Diamond & Related Materials 107 (2020) 107907

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Diamond & Related Materials

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

Carbon nanotubes reinforced aluminum matrix composites with high T

elongation prepared by flake powder metallurgy
⁎ ⁎
N.Y. Li1, C. Yang1, C.J. Li , H.D. Guan, D. Fang, J.M. Tao, Y.C. Liu, J.H. Yi
Faculty of Materials Science and Engineering, Kunming University of Science and Technology, 650093 Kunming, China
Key Lab.(MOE) of Advanced Materials of Rare and Precious and Nonferrous Metals, Kunming University of Science and Technology, 650093 Kunming, China

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

Keywords: High elongation aluminum matrix composites reinforced with carbon nanotubes (CNTs) were prepared by flake
Carbon nanotubes powder metallurgy, and densified by hot extrusion with a high extrusion ratio. After hot extrusion, fine and
Al matrix composite equiaxed grains were obtained in 2 wt% CNT/Al composite, and interfacial product (Al4C3) as well as bridge-
Flake powder metallurgy connected CNTs aligned along the extrusion direction were found both in 1 wt% CNT/Al and 2 wt% CNT/Al
Hot extrusion
composites. Both composites obtained high elongation while their strength was enhanced. Especially the elon-
High elongation
gation of 2 wt% CNT/Al composite is comparable to that of pure Al prepared by the same method, which
reached about 30%. The good ductility mainly attributes to firm interfacial combination between CNTs and
matrix, fine and equiaxed grains formed by dynamic recrystallization during hot extrusion, and bridge-con-
nected CNTs aligned along the extrusion direction.

1. Introduction arrangement of CNTs, forming good CNT/Al interfacial combination,

and obtaining fine and equiaxed grains in the matrix are three critical
As an ideal reinforcement of composites, carbon nanotubes (CNTs), factors to efficiently fabricate high performance CNT/Al composites
more and more attention has been paid owing to its unique properties, with excellent ductility [12,13].
such as low density, excellent mechanical properties, prominent elec- Spherical Al powders limit the adsorption of CNTs on its surface,
trical properties since it's discovered in 1991 [1,2]. Numerous re- owing to the existence of curvature effect which is caused by the in-
searchers investigated the preparing technology, microstructure, and compatibilities of morphology and size between spherical Al powders
properties of CNTs reinforced metal matrix composites in the past two and CNTs [14]. For flaky powder metallurgy, flaky Al can overcome the
decades, especially CNTs reinforced Al matrix (hereafter named CNT/ curvature effect to a great extent, which increases the contact area
Al) composites after the first article reported in 1998 [3,4], owing to between Al powders and CNTs, thus improving the morphology and
their high specific strength and modulus, and great potential applica- size compatibilities between Al powders and CNTs. What's more, the
tion value in transportation and space industry. A large amount of adsorption amount of CNTs increases greatly, especially for longer
achievements have been carried out on preparing methods and in- CNTs. Therefore, it has been widely used to prepare CNT/Al compo-
creasing the strength of composites [5–8]. However, most of previous sites. Xu et al. [15] fabricated CNT/Al composites by this method
work improved the strength of CNT/Al composites at the expense of combined with different speed of ball milling, acquiring evenly dis-
ductility. Especially when the content of carbon nanotubes (CNTs) ex- persed CNTs with relatively complete structure, as well as good CNT/Al
ceeds 1 wt%, CNT/Al composites are much more brittle and prone to interfacial combination, and the ductility of the composite reached
destructive fracture. Hence improving the ductility of CNT/Al compo- nearly 12%. Chen et al. [11] fabricated CNT/Al composites by this
sites has become an important task. method with high sintering temperature, and the ductility of the com-
To solve this problem, there are three key factors should be con- posite reached nearly 20%. Fan et al. [10] also used flake powder
sidered: (I) the dispersion and arrangement of CNTs; (II) the CNT/Al metallurgy to prepare CNT/Al composites, followed by hot pressing
interfacial combination; (III) the grain size and morphologies of Al sintering and hot extrusion to make bulk nearly completely dense, and
matrix [9–12]. Acquiring uniform dispersion and directional the ductility of the composite reached nearly 9%. Appropriate

