interestingly, maintains an elongation
up to 12% due to the homogeneous nanoparticles in fine Al grains. Theoretical analysis shows that the dominant
strengthening factor is Orowan strengthening related to the high content intragranular SiCnp, with second factor
grain boundary strengthening due to ultrafine Al grains.

1. Introduction
Metal-matrix nanocomposites (MMNCs) reinforced with nano-re-
inforcements have attracted considerable attention due to their unique
mechanical and physical properties [1,2]. Generally, basic nano-
composite microstructures are classified into intra-type, inter-type and
nano/nano type. Among them, the most important structure is the
intra-type nanostructure, where the dispersed nanoparticles are em-
bedded within the matrix grains [3]. However, for such intragranular
nanoparticles, the allowable nanoparticle content is relatively low, ty-
pically about 1–5 vol% [4]. Therefore, how to uniformly disperse high
content nanoparticles into matrix alloy grains is a tough challenge in
the preparation of structural nanomaterials.
High strength and ductility are essential for structural material ap-
plications [1]. It is very interesting to use nanoparticles instead of mi-
croparticles to enhance the mechanical performances [5]. Nie et al.
fabricated AZ91/SiC nanocomposites and found that when 1 vol% SiC
nanoparticle (SiCnp) with diameter 60 nm replaced 10 vol% SiC mi-
croparticles with 10 µm, the ultimate tensile strength (UTS) was
enhanced from 267 MPa to 302 MPa, and elongation was improved
from 1.61% to 9.2% [6]. For intragranular [6] and intergranular [7–9]
nanocomposites, the addition of a small amount of nanoparticles can
retain good ductility besides enhanced strength. With further increasing
of the nanoparticle content, the strength was enhanced, but ductility
was reduced [2,10–12]. Especially, when high content nanoparticles up
to 10 vol% were added, the high strength was usually accompanied by
serious ductility loss [11–13]. For example, in ultrafine-grained SiC/
6063 nanocomposites, when SiC content was increased from 1 vol% to
10 vol%, UTS was increased from 343 MPa to 603 MPa, but elongation
was reduced from 10% to 2.3% [12]. So far, little work has been re-
ported on an excellent combination of strength and ductility in MMNCs
reinforced with high content nanoparticles.
Besides the effective strengthening capacity of nano-reinforcements
[5,14,15], decreasing the matrix grain size from micrometer to sub-
micrometer or nanometer also favors the mechanical properties
[1,12,16]. However, high strength nanocrystalline (< 100 nm) and
ultrafine-grained (e.g. 100–1000 nm) metals often show seriously re-
duced room temperature tensile ductility compared with their coarse

⁎
Corresponding authors.
E-mail addresses: xxzhang@hit.edu.cn (X.X. Zhang), ghfan@hit.edu.cn (G.H. Fan).

https://doi.org/10.1016/j.msea.2018.12.090
Received 1 September 2018; Received in revised form 17 December 2018; Accepted 18 December 2018
Available online 19 December 2018
0921-5093/ © 2018 Elsevier B.V. All rights reserved.
A.B. Li et al. Materials Science & Engineering A 745 (2019) 10–19

grained counterparts [17,18]. Recently, ultrafine-grained nanocompo-

sites have been fabricated through the introduction of the nanoparticles
into ultrafine-grained alloys [12,16,18–20], which promoted the strain
hardening ability and ductility [12,18,19]. However, the ultrafine-
grained nanocomposites exhibited poor ductility when the nanoparticle
content reached 10 vol% [12]. To date, the coupled effects of high
content nanoparticles and ultrafine grains on strength and ductility
have been rarely reported. Here, we have attempted to prepare 10 vol%
SiC/Al nanocomposites with ultrafine grains and intragranular nano-
particles using mechanical alloying and sintering followed by hot ex-
trusion. Their microstructure evolution, tensile properties and
strengthening mechanisms were investigated. A simultaneous en-
hancement of strength and ductility was demonstrated in the extruded
10 vol% SiC/Al nanocomposites.

2. Experimental details

Fig. 1. X-ray diffraction (XRD) patterns of 10 vol% SiC-Al nanocomposite

2.1. Fabrication of 10 vol% SiC/Al nanocomposites
powders ball-milled for different time durations 6–21 h.

Aluminum powders of 99% purity with average diameter 50 µm and

SiCnp of 99% purity with mean diameter 40 nm were selected as the
matrix alloy and reinforcement, respectively. 10 vol% SiC/Al nano-
composites were fabricated by mechanical alloying and hot pressure
sintering followed by hot extrusion. Firstly, under a small amount of
process control agent, Al powders with 10 vol% SiC nanoparticles were
mechanical alloyed with a ball-to-material ratio of 15:1 at 200 rpm for
various time durations (6, 9, 12, 15, 18 and 21 h) in a planetary ball
mill, respectively, from which an optimum milling time was de-
termined. Then the milled powders were vacuum sintered at 580 °C for
1 h under a pressure of 20 MPa. Finally, the sintered billets were ex-
truded at 450 °C with an extrusion ratio of 25:1.

