CARBON 4 7 ( 2 0 0 9 ) 5 7 0 –5 7 7

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Combination of hot extrusion and spark plasma sintering

for producing carbon nanotube reinforced aluminum
matrix composites

Hansang Kwon, Mehdi Estili, Kenta Takagi, Takamichi Miyazaki, Akira Kawasaki*
Department of Materials Processing, Graduate School of Engineering, Tohoku University, Sendai 980-8579, Japan

A R T I C L E I N F O A B S T R A C T

Article history:
Received 12 August 2008
Accepted 24 October 2008
Available online 12 November 2008
Aluminum (Al)/carbon nanotube (CNT) composites with nanoscale dispersion and regular
orientation of the CNTs were fabricated by a combination of some advanced powder pro-
cesses. The CNTs were well dispersed onto the Al particles by a nanoscale dispersion
method. Moreover, the highly densified CNT composites were prepared by spark plasma
sintering and subsequent hot extrusion. Microstructural observations by optical, field-
emission scanning electron, and high-resolution transmission electron microscopies con-
firmed that the sintered Al/CNT compact and extruded bulk material had a good dispersion
of oriented CNTs. Raman spectroscopy showed that the processing did little damage to the
CNTs. As a result, the composites exhibited tensile strengths that were thrice larger than
pure aluminum because of the CNT reinforcement.
Ó 2008 Elsevier Ltd. All rights reserved.

1. Introduction neously mixed in a matrix by utilizing their electrokinetic po-

Many industries, such as the automobile, aerospace, and air-
craft industries, are expected to develop super-materials that
are ultralight and that have high hardness and high strength.
In addition, next-generation materials must be environmen-
tally friendly, energy saving, and inexpensive. Carbon nano-
tubes (CNTs), which were first discovered in 1991 [1], are
now well known to possess an extremely high strength, high
elastic modulus, and low weight, exceeding that of conven-
tional fibers [2]. Therefore, CNT–metal matrix composites
[3–5] are expected to assume the role of structural materials
in the next-generation. However, CNT–metal matrix compos-
ites are currently falling behind in bulk fabrication due to the
difficulty of dispersing the CNTs, as compared to polymer-
and ceramic-CNT composites [6–11]. In general, powder met-
allurgy and casting techniques are utilized for the fabrication
of composites. In the cases of polymer and ceramic matrices,
some reports have demonstrated that agglomerated CNTs
with a huge cohesive force could be broken up and homoge-
tential, and the resultant composites exhibited the expected
performances [12,13]. However, most of these approaches
are unavailable for CNT dispersion in metals because of the
low controllability of the zeta potential of metal particles
and the large density gap between the metal and CNT. For this
reason, the development of bulk fabrication methods for
CNT–metal matrix composites was started on the basis of a
mechanical mixing approach [14,15].
Kuzumaki is a pioneer in the production of Al/CNT com-
posite materials by mechanical mixing and hot extrusion
[15]. However, they achieved less strengthening of the Al than
expected, up to 84 MPa by a 5 vol% addition of CNT, which is
same as that of pure Al and slightly increased by post process.
This underperformance may be due to the poor CNT disper-
sion even though they improved the CNT dispersion by
mechanical mixing. Esawi and Morsi also tried to mix CNTs
with Al powders by highly efficient mixing using a tubular
shaker-mixer and planetary mill, but recognized the difficulty
of dispersing the CNTs [16]. Because of these conventional

* Corresponding author: Fax: +81 22 795 7312.