⁎
Corresponding authors at: Key Lab.(MOE) of Advanced Materials of Rare and Precious and Nonferrous Metals, Kunming University of Science and Technology,
650093 Kunming, China.
E-mail addresses: lcj@kust.edu.cn (C.J. Li), yijianhong@kust.edu.cn (J.H. Yi).
1
These authors contributed equally to this work.

https://doi.org/10.1016/j.diamond.2020.107907
Received 15 February 2020; Received in revised form 15 April 2020; Accepted 28 April 2020
Available online 30 April 2020
0925-9635/ © 2020 Elsevier B.V. All rights reserved.
N.Y. Li, et al. Diamond & Related Materials 107 (2020) 107907

formation of interface products between CNTs and Al matrix can im- in Fig. 1. Firstly, 200 ml absolute ethyl alcohol and 0.3 g CNTs or 0.6 g
prove the interfacial combination, hence promoting load transfer and CNTs were placed together into a beaker and ultrasonic oscillated for
inhibiting the propagating of cracks, which can improve the strength 1 h to get suspensions with different CNTs content. Meanwhile, 30 g
and ductility of CNT/Al composites simultaneously. Xu et al. [16] raw spherical Al powders and 300 g steel balls with a diameter of 8 mm
prepared Al matrix composite reinforced by CNTs and in situ Al4C3 by were placed together into a cemented carbide jar in an argon atmo-
two-step ball milling, which showed high elongation of 19.5%. Liu et al. sphere glove box. Pre-milling was executed at a speed of 400 rpm for
[17] improved the interfacial combination by adding Ti particles into 4 h to obtain the flaky Al powders. Secondly, the prepared flaky Al
CNT/Al composite, and TiAl3 and TiC can be found in the micro- powders, CNTs suspensions and 300 g steel balls were placed together
structure of composite, indicating the elongation was improved with into a cemented carbide jar and ball milled for 6 h at a speed of 300 rpm
the increase of Ti content. Good interfacial combination can also be to get CNT/Al composite slurries. Then, the CNT/Al composite slurries
obtained by chemical vapor deposition (CVD) method. Zhou et al. [18] were filtrated, and the mixed powders were vacuum dried at 50 °C for
fabricated the CNT/Al composites with CVD method and a balanced 12 h. Finally, the mixed powders were consolidated into ϕ28 mm cy-
amount of Al4C3 was generated at the CNT/Al interface by proper heat linders by spark plasma sintering for 20 min under the condition of
treatment, the ductility of composite reached almost 25%. Yang et al. 600 °C and 50 MPa. Then, the sintered cylinders were hot extruded into
[19] used CVD method to grow CNTs on the surface of Al particles ϕ6 mm rods at the temperature of 500 °C, which adopted a high ex-
firstly, and then prepared CNT/Al composites by flake powder me- trusion ratio (31,1). Pure Al as the comparison material was fabricated
tallurgy, obtaining evenly dispersed CNTs with good interfacial com- by the same method.
bination, and the ductility of the composite reached almost 20%. The
acceptable ductility of the composites prepared by flake powder me-
tallurgy has been obtained, but it is still not high. Furthermore, some 2.2. Characterization
preparation processes are extremely complicated and the related
parameters are difficult to control during the long preparing process. X-ray diffractometer with Cu Kα radiation (Empyrean, Palmernaco)
In this work, to improve the ductility of CNT/Al composite, Pure Al, was used to identify phase information of the composites. Raman
1 wt% CNT/Al composite (hereafter named composite 1) and 2 wt% spectroscopic (LabRAM, HR800, HORIBA), and the defects of CNTs can
CNT/Al composite (hereafter named composite 2) were fabricated by be characterized by intensity ratio (ID/IG) of damage-band to graphite-
flake powder metallurgy combined relatively simple ball-milling, spark band. Particle size and morphology of Al powders, the size and dis-
plasma sintering and hot extrusion with a high extrusion ratio. The tribution of carbon nanotubes, fractography of tensile samples were
results show a remarkable improvement on ductility of CNT/Al com- observed by field emission scanning electron microscopy (FESEM; Nova
posites, and the microstructure, tensile mechanical properties and Nano 450; FEI). The fine structure of Al matrix after extrusion, the
toughening mechanisms of the composites were investigated. arrangement of carbon nanotubes in Al matrix, and the in-situ formed
Al4C3 were examined by transmission electron microscopy (TEM, FEI
Tecnai G2 TF30, S-Twin) at 200 kV. For the preparation of TEM sam-
2. Experimental
ples, 3 mm slice samples with a diameter of 3 mm were mechanical
grinded to the thickness of 100 μm, and further thinned by the Gatan
2.1. Materials and methods
Precision Ion Polishing System at 5 kV. Tensile testing for pure Al and
CNT/Al composites were measured on a mechanical tester (AG-X-100
Spherical pure Al (purity of 99.95%) powders and hydroxylated
kN; Shimadzu) at room temperature with a strain rate of 0.5 mm/min.
multi-walled carbon nanotubes (MWCNTs) as raw materials. The dia-
meter and the length of MWCNTs are 30–80 nm and 5–30 μm, re-
spectively. The fabrication process of composite powders is illustrated