2.2. Microstructure and tensile properties

The microstructure evolution of 10 vol% SiC/Al nanocomposites

during the whole fabrication process and the tensile fracture
morphologies were characterized using a Hitachi S-3000N scanning
electron microscope (SEM). SiCnp distribution, Al grains and SiC-Al
interfacial integrity were observed on a transmission electron micro- Fig. 2. Variation of Al grain size with milling time in 10 vol% SiC-Al nano-
scope (TEM) and high-resolution TEM (HRTEM). The constituent composite powders.
phases of the mechanical alloyed nanocomposite powders were de-
termined by Philips X′pert X-ray diffraction (XRD) using Cu Kα radia- the addition of high content SiCnp. Meanwhile, Al peaks are found to be
tion (λ = 0.154051 nm). Al grain size dXSR during mechanical alloying gradually broadened due to grain refinement and lattice strain accu-
process was estimated using the following Scherrer equation [21]: mulation.
0.9λ Fig. 2 shows the Al grain size determined by the full width at half
dXSR =
B cos θ (1) maximum (FWHM) of the main diffraction peaks in Fig. 1. With in-
creasing milling time, the Al grain size decreases rapidly, until a steady
where B is full width at half maximum (FWHM) of the diffraction peaks
value about 55 nm was reached after 15 h. This suggests that ball mil-
after removing the instrumental broadening, λ is wavelength of in-
ling reaches a steady state after 15 h, which produces steady nano-
cident X-ray radiation and θ is Bragg's diffraction angle. For extruded
crystalline Al in the nanocomposite powders. The grain refinement to
nanocomposites, the grain size distribution of the Al matrix alloy was
nanometer scale by mechanical alloying is attributed to the high dis-
determined from TEM images using Image-Pro Plus 6.0 software. The
location generated by severe plastic deformation [22]. Furthermore, the
relative densities of the sintered and extruded nanocomposites were
addition of nanoparticles accelerates the plastic deformation of the
measured by Archimedes method. Tensile stress-strain curves at room
matrix alloy and formation of nanocrystal grains [23,24] because the
temperature for Al alloy and SiC/Al nanocomposite were tested on an
interaction between nanoparticles and dislocations can induce the for-
Instron-5500 universal testing machine with a rate of 0.5 mm/min.
mation of high density dislocations. Therefore, the grain size decreases
quickly at the beginning until a balance between the grain refinement
3. Results and discussion
induced by severe impact deformation and grain coarsening by thermal
recovery was reached, after which the grain size keeps intact [25].
3.1. Microstructural evolution during mechanical alloying

3.1.1. Nanocrystalline Al in nanocomposite powders
In order to analyze the effect of milling time on the Al grain size
during mechanical alloying, XRD patterns of 10 vol% SiC-Al nano-
composite powders were tested, as shown in Fig. 1. It can be seen in
Fig. 1 that besides Al peaks, obvious SiC peaks are observed because of
3.1.2. Nanoparticle distribution in the nanocomposite powders
It is a challenging task to realize the uniform distribution of high
content nanoparticles in the nanocomposites. Mechanical alloying is
effective in achieving a homogeneous distribution of nano-[23–27] and
micro-[14,15] particles in matrix alloys. Fig. 3 displays SEM