E-mail address: kawasaki@material.tohoku.ac.jp (A. Kawasaki).
0008-6223/$ - see front matter Ó 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.carbon.2008.10.041
 CARBON 4 7 (2 0 0 9) 5 7 0–57 7
mechanical mixing results, Noguchi et al. developed a new
mixing method called nanoscale dispersion (NSD), which dis-
perses the CNTs with a metal powder using natural rubber
(NR) as a mixing medium [10,17–19]. They demonstrated that
the resulting Al–CNT composite materials presented better
dispersion. However, in order to get the best out of this meth-
od, it is necessary to develop a new fabrication approach that
is able to give high density and an orientational microstruc-
ture to the Al–CNT composite.
This study examined the feasibility of fabricating bulk Al–
CNT composites with regularly oriented CNTs from a nano-
scale dispersed powder by combining the processes of spark
plasma sintering (SPS) and hot extrusion. In the first step,
the SPS [20,21] underwent a uniaxial pressing carried out to
densify the Al–CNT mixed powder, and then the orientation
in the sintered compact powder was enhanced by hot extru-
sion. The microstructure and mechanical properties of the
Al–CNT composites were then characterized.
2. Experimental procedure
The procedure for our suggested method of fabricating Al–
CNT composites is shown in Fig. 1. First, a precursor was pre-
pared by the NSD method with the goal of dispersing the
CNTs in the aluminum powder [10,17–19]. This precursor con-
sisted of commercial gas atomized Al powder (ECKA Granules
Japan Co. Ltd., purity 99.85%, average particle size 14.82 lm),
multi-walled carbon nanotubes (MWCNTs) (Iljin Co. Ltd., pur-
ity 99.5%, diameter 20 nm, length 15–50 lm), and natural rub-
ber (NR). The powder composition was adjusted for 5 vol%
CNT–Al powder. The precursor was heat treated at 500 °C
for 2 h in an argon atmosphere (1 l/min) to evaporate the
NR. The obtained Al–CNT mixture powder was sintered in a
carbon mold using a spark plasma sintering device (SPS-
S515) manufactured by Sumitomo Coal Mining Co. Ltd. The
sintering conditions were a maximum temperature of
600 °C, holding time of 20 min, heating rate of 40 °C/min,
and pressure of 50 MPa. The sintered compact had a diameter
of 15 mm and a length of 30 mm.
The sintered compact was extruded in a 60° conical die at
400 °C with a pressure of 500 kN (UH-500 kN1, Shimadzu Cor-
poration, Japan). The extrusion velocity and the extrusion ra-
tio were fixed at 2 mm min 1 and 20, respectively. The oxygen
content of the raw Al powder, the Al–CNT mixed powder, the
sintered compact, and the extruded composite was measured
by LECO (TC-444, LECO Co. Ltd., USA). The microstructures of
the samples after every step were observed with an optical
microscope (PMG-3, Olympus, Japan), field-emission scanning
electron microscope (FE-SEM6500, JEOL Co. Ltd., Japan), and
Fig. 1 – Fabrication procedure for Al–CNT composites.
571
high-resolution transmission electron microscope (HR-TEM,
Hitachi, Japan) using energy-dispersive spectrometry (EDS)
and selected-area diffraction patterns (SAD). Raman spectros-
copy (SOLAR TII Nanofinder, Tokyo Instruments Co. Ltd., Ja-
pan) was used to evaluate the disorder of the CNTs after
each step.
The macro-hardness of the extruded Al–CNT composite
was evaluated using a Vickers hardness tester (MVK-TypeG7,
Akashi Co. Ltd., Japan) with a load of 200 g. The micro-hardness
of the raw Al particle and extruded bulks were measured by a
nano-indentor (TMZ-512, Akashi Co. Ltd., Japan). The condi-
tions for nano-indentation were a load of 0.4 g and a loading
time of 10 s. A three-sided pyramidal diamond (Berkovich) in-
denter was chosen after referring to the literature related to
the nano-indentation of Al alloys [22,23]. To evaluate the tensile
strength, the extruded bulks were machined into test pieces
with 3 mm diameters in accordance with ICS 59.100.01. The
tensile strength was measured by a universal testing machine
(AUTOGRAPH AG-I 50 kN, Shimadzu Co. Ltd., Japan).
3. Results and discussion
Fig. 2 shows the HR-TEM micrographs of the pristine
MWCNTs employed in this study. The MWCNTs had a curled
shape and a bamboo-like structure (Fig. 2a). Moreover, there
were many disordered regions (black arrow), and some amor-
phous carbons were absolved on their surface (white arrow),
as shown in Fig. 2b.
Fig. 3 shows the FE-SEM micrographs of the powder mix-
ture after debinding. No remaining NR was found by observa-
tion, which indicates the perfect removal of the NR. The Al
particles almost retained their spherical shape, even though
they were subjected to kneading and heat treatment.
The observation at higher magnification confirmed the
good uniform dispersion of the CNTs on the Al particles, as
seen in Fig. 3b. However, there were some regions where the
CNTs were not well dispersed, as shown in Fig. 3c.
Such condensations are supposed to arise because the
CNTs that were dispersed in a void surrounded by Al particles
before the debinding moved and gathered together onto the
Al particles by the capillary effect of the melting NR. In the
present study, even though condensations of CNTs were occa-
sionally observed, the mixed powder prepared by the NSD
method was demonstrated to have more advanced dispersion
than that prepared by other methods. Additionally, the CNTs
omnidirectionally lie on the surface of the Al particles at this
stage.
The relative density of the sintered compact was 96.1%, as
indicated in Table 1. In general, Al powders have low sinter-
572 CARBON 4 7 ( 2 0 0 9 ) 5 7 0 –5 7 7