Fig. 1. Fabrication process of CNT/Al composite powders.

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N.Y. Li, et al. Diamond & Related Materials 107 (2020) 107907

Fig. 2. SEM images of Al powders before and after ball milling: (a) raw spherical Al powders, (b) flaky Al powders.

3. Results Table 1
ID/IG ratio of raw CNTs and CNTs in ball-milled composite powders.
3.1. Microstructure of pure Al powders and composite powders CNT Raw 1 wt% CNTs in ball-milled 2 wt% CNT in ball-milled
CNTs composite powders composite powders
Fig. 2(a) is the morphology of raw Al powders, which appears
spherical shape on the whole with the average particle size about ID/IG 0.79 0.88 0.89

25 μm. For increasing the attachment surface between Al and CNTs and
making CNTs uniformly distribute on Al powders, Al powders changed
agglomerations can be observed. Meanwhile, some fragmented CNTs
from spherical shape into flaky shape with the thickness of 10 μm ap-
produced from ball milling can be found, and the lengths of CNTs are
proximately after pre-milling owing to the effect of intense shear force
different. It also indicates that the addition of absolute ethyl alcohol as
during ball milling as illustrated in Fig. 2(b).
process control agent can effectively reduce the agglomeration and
Fig. 3 shows the XRD patterns of pure Al and ball-milled CNT/Al
damage of CNTs, and disperse them into Al powders evenly during ball
composite powders, revealing no peaks other than Al. The degree of
milling.
structural integrity of CNTs can be characterized by intensity ratio (ID/
IG) of damage-band (ID~1340 cm−1) to graphite-band (IG
3.2. Microstructure of CNT/Al composites
~1570 cm−1). ID/IG value of Raman spectra of the raw CNTs and CNT/
Al composite powders after ball milling of 6 h is listed in Table 1. The
After spark plasma sintering, CNT/Al composites were further
ID/IG of raw CNTs is approximately 0.79, and increased to about 0.88
densified by hot extrusion. In TEM images of CNT/Al composites, the
for 1 wt% CNT/Al composite powders, and 0.89 for 2 wt% CNT/Al
reaction product Al4C3 can be found in both composite 1 and composite
composite powders, respectively. The slight increase of ID/IG indicates
2, which was in-situ formed during sintering and hot extrusion, as il-
that there is no noticeable structure damage of CNTs during ball mil-
lustrated in Figs. 5(b), (c) and 6. It can be seen from Fig. 6 that the
ling, which means that absolute ethyl alcohol as process control agent
sharp of many Al4C3 in composite 2 is short rod with small size, and can
can not only prevent flaky Al powders from cold welding, but also
be identified that Al4C3 are mostly produced by fragmented CNT
protect the CNTs structure from being damaged badly.
[Fig. 6(a), (b) and (c)] and small part of relatively complete CNT
Fig. 4 exhibits the morphologies of the CNTs distributed on the flaky
[Fig. 6(a)]. The average size of Al4C3 in composite 2 has been calcu-
Al powders. It can be observed from the figures that CNTs are almost
lated, which is about 79.72 nm, as illustrated in Fig. 6(d). The forma-
evenly distributed on the surface of flaky Al powders due to the me-
tion of Al4C3 is primarily attributed to the diffusion of Al and C atoms.
chanical cutting effect of ball milling [5], and few obvious
The nucleating and growing of Al4C3 occurs mostly on the top or the
surface of CNTs during heating. Especially the fragmented CNTs gen-