11
A.B. Li et al.
Fig. 3. Representative morphologies of 10 vol% SiC-Al mixed powders after ball-milling for various time durations of (a) 9 h and (b) 15 h. (c) is an enlarged
micrographs of (b).
micrographs of 10 vol% SiC/Al powders milled for 9 h and 15 h, which
represent two typical morphologies before and after steady state, re-
spectively. Obviously, the nanocomposite powders are flat-shaped after
milling for 9 h (Fig. 3(a)) and equiaxed for 15 h (Fig. 3(b)). The re-
peated welding-fracturing processes contribute to the change from
flattened to equiaxed particles, during which homogenous dispersion of
nanoparticles was realized [26,27]. Moreover, the addition of high
content nanoparticles in Al powders helps in enhancing the Al work
hardening rate and nanocomposite powder fracture tendency, thus ac-
celerating the SiCnp dispersion process [25]. Ultimately, SiCnp are uni-
formly distributed in the nanocomposite powders after 15 h milling, as
shown in Fig. 3(c).
3.2. Microstructure of sintered nanocomposites
Mechanical alloying is usually used to fabricate uniformly dis-
tributed nanoparticle reinforced Al matrix composites. However, the
surfaces of milled aluminum powders are often covered by nanometer-
thick oxide films [28]. Therefore, it is necessary to break and shear off
these oxide films during the bulk material densification process [29].
Usually, hot pressure sintering and hot extrusion are used to consolidate
the milled powders into the bulk materials. The microstructure of the
as-sintered 10 vol% SiC/Al nanocomposite is characterized in Fig. 4.
Some prior particle boundary (PPB), a few nanoparticle clusters/pores
and debonding along PPB on the fracture surface are found in Fig. 4(a),
(b) and (c), respectively, suggesting that some oxide films and weak
bonding between the powder particles exist in as-sintered nano-
composites. The relative density of 94.2% further proves that the sin-
tered nanocomposites are incompletely compacted. In addition, the
high magnification fractograph in Fig. 4(d) reveals that most SiCnp are
homogeneously distributed in Al matrix alloys. During conventional hot
pressure sintering, the pressure can hardly provide high enough de-
formation to completely break up the oxide films along PPB of Al alloys
[28]. Such residual PPB with the oxide films deteriorates the bonding
strength between the milled Al particles, thereby inhibiting the material
densification. Therefore, hot pressure sintering is difficult to completely
eliminate PPB and to fully densify powders.
3.3. Microstructural characterizations of extruded nanocomposites
3.3.1. PPB elimination and nanocomposite densification
In order to further eliminate PPB and fully densify the materials, it is
necessary to perform the severe deformation for the sintered
12
Materials Science & Engineering A 745 (2019) 10–19
nanocomposites. In conventional extrusion process, a high enough ex-
trusion ratio is often required to completely break down PPB [30]. The
deformation standard of breaking down PPB during hot extrusion is
given as follows [28]:
ER 1 ⎞
Rs = 0.4 ⎜⎛ ER × AR + + ⎟
⎝ AR ER ⎠ (2)
where Rs is the PPB area ratio between the extruded and sintered ma-
terial, ER is extrusion ratio, and AR is the aspect ratio of extruded bar
cross-sections (AR = 1 for extruded round rod). When Rs > 4, the ex-
trusion deformation can fully eliminate PPB. In the present work, a
large extrusion ratio of 25:1, corresponding to Rs = 4.0 using Eq. (2), is
selected to extrude the as-sintered nanocomposites into the round rod.
Fig. 5 shows microstructure of the extruded 10 vol% SiC/Al nano-
composites with Rs = 4.0. As shown in Fig. 5(a), no PPBs are found in
the extruded nanocomposites, which is consistent with the result pre-
dicted by Eq. (2). A bright field TEM image in Fig. 5(b) further confirms
the homogeneous distribution of the SiCnp in the extruded nano-
composites. Meanwhile, relative density up to 99.4% was realized after
extrusion. These facts confirm that hot extrusion with Rs = 4.0 may
effectively eliminate PPB with oxide films, the particle clusters and
micro-pores. So, completely consolidated composites was obtained
[31].
3.3.2. Ultrafine grains and intragranular nanoparticles formed during
dynamic recrystallization (DRX)
Besides eliminating PPB and densifying nanocomposites, hot ex-
trusion also works in obtaining new microstructures for high strength
and ductility via DRX. TEM micrographs in Fig. 6 show morphology of
the Al grains in the extruded nanocomposite. Equiaxed Al grains formed
by recrystallization are observed in Fig. 6(a), suggesting that dynamic
recrystallization (DRX) happens during hot extrusion of 10 vol% SiC/Al
nanocomposites. During DRX of the metallic materials, new grains
nucleate and grow under the driving force provided by the storage
dislocation energy. It is noteworthy that the addition of second phase
particles in metals may accelerate recrystallization due to the particle
stimulated nucleation or retard recrystallization by pinning of the grain
boundaries [32]. The transition from accelerated to retarded re-
crystallization typically occurs when f/dp > 0.1–0.2 µm−1 [33], where
f is particle volume fraction and dp is particle diameter. In the present
work, the calculated f/dp is 2.5 µm−1, revealing that the addition of
10 vol% SiCnp with diameter 40 nm may retard DRX of the nano-
composites during hot extrusion. The nanoparticles may pin the grain
A.B. Li et al. Materials Science & Engineering A 745 (2019) 10–19

Fig. 4. Optical (a, b) and SEM (c, d) micrographs showing the microstructure of the as-sintered 10 vol% SiC/Al nanocomposite. (a) Prior particle boundaries (PPB)
morphology; (b) Nanoparticle clusters and pores; (c) Debonding along PPB on the fracture surface; (d) Homogeneous distributed nanoparticles in Al matrix alloys.