Fig. 2 – TEM micrographs of a bundle of pristine MWCNTs (a) low magnification, (b) high magnification.

Fig. 3 – FE-SEM micrographs of (a) Al–CNT mixture powder, (b) region of uniform dispersion, and (c) region of CNT
condensation on Al powder.

Table 1 – Some properties of the samples for every process.

Relative Oxygen content ID/IG Vickers Nano-indentation

density (wt.% ± 2%) hardness (HV) (Hu, mN/lm2)

Al powder – 0.403 – 22 37
Heat treated Al–CNT mixes powder – 1.104 CNT:0.877 Al–CNT:0.831 – –
Sintered Al–CNT compact 96.1 0.798 0.858 – –
Extruded Al–CNT bulk 98 0.791 0.843 52 Pure Al:37 Al–CNT:40

ability because the strong oxide scale on the surfaces of Al
particles prevents direct contact between the particles
[21,24–26]. The high density obtained in the present study
was attributed to the reduced atmosphere due to the use of
a carbon mold. Moreover, it is estimated that some regions
of oxide scale on the surfaces of the Al particles were de-
stroyed by the 50 MPa load pressure, and particularly by the
specific surface cleaning effect of the SPS [21,24–26].
The change in the oxygen content by this process is also
indicated in Table 1. The oxygen content was increased by
the debinding process in spite of its non-oxidative atmo-
sphere. This is supposed to be due to the adsorption of oxy-
gen impurities in the commercial gas source. However, the
increased oxygen content was reduced by the SPS process.
This result proves the oxide-destroying effects of the SPS, as
described above. Furthermore, there was no significant
change in the oxygen content after the hot extrusion. There-
fore, the subsequent hot extrusion could achieve further den-
sification of up to 98%. In other words, a combination of the
SPS and hot extrusion processes was very effective, at least
for the densification of Al–CNT composites.
Fig. 4 shows micrographs of the transverse and longitudi-
nal cross sections of the sintered compact. A comparison of
Fig. 4a and b with Fig. 3a shows that grain growth did not oc-
cur, even though the process was conducted at a high temper-
ature of 600 °C. This restraint of grain growth is estimated to
be due to the pinning effect of the CNTs and remaining Al
oxide, despite the surface cleaning effect of the SPS process.
 CARBON 4 7 (2 0 0 9) 5 7 0–57 7 573

Fig. 4 – Micrographs of (a–c) transverse cross section and longitudinal cross section of Al–CNT sintered compact. (c) and (d)
represent the grains and grain boundary by FE-SEM at high magnifications.