erated from ball milling, which can be a source of C atoms and facilitate
the fragmented CNTs to transform into Al4C3 rods [20]. The formation
of Al4C3 rods also manifests that interfacial combination between CNTs
and Al matrix is very strong and helpful to enhance the composites.
TEM images of microstructures of composite 1 and composite 2 after
hot extrusion are shown in Fig. 5. As shown in Fig. 5(a), the
morphologies of Al matrix grains in composite 1 appear strip-shaped
due to the plastic flow of Al matrix during extrusion deformation.
Compared with the microstructure of composite 1, the morphologies of
Al matrix grains in composite 2 are fine and equiaxed [Fig. 5(d) and
(e)]. The average grain size of Al matrix of composite 2 has been cal-
culated and the statistical result is illustrated in Fig. 5(f), which is about
440 nm. That implies that the formation of such a microstructure (fine
and equiaxed grains) of composite 2 after hot extrusion is due to the
occurrence of dynamic recrystallization in the Al matrix, and fine and
equiaxed grains are beneficial to the ductility of composite. However,
Al is a high stacking fault energy metal, and a lot of CNTs exist in the
matrix can inhibit the growth of grains due to Zener pinning, making it
less prone to dynamic recrystallization. But during hot extrusion with a
Fig. 3. XRD patterns of pure Al and CNT/Al composite powders. high extrusion ratio (31:1), high storage dislocation energy induced by

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N.Y. Li, et al. Diamond & Related Materials 107 (2020) 107907

Fig. 4. SEM images of morphologies and CNTs dispersion of (a) 1 wt% CNT/Al composite powders and (b) 2 wt% CNT/Al composite powders.

drastic plastic deformation can possibly provide a strong driving force Additionally, Fig. 5(a) and (e) show that CNTs in composite 1 and
to overcome the pinning force for grain boundaries and promote the composite 2 are basically aligned along the direction of extrusion,
occurrence of dynamic recrystallization in Al matrix significantly [13]. forming bridge connection arrangement, which may benefit the com-
Additionally, according to statistics result of Al4C3 size (79.72 nm) posite to obtain good mechanical properties. The formation of this di-
[Fig. 6(d)], it means there are many nano-sized fragmented CNTs in the rectional arrangement is the result of the movement of CNTs along with
microstructure of composite 2. During dynamic recrystallization of Al the plastic flow of Al matrix during hot extrusion.
matrix, nucleating and growing of new grains occurs owing to the ex-
istence of more fragmented CNTs, and eventually obtain fine and
equiaxed grains [21], which is helpful to increase the strength and 3.3. Mechanical properties of extruded CNT/Al composites
ductility of the composite. Similar microstructures of dynamic re-
crystallization are also discovered in the composites reinforced by small Tensile engineering stress−strain curves of the pure Al and CNT/Al
particles after severe plastic deformation [13,22]. composites are illustrated in Fig. 7. As it shown, the tensile strength of
composite 1 and composite 2 reach 152 MPa and 144 MPa,

Fig. 5. TEM images of composite 1 and composite 2 after extrusion: morphologies of Al matrix grains in composite 1 (a) and composite 2 (d) after extrusion, (b) (c)
morphologies of Al4C3, (e) the arrangement of CNTs after extrusion in composite 2, (f) the statistics result of grain size in composite 2.