boundaries (namely Zener pinning) during grain growth. However,
during hot extrusion with high extrusion ratio, the high dislocation
density induced by the intense shear deformation may provide a large
driving force to overcome Zener pinning. Therefore, new grains can
nucleate and grow in spite of the nanoparticle pinning on the grain
boundaries. Similar recrystallized structures have also been found in
composites with small secondary phases processed by severe plastic
deformation [18,34].
It can clearly be seen from Fig. 6(b) that most SiCnp are uniformly
dispersed within the recrystallized Al grains, forming an intragranular
structure. During grain growth of DRX, when the large driving force
provided by severe plastic deformation is larger than Zener pinning
force, the grain boundaries will migrate and pass through the nano-
particles until the driving force is equal to Zener pinning force. Con-
sequently, most nanoparticles are left inside the recrystallized Al grains
due to DRX. Likewise, such nanoparticles distributed within the re-
crystallized grains have also been observed in SiCnp/AZ91 nano-
composite processed by forging [6]. Moreover, the effect of particle
pinning on grain growth has been analyzed by three-dimensional phase-
field simulations [35].
Fig. 7 shows the size distribution histogram of the ultrafine Al grains
in the extruded nanocomposite. Obviously, Al grain size is mainly dis-
tributed in the sub-micron range, with average diameter ~320 nm.
During DRX, such ultrafine grains are formed through the gradual
transformation of the dislocation sub-boundaries produced at low
strains into ultrafine grains with high angle boundaries produced at
large strains [36]. For high volume fractions of particles f ≥ 0.1, the
grain diameter D can be estimated based on the effect of second phase
particles on the grain growth using Zener-pinning relation [37]:
dp
D = 0.728
f 1.02 (3)
where D is grain diameter, while dp and f are particle diameter and
volume fraction, respectively. The calculated grain diameter D
= 306 nm is close to the experimentally measured value of 320 nm,
further demonstrating that the addition of 10 vol% SiC nanoparticles
with diameter 40 nm can indeed result in the formation of ultrafine-
grained Al alloy due to the nanoparticle pinning effect on the grain
growth during DRX. Meanwhile, the ultrafine grains exhibit an ex-
tensive size range, as shown in Fig. 7, which has also been attained
through DRX in other composite materials [18].

Fig. 5. (a) Optical microscope and (b) Bright field TEM micrographs showing the microstructure of the extruded 10 vol% SiC/Al nanocomposite.