The rapid heating and applied pressure of the SPS would also
be effective in suppressing grain growth. All of the CNTs were
found in grain boundaries after sintering, as shown in Fig. 4c
and d. The grain boundaries that included CNTs can be ob-
served as black outlines in the optical micrographs (Fig. 4a
and b). Because the outlines seem to surround all of the grains
with the same thickness, the added CNTs were predicated to
be dispersed homogeneously in the sintered compact. The
SEM observation also showed that the grain boundary layers
have an average thickness of about 200 nm and that the inter-
face between the CNTs and Al grain seemed to be closely ad-
hered, but the detail of the internal structure could not be
identified. Thus, the grain boundaries of the sintered compact
were observed in detail by the TEM.
As seen in Fig. 5, the observation revealed that the grain
boundary of the sintered compact was definitely filled with
several phases. These phases were identified by EDS, the
SAD pattern, and HR-TEM as the CNTs, amorphous carbon,
Al oxide, graphite, and a small quantity of aluminum carbide.
The alumina phases, which were determined to have an
amorphous structure by the SAD, were derived from the oxide
scale on the raw Al particles, because they surround the Al
grains, as seen in Fig. 5b. In addition, broken alumina layers
were occasionally found (the arrow in Fig. 5a).
The presence of aluminum carbide between the Al and
CNTs is a particularly important fact to emphasize. Laha
et al. reported that, although the Al–graphite system ordinar-
ily presents a high wetting angle of 135–140° at 1190 °C, the
presence of the interfacial aluminum carbide reduces it down
to 55° [27]. In other words, the formation of carbide will be
helpful for a strong bonding between the Al matrix and CNTs.
However, the surface of an ideal CNT with a perfect graphene
structure is known to be chemically inert with the Al liquid
phase. Thus, this formation of aluminum carbide means that
the CNTs exposed their reactive prism planes, i.e. structural
defects, at the sintering stage. Therefore, the following possi-
bilities for forming the aluminum carbide (Al4C3) can be sug-
gested [28]: the molten aluminum and the open ends of the
CNT tips react with the Al4C3. Otherwise, the Al4C3 results
from the reaction between the molten Al and the amorphous
carbon or the defect region of the graphite sheet on the CNTs.
In either case, it must be assumed that molten Al was gener-
ated between the surfaces of the particles in spite of the solid
state sintering.
Fig. 5c represents one of the Al4C3 phases at higher mag-
nification. The average size of the Al4C3 was within 20–
40 nm, which is much larger than the reported size of about
5 nm [27]. It is thought that the size of the defect sites of
574 CARBON 4 7 ( 2 0 0 9 ) 5 7 0 –5 7 7

Fig. 5 – TEM micrographs of the grain boundary layer of the sintered compact. (a) Micrograph of the entire grain boundary, in
which the boundary layer between the Al grains consists of alumina 2, CNT 3, amorphous carbon black 4, graphite 5, and
Al4C3 6 phases. The white arrow indicates the broken alumina phase. (b) The region between the CNTs and Al matrix. Inset,
the SAD pattern of the boundary between the CNTs and Al. (c) The region of the Al4C3 phase. Left inset, the HR-TEM image
and the SAD pattern of the Al4C3 phase. Right inset, an illustration of the interface between the carbide and Al grains.

raw CNTs in this study were larger than given in the litera-
ture. Fig. 5c also shows a black layer beside the carbide phase,
which was identified as Al oxide, as described above. A black
layer between the carbide and grains is also seen, but this
may be an overlapping image of the oxide existing under
and/or over the carbide due to the transmitting characteris-
tics of the TEM. Although it is difficult to know the exact spa-
tial relationship between the Al oxide and carbide, the carbide
directly bonds with the Al grains, as illustrated in the inset of
Fig. 5c. Further analysis is necessary to obtain more detailed
information about the microstructure of the Al–CNT sintered
compact because this microstructure directly affects the for-
mation of the microstructure of the extruded Al–CNT bulk.
Fig. 6 shows micrographs of the longitudinal cross sections
of the extruded Al–CNT composite. The microstructure of the
Al–CNT composite was extended parallel to the extrusion
direction and the grain size was reduced to around 1 lm along
the minor axis (the white arrow in Fig. 6b). The occasional
pores (the black arrow in Fig. 6a) can be identified as etch
grooves derived from the agglomeration of CNTs, because
they were not seen before the etching. Additionally, as seen
in Fig. 6b, the grain boundaries have only a few CNTs in the

Fig. 6 – Micrographs of longitudinal cross section of Al–CNT composite by (a) optical microscopy and (b) FE-SEM.
 CARBON 4 7 (2 0 0 9) 5 7 0–57 7
thickness direction as a result of the rearrangement of the
bundled CNTs in the sintered compact (see Fig. 4d). This
microstructure was formed through the flowing of CNTs with
a large plastic deformation of the soft Al matrix by the high
extrusion pressure. The observations so far demonstrated
that the present method for the production of Al–CNT com-
posites is capable of providing a uniform CNT dispersion
and a higher degree of CNT orientation, as well as a dense
and fine microstructure. Such a microstructure is expected
to be very helpful in increasing the mechanical properties of
Al–CNT composites [29].
Fig. 7 shows the Raman spectra [30] of the raw CNTs,
debinded Al–CNT mixed powder, sintered Al–CNT compact,
and extruded bulk. The peaks at 1572.7 and around
1320 cm 1 correspond to a typical G-line (graphite) and D-line
(defect), respectively. The relative intensity between the two
peaks is known to provide information about the quality of
the internal CNTs. There was no change in either the magni-
tude or shape of the peaks from any of the processes. From
Fig. 7, the ratios of the peak intensity between the D-and G-
bands, ID/IG, were calculated as indicated in Table 1. The value
of ID/IG was nearly 0.8 after every process. This implies that no
structural change in the CNTs appeared for any of the
processes.
The general reason for a structural change in a CNT is a
reaction with oxygen at high temperature. However, in the
present process, the reaction of 4/3Al + O2 = 2/3Al2O3 might
occur at up to 2000 °C, with a higher priority than the CNT oxi-
dation, with reference to the Ellingham diagram [31]. In other
words, the CNT is hardly decomposed during this process,
which has a maximum temperature of 600 °C. Here, a slight
reduction of ID/IG in the debinding was found, but it arose
from the release of the residual stress in the CNTs by
annealing.
The macro-hardness of the extruded Al–CNT composite
was about 52 HV, whereas that of pure Al was 22 HV, as indi-
cated in Table 1. The CNT reinforcement would increase the
hardness by a factor of around two. However, it cannot be de-
nied that the work hardening by the extrusion enhanced the
hardness of the Al–CNT composites.
Fig. 7 – Raman spectra of the raw CNT, debinded Al–CNT
mixed powder, sintered Al–CNT compact, and extruded Al–
CNT composite.
575
Thus, we performed a nano-indentation to distinguish be-
tween the CNT reinforcement and the work hardening effects.
Nano-indentation [22,23], which is capable of measuring
hardness within a micrometer region, allows us to measure
the hardness of just the matrix, apart from the grain bound-
ary. In this study, the nano-indentation hardness of the raw
Al particles, inside the grain in the extruded pure Al, and
the Al–CNT bulks were measured for comparison. These mea-
surements showed that the Al powder and the extruded Al
bulk had the same hardness of 37 Hu, with the extruded Al–
CNT composite having a value of 40 Hu (see Table 1). This
small difference in hardness, which is interpreted as the work
hardening, scarcely affects the hardness enhancement. In
addition, because there was no change in the hardness of
the aluminum, even though the extrusion ratio was changed
[18], the dynamic recrystallization [32,33] and recovery are lar-
ger than the accumulation of the strain. In other words, it is
supposed that work hardening did not occur during the hot
extrusion process. Therefore, we conclude that the main con-
tribution to the increase in the hardness of the composite is
reinforcement from the CNTs.
Fig. 8 shows the true stress versus true strain curve of the
extruded Al–CNT composite, compared with the extruded
pure Al. The true tensile strength of the extruded Al–CNT
composite was 194 MPa, which is twice that of pure Al. More-
over, the composite maintained good ductility, with an elon-
gation of 10.1%. Here, the true tensile strength of pure Al is
generally reported to be about 100–110 MPa, whereas the ob-
tained true tensile strength of the extruded pure Al bulk in
this study was a lower value of 85 MPa. This disagreement ar-
ose from differences in fabrication processing and testing
conditions. In any case, a strength enhancement of more
than double was outstanding in comparison with other re-
ports [3,15,16,26,34,35].
As proven above, the extruded bulk does not include work
hardening. Therefore, the enhancement in strength came pri-
marily from the reinforcement effect of the CNTs. In particu-
lar, the aluminum carbide phases are supposed to bring out
the reinforcement effect. The aluminum carbide that was
generated during the sintering process was implanted into
Fig. 8 – True stress–true strain curve of the extruded Al–CNT
composite and the extruded Al bulk. Inset, the specimen
used for the tensile test.
576 CARBON 4 7 ( 2 0 0 9 ) 5 7 0 –5 7 7