13
A.B. Li et al.
Fig. 6. Bright field TEM micrographs showing morphologies of the Al grains in the extruded 10 vol% SiC/Al nanocomposites. (a) Recrystallized Al grains, (b)
Intragranular SiCnp.
Fig. 7. The grain size distribution histograms of the extruded 10 vol% SiC/Al
nanocomposites.
3.3.3. Interfacial integrity between SiC nanoparticle and Al alloy
Fig. 8 shows the interfacial microstructure of the extruded SiC/Al
nanocomposite characterized by TEM and HRTEM. The clean particle-
matrix interface without any reaction phases is displayed in Fig. 8(a).
The absence of reaction between SiC and Al may be attributed to the all
solid state during ball milling, sintering and hot extrusion, thus the
prevention of the interfacial reaction [38].
HRTEM image in Fig. 8(b) shows the presence of some specific
Fig. 8. (a) TEM and (b) HRTEM images showing the SiC-Al interfacial microstructure in the extruded 10 vol% SiC/Al nanocomposites.
14
Materials Science & Engineering A 745 (2019) 10–19
orientation relationship in some interfaces between Al and SiC, e.g. (11-
1)Al//(11-1)SiC and < 011 > Al// < 011 > SiC. Generally, the grain nu-
cleation and growth processes during DRX obey the law of the lowest
free energy. Moreover, the nanoparticles can act as the nucleation sides
during DRX [39]. Along the {111}Al plane and < 110 > Al direction,
the highest growth rate of Al on the surface of SiC can be achieved to
decrease the free energy [40]. At the same time, there is a small lattice
match between {111}Al and {111}SiC due to their identical face cen-
tered cubic structure and similar inter-planar spacing. Therefore, pre-
ferred orientation relationships, e.g. (11-1)Al//(11-1)SiC and < 011 >
Al// < 011 > SiC, exist in the nanocomposite which helps in the crea-
tion of a strong interfacial bonding strength between Al and SiC. So an
optimal microstructures for 10 vol% SiC/Al nanocomposites with uni-
formly distributed intragranular nanoparticles and ultrafine-grained
matrix as well as the strong bonding interfaces have been realized using
mechanical alloying, hot sintering and hot extrusion processes.
3.4. Tensile properties of extruded 10 vol% SiC/Al nanocomposite
Fig. 9 illustrates the tensile engineering and true stress-strain curves
and corresponding fractograph of the extruded pure Al and 10 vol%
SiC/Al nanocomposite. From the engineering stress-strain plots in
Fig. 9(a), the yield strength (YS) 280 ± 6 MPa and UTS 395 ± 7 MPa
was determined in the nanocomposite, which increase by 284% and
259% compared to those of the Al alloy with YS 73 ± 3 MPa and UTS
110 ± 4 MPa, respectively. More interestingly, the nanocomposite
exhibits a high elongation up to 12 ± 1%. Similar with the pure Al
(Fig. 9(b)), the fractograph of the nanocomposite shown in Fig. 9(c)
A.B. Li et al.
Fig. 9. (a) Tensile engineering and true stress-strain curves of the Al alloy and 10 vol% SiCnp/Al nanocomposite, (b) Fractograph of Al alloy, (c) Fractograph of
nanocomposite.
contains high-density ductile dimples, which is consistent to the high
elongation of the nanocomposite. Moreover, such ductile dimples in
nanocomposite are much smaller and shallower than those in pure Al,
also verifying that Al matrix grains are very fine in the nanocomposite.
In order to better evaluate the mechanical properties of nano-
composites with high content intragranular SiC nanoparticles and ul-
trafine-grained Al matrix, some tensile properties of Al matrix compo-
sites reinforced by micro- and nano-sized SiC particles are summarized
in Fig. 10. Obviously, the addition of both micro- and nano-particles
enhances the tensile strength, but reduces the ductility [2,11,12,41]. It
is worth noting that the introduction of small amount of nanoparticles
retains good ductility [2,11,12], but a high content nanoparticles up to
10 vol% often results in the poor ductility [11,12]. Different from the
above-mentioned 10 vol% SiC/Al nanocomposite [11], the nano-
composite synthesized in the present work exhibits high strength as
well as good ductility. Moreover, UTS of the present nanocomposite
(395 MPa) is much higher than that of the 10 vol% SiC microparticle
reinforced Al composite (215 MPa) [41], with elongation slightly
Fig. 10. The ultimate tensile strength (UTS) and elongation of the present
10 vol% SiC/Al nanocomposite and some other Al matrix nanocomposites re-
inforced by micro- and nano-sized particles with different volume fractions.
15
Materials Science & Engineering A 745 (2019) 10–19
decreasing from 17% in the latter [41] to 12% in the former composite.
Meanwhile, the tensile properties of the present composite are also
favorably comparable with those of the Al-6Cu-0.4Mn composite re-
inforced by 10 vol% SiC microparticles [42]. Therefore, the present
nanocomposite with homogeneously dispersed high content in-
tragranular SiCnp and ultrafine Al grains possesses excellent combina-
tion of strength and ductility.
3.5. Strengthening mechanisms of the nanocomposites
The present nanocomposite with high content intragranular SiCnp
exhibits the high YS up to 280 MPa, which is 284% higher compared
with Al alloy. Therefore, it is necessary to identify the contributions of
the various strengthening effects on the nanocomposite strength.
For the microstructure aspects of MMNCs, the matrix may be na-
nocrystalline, ultrafine or coarse grained metals, and may contain in-
tragranular or intergranular nanoparticles. Such complex structures
will play different contributions to MMNCs strength. In general, the
strengthening mechanisms of MMNCs include the grain boundary
strengthening (namely Hall-Petch strengthening ΔσHP), nanoparticle
strengthening (namely Orowan strengthening ΔσOR), thermal mismatch
strengthening (ΔσCTE) and load transfer from matrix to reinforcements
(ΔσLT) [43,44].
3.5.1. Orowan strengthening associated with intragranular nanoparticles
As is known, Orowan strengthening is induced by the interaction of
dislocations with intragranular nanoparticles. Therefore, such me-
chanism is effective only when the second phase particles are located
within the matrix alloy grains. The contribution of Orowan strength-
ening ΔσOR can be determined according to [43,44]:
0.13Gb dp
ΔσOR = ln
dp [(1/2f )1/3 − 1] 2b (4)
where G is the shear modulus of the matrix alloy (26 GPa for Al), b is the
Burger's vector (0.286 nm for Al) [45,46], dp is the particle diameter
and f is the particle volume fraction. As expected for the present na-
nocomposites, the estimated contribution of Orowan strengthening to
YS can reach up to 145 MPa. This is because that the addition of high
content nanoparticles up to 10 vol% can significantly reduce the par-
ticle inter-spacing and create a strong interaction between dislocations
A.B. Li et al.
and nanoparticles. Therefore, intragranular nanoparticle strengthening
makes a dominant contribution to the present nanocomposite.
3.5.2. Grain boundary strengthening associated with grain size
The above-mentioned experimental and theoretical results all prove
that high content SiCnp can create ultrafine Al grains, which was formed
by pinning of Al grain boundaries by SiCnp during grain growth process
of DRX. For the ultrafine-grained matrix alloys, the grain boundary
strengthening effect ΔσHP can also be calculated by Hall-Petch equation
[45–47]:
∆σHP = KD−1/2 (5)
where K is a constant, D is average grain diameter. For ultrafine-grained
pure aluminum, K = 40 MPa μm1/2 [45,46]. The average grain dia-
meter is 320 nm measured in our study). Using Eq. (5), the strength-
ening value is estimated to be 71 MPa, suggesting that the grain
boundary strengthening plays a relatively important role in the strength
improvement of 10 vol% SiC/Al nanocomposites.
3.5.3. Thermal mismatch strengthening
Generally, the mismatch of the coefficient of thermal expansion
(CTE) between reinforcement and matrix generates the dislocations in
the near-interface areas of the reinforcement, and thus strengthens the
matrix alloy. It is noteworthy that, for micro-particle reinforced com-
posite, only when the particle volume fraction is larger than 20%, the
thermal mismatch induced dislocations can strengthen the entire matrix
alloys [48]. However, for nanoparticle reinforcements, the content is
difficult to reach up to 20 vol%. Consequently the dislocations punched
out from the nanoparticles into the matrix can only strengthen the small
punched zone around the nanoparticles rather than the entire matrix.
Therefore, the dislocation density ρ in the punched zone due to the
thermal mismatch is given by [49]:
6fΔαΔT k
ρ= ⎛ ⎞ ln(f −1/3 )
b2 ⎝ G ⎠ (6)
where Δα is the CTE difference between matrix αm and reinforcements
αp, k is matrix shear strength, ΔT is difference between processing and
room temperatures. For the present SiC/Al composites, αm
= 23.6 × 10−6 /K, αp = 4.3 × 10−6 /K [49] and ΔT = 430 K. The
corresponding strengthening effect ΔσCTE due to the dislocations gen-
erated by CTE mismatch can be calculated by [48–50]:
ΔσCTE = aGbρ1/2 (7)
where a is a constant, equal to 1 [49] or 1.25 [48,50]. The contribution
of thermal mismatch strengthening is predicted to be 45–56 MPa.
3.5.4. Load transfer from matrix to reinforcements
As shown in Fig. 8, the present SiC/Al nanocomposite has a good
interfacial bonding between Al matrix and SiC nanoparticles, sug-
gesting an effective load transfer from matrix to nanoparticles. A widely
accepted equation of increase in YS due to load transfer ΔσLT can be
given by [16,43,44]:
ΔσLT = 0.5σm f (8)
where σm is YS of unreinforced Al matrix (73 MPa measured in our
work). The value of ΔσLT is calculated to be 4 MPa, suggesting that
strength improvement due to load transfer is small.
For 10 vol% SiC/Al nanocomposite, the contributions of the
abovementioned various strengthening strategies ΔσOR, ΔσHP, ΔσCTE and
ΔσLT are 145, 71, 45–56 and 4 MPa, respectively. In the present in-
tragranular nanocomposites, SiCnp mainly locate within the Al grains
through DRX. Such high content intragranular nanoparticles, which
directly interact with moving dislocations, can give full play to the
Orowan strengthening mechanism. Therefore, nanoparticle strength-
ening provides very high contribution to YS (145 MPa). As reported by
Zhang et al., Orowan strengthening contributes the most to YS of the
16
Materials Science & Engineering A 745 (2019) 10–19
composites reinforced with particles less than 1 µm [51]. Orowan
strengthening mechanism is known as an important strengthening
mechanism in MMNCs with grain size larger than particle size. How-
ever, in some nanocomposites, particles mainly located at grain
boundaries, thus the strengthening effect due to Orowan mechanism
was not considered [16].
In present ultrafine-grained aluminum nanocomposites, the addi-
tion of 10 vol% SiCnp with diameter 40 nm can pin the grain boundaries
during the grain growth, forming ultrafine-grained Al matrix with grain
diameter 320 nm. Meanwhile, such ultrafine grains contribute 71 MPa
to YS by Hall-Petch strengthening; thus it is an important strengthening
factor. For some ultrafine-grained nanocomposites, the grain boundary
strengthening still makes the largest contribution to strength due to the
existence of intergranular nanoparticles [12,16]. During the cooling
process of the nanocomposite fabrication, thermal mismatch between
reinforcement and matrix induces dislocations around the nanoparticle
interfaces. Meanwhile, high dislocation density exists near the interface
between the matrix and reinforcement particles [52]. Therefore, such