Fig. 9 – TEM micrograph of the extruded Al–CNT composite. (a) Micrograph of the entire grain boundary, (b) the implanted
Al4C3 between the Al matrix and grain boundary.

Fig. 10 – FE-SEM micrograph of the fracture surface of the Al–CNT composite after tensile test. (a) Some dimples and (b) CNT
bridging (white arrow).

the aluminum matrix in the extrusion process, as seen in
Fig. 9. Such implanted aluminum carbides would conjoin
the Al matrix and the CNTs more strongly.
Fig. 10 shows an FE-SEM micrograph of the fracture sur-
face of the Al–CNT composite after the tensile test. The frac-
ture surface of the Al–CNT composite has a lot of dimples
associated with ductile fracture, as shown in Fig. 10a. The
appearance of these dimples means that the joining between
the Al particles was very strong. Detailed observation of the
dimple walls revealed a lot of bridging of the aluminum ma-
trix by the CNTs (arrow in Fig. 10b). In this case, any stress
in the matrix can be transferred to the CNTs by the aluminum
carbide [36–38]. Consequently, the tensile strength of the Al–
CNT composite in this study was increased.
4. Conclusion
We aimed to produce Al–CNT composites with well-dispersed
and regularly oriented CNTs using the nanoscale dispersion
(NSD) method, along with a combination of spark plasma sin-
tering (SPS) and hot extrusion processes.
The SPS could fabricate Al–CNT with a relatively high den-
sity and degree of orientation for the CNTs. The CNTs were al-
ready well dispersed prior to this step because the NSD was
used to produce a homogeneously mixed powder. Further-
more, grain growth in the matrix and damage to CNTs did
not occur during the SPS, because of the pinning effect by
the CNTs and oxides, and the rapid heating. A small quantity
of carbide was generated during the SPS process and thereby
affected a strong bonding between the Al matrix and CNTs.
The subsequent hot extrusion process allowed further
enhancements of density, dispersity, and CNT orientation.
As a result, the slight addition of 5 vol% CNTs could remark-
ably elevate the strength to about thrice that of pure Al. The
increase in the mechanical properties was attributed to par-
ticular strengthening by the CNTs, which strongly bonded
with the matrix through the generated aluminum carbide
phase.
 CARBON 4 7 (2 0 0 9) 5 7 0–57 7
However, the combination of SPS and hot extrusion pro-
cesses is effective for strengthening an Al–CNT composite.
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