high dislocations only strengthen the small punched zone around the
nanoparticle interfaces rather than the entire matrix, consequently
contributing only 45–56 MPa to YS by thermal mismatch strengthening.
Unlike continuously reinforced composite, the load transfer from ma-
trix to nanoparticles through interfacial shear stresses is minor [12] due
to the small aspect ratio and low volume fraction of nanoparticles
[12,16,44,52]. In a word, Orowan strengthening due to high content
intragranular nanoparticles plays the dominant role in the nano-
composite strength followed by the grain boundary strengthening due
to ultrafine grains.
3.5.5. Overall strengthening behaviors based on available models
From the calculation results of the indirect strengthening (Orowan
strengthening, grain refinement, thermal mismatch) and direct
strengthening (load transfer) effects, the overall strengthening beha-
viors can be estimated. Generally, the contributions to the increase in
YS by various strengthening mechanisms could be taken as a simple
summation or the root of the sum of squares of the different mechan-
isms [16,43–45,47,53]. In addition, a modified shear lag model con-
sidering micromechanics strengthening mechanisms (indirect con-
tribution of Orowan effect), grain size strengthening and CTE mismatch
strengthening, was often used to calculate YS of the composites
[16,50–52,54,55]. The above-mentioned theoretical predictions were
found to be in good agreement with the experimental data. Akbarpour
et al. has applied these three calculation methods to more accurately
estimate the overall strengthening behavior of ultrafine-grained Cu
matrix nanocomposites with 2 vol% SiCnp [16]. Therefore, in our work,
YS of nanocomposites σcy is estimated by three common calculation
methods using the simple linear summation, the root of the sum of
squares and modified shear lag model. The first model using simple
linear superposition of several strengthening mechanisms can be given
as follows [16]:
σCy = σ0 + ΔσHP + ΔσOR + ΔσCTE + ΔσLD (9)
where σ0 is the intrinsic frictional stress of the material in the absence of
any other strengthening mechanism (20 MPa for pure Al [45]). In Eq.
(9), σ0+ΔσHP represent the yield strength of the matrix in the composite,
while ΔσOR + ΔσCTE +ΔσLD are the increase of the yield strength due to
the present of nanoparticles. The yield strength σcy of nanocomposites is
calculated to be 285–296 MPa, and it is reasonably close to the ex-
perimental yield stresses of 280 MPa
The second model using square root of the sum of the squares can be
applied to calculate the total improvement in YS of the composite Δσ ,
giving the following equation [16,43]:
Δσ = (Δσ 2HP + Δσ OR
2 2
+ Δσ CTE + Δσ 2LD) (10)
The total improvement in YS of the composite Δσ can also be
A.B. Li et al.
obtained according to [44]:
2 2
Δσ = ΔσHP +ΔσLD + Δσ OR + Δσ CTE (11)
Thus, YS of the composite σcy is described [16]:
σcy = σm + Δσ (12)
where YS of unreinforced Al matrix σm = 73 MPa. Using Eq. (10) and
Eq. (11), the total improvement in YS of nanocomposite Δσ is predicted
to be 168–171 MPa and 227–230 MPa, and the corresponding YS of
nanocomposites σcy is calculated to be 241–244 MPa and 300–303 MPa.
Compared with the experimental YS of 280 MPa, the prediction value
using the root of the sum of squares of ΔσOR and ΔσCTE is more accurate
than the root of the sum of squares of all strengthening factors, sug-
gesting that the analysis model using the root of the sum of squares of
ΔσOR and ΔσCTE is more suitable to predict the nanocomposite
strengthening behavior. This is because both Orowan and thermal
mismatch strengthening are associated with the particle-dislocation
interaction.
The third model of modified shear lag theory considering the load
transfer mechanism, which is used to predict YS for discontinuously
reinforced composites, can be expressed by the following equation
[51,55]:
σcy = σmy [f (S+2)/2 + (1−f )] (13)
where σcy and σmy are YS of the composite and matrix materials, S is the
aspect ratio of the reinforcement (S = 1 for equiaxed particles).
Therefore, YS of particle reinforced composites σcy can be simplified as
follows [16,50]:
σcy = σmy (1 + 0.5f ) (14)
where σmy represents the YS of matrix with the presence of nano-
particles. The addition of nanoparticles in the matrix may change the
matrix microstructure (i.e. grain size, dislocation density formed by
Orowan strengthening and CTE mismatch) and thus indirectly en-
hanced the matrix alloy strength. Therefore, considering the indirect
contribution of Orowan strengthening ( ΔσOR ), grain size strengthening
( ΔσHP ), and CTE mismatch strengthening ( ΔσCTE ), σmy can be written as
[50,51]:
σmy = σ0 + ΔσOR + ΔσHP + ΔσCTE (15)
According to the modified shear lag model combining indirect and
direct strengthening effects, YS of nanocomposites σcy is determined to
be 295–307 MPa, which is similar to the yield stress using the root of
the sum of squares of the different mechanisms.
Using the simple linear summation and the root of the sum of
squares of the different mechanisms as well as a modified shear lag
model, the yield strength σcy is estimated to be 285–296 MPa,
300–303 MPa and 295–307 MPa, respectively. These prediction values
are comparable to the experimental YS 280 MPa, showing that these
theoretical methods can be applied to predict the overall strengthening
behavior of ultrafine-grained aluminum composites reinforced with
high content intragranular nanoparticles, and to determine the con-
tributions of each strengthening mechanism.
3.6. Ductility analysis of the nanocomposites
Besides the high strength, ultrafine-grained aluminum composites
reinforced with high content intragranular nanoparticles simulta-
neously exhibit good ductility up to 12% total elongation to failure,
which is quite different from the limited uniform elongation in nano-
crystalline and ultrafine-grained metals due to the high YS and poor
strain hardening [56,57]. Therefore, a correlation between the plastic
instability and necking failure tendency was introduced to explain the
obtained ductility of ultrafine-grained aluminum nanocomposites. The
uniform elongation on the curves in Fig. 9(a) was determined by the
17
Materials Science & Engineering A 745 (2019) 10–19
Fig. 11. Strain hardening rate - true strain and true stress - true strain curve and
their intersection point (necking point).
Considère criterion (Eq. (16)) governing the onset of localized de-
formation for plastic instability [18,56]:
dσ
σ≫⎛⎜ ⎞⎟
⎝ dε ⎠ε̇ (16)
where σ and ε are true stress and true strain in Fig. 9(a), respectively, so
that dσ is the strain-hardening rate.
dε
Fig. 11 shows the strain hardening rate - true strain and true stress-
true strain curves. Obviously, ultrafine-grained aluminum nano-
composites exhibit higher strain-hardening rate due to homogeneously
dispersed nanoparticles within the ultrafine-grained alloys [56]. It is
well known that high work-hardening rate helps in delaying the loca-
lized deformation (necking) under tensile stress, and thus is favorable
for the uniform plastic deformation. As expected, the necking point
occurs at a true strain of 5.8%, which is in good agreement with 6%
uniform elongation measured from the engineering stress–strain curves
in Fig. 9(a). This confirms the high uniform elongation in 10 vol% SiC
reinforced ultrafine-grained aluminum nanocomposites, which is im-
portant for various structural applications. For the intragranular na-
nocomposites, introducing high content intragranular nanoparticles can
induce high density dislocation in ultrafine-grained aluminum matrix
due to Orowan strengthening and thermal mismatch, providing a sig-
nificant strain hardening effect. Therefore, large uniform elongation
accompanies by high tensile strength. Similar results has also been re-
ported by Takata et al., in which nanoparticles dispersed in the ultra-
fine-grained matrix significantly enhanced strain hardening, resulting
in the simultaneous improvement of uniform elongation and tensile
strength [56].
On the other hand, the composite plasticity is very sensitive to na-
noparticle content and distribution. During the deformation of the in-
tergranular nanocomposites, high content intergranular nanoparticles
form a continuous network along the grain boundaries and conse-
quently induce serious grain boundary embrittlement and catastrophic
macro-brittle fracture at a small strain [7]. Compared to intergranular
nanocomposites, high content intragranular nanoparticles uniformly
dispersed within the plastic matrix grains do not deteriorate the con-
tinuity of the matrix alloy, and therefore are favorable for the plastic
deformation of the matrix. So a good combination of ductility and
strength is achieved in the ultrafine-grained Al matrix composites re-
inforced with high content intragranular nanoparticles.
Besides the introduction of second phase particles, the appropriate
grain size distribution favors the strain hardening and thus the ductility
of ultrafine-grained metals [58]. In the present work, the wide grain
size distribution in 50–900 nm range (in Fig. 7) and large amount of
intragranular nanoparticles (in Fig. 6) prevent the localized deforma-
tion and premature fracture, and thus induce significant strain hard-
ening.
A.B. Li et al.
4. Conclusion
10 vol% SiC/Al nanocomposites with intragranular nanoparticles
and ultrafine-grained matrix were successfully prepared by mechanical
alloying and hot pressure sintering followed by hot extrusion. The main
conclusions can be drawn as follows:
(1) Mechanical alloying process of 10 vol% SiC-Al nanocomposite
powders reached a steady state after 15 h. Nanocomposite powders
with nanocrystalline Al grains and high content SiC nanoparticles
homogeneously embedded in the Al powders were obtained at a
milling time of 15 h. The composite billet prepared by sintering at
580 °C under a pressure of 20 MPa exhibited obvious PPB, a few
nanoparticle clusters and pores.
(2) Hot extrusion at 450 °C with an extrusion ratio 25:1 not only
eliminated PPB retained in the as-sintered nanocomposites, but also
produced submicron Al matrix grains via dynamic recrystallization
(DRX). In addition, extruded nanocomposites exhibited minimal
porosity, good interfacial bonding between SiC and Al, and in-
tragranular particle distribution state formed by DRX process.
(3) The introduction of intragranular nanoparticles and formation of
ultrafine matrix grains in pure aluminum remarkably increased the
ultimate tensile strength (UTS) from 110 MPa to 395 MPa (increase
up to 259%) and yield strength (YS) from 73 MPa to 280 MPa (up to
284%), while retaining a good fracture elongation up to 12%.
(4) For 10 vol% SiC/Al nanocomposites, Orowan strengthening attrib-
uted to high content intragranular SiC nanoparticles was the
dominant mechanism for the enhancement of strength, followed by
grain boundary strengthening due to ultrafine Al grains.
Acknowledgements
We gratefully acknowledge the financial supports from (a) National
Key Research and Development Plan, No: 2017YFB0703103), (b) Fund
of National Key Laboratory of Materials Behavior and Evaluation
Technology in Space Environment and (c) National Natural Science
Foundation of China (Grant Nos. U1537201, 51401068, 51101041,
51201047 and 51771064).
Data availability statement
The raw data required to reproduce these findings are available
from the corresponding author upon request.
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