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N.Y. Li, et al. Diamond & Related Materials 107 (2020) 107907

Fig. 6. TEM images of composite 2 after hot extrusion: (a) (b) (c) some Al4C3 distributed in the matrix of composite 2, (d) statistics result of the average length of
Al4C3 in composite 2.

respectively, which is increased about 103% and 92% compared with suggesting the good plasticity of both pure Al and composite 2. The size
that of pure Al (80 MPa). The tensile strength was enhanced by the and depth of ductile dimples of pure Al and composite 2 are almost the
addition of carbon nanotubes, which is consistent with most conclu- same, indicating the ductility of two samples is almost close. Fig. 9(c)
sions of related reports [4,9,14,23,24]. Three strengthening mechan- shows the FESEM images of fractography of composite 2, which further
isms have been put forward for CNT/Al composites, including Orowan demonstrating a good ductility of the composite. Additionally, there are
strengthening, load transfer and thermal mismatch strengthening [25]. some small cracks (hereafter named microcracks) on the fracture sur-
Therefore, there is not much retelling of strengthening mechanisms of face of composite 2. A few agglomerations of CNTs can be found in the
CNT/Al composite in this study, and we concentrate more attention on cracks from the Fig. 9(b), indicating the microcracks are mostly gen-
the analysis of the toughening mechanism of CNT/Al composite. erated from the agglomerations of CNTs. However, the cracks in the
Compared with the tensile mechanical properties of most studies on composite are very small and discontinuous, suggesting the propagation
CNTs reinforced Al matrix composites, more prominent is the ductility of cracks was restrained by something during the deformation of the
in this work. A slight decrease in elongation occurred to composite 1 composite. In addition, some pointed protrusions are discovered on the
(nearly 23%) compared to pure Al, and composite 2 has almost the fracture surface, which are pulled out CNTs, as shown in Fig. 9(a) and
same ductility as pure Al (nearly 30%). That is to say, the CNT/Al (d).
composites possess good comprehensive mechanical properties.
The SEM images of the fractography of pure Al [Fig. 8(a) and (b)]
and composite 2 [Fig. 8(c) and (d)] are exhibited in Fig. 8. There are 4. Discussion
numerous ductile dimples can be observed in both of samples,
CNTs can be transformed into large sized Al4C3 rods owing to

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N.Y. Li, et al. Diamond & Related Materials 107 (2020) 107907

smallest average size of Al4C3 rods (~82 nm) with the highest elon-
gation (~15%) among all composites, and proved that the size of Al4C3
is the most important factor affecting the mechanical properties of
composite. Xu et al. [8] prepared 2 wt% CNT/Al composite by long
time ball milling (24 h), and the average Al4C3 rods size in the com-
posite is about 148.8 nm, obtaining the elongation of the composite is
15.8%. In this work, the average size of the Al4C3 short rods in com-
posite 2 are controlled very small (~79.72 nm) while the interfacial
combination is improved, and therefore obtains more outstanding
elongation (30%). Microcracks are not easy to generate and propagate
at the interface during plastic deformation due to the existence of
strong interfacial combination.
Compared with composite 1, the formation of such a microstructure
in composite 2 may be attributed to two reasons. On one hand, the more
addition of CNTs promotes Al matrix to undergo more severe plastic
deformation during ball milling, and generates more deformation sto-
rage energy due to the high density dislocations induced by the inter-
action between fragmented CNTs and dislocations, which is helpful to
Fig. 7. The engineering tensile stress-strain curves of pure Al, composite 1 and promote Al matrix to undergo dynamic recrystallization during hot
composite 2. extrusion [27,28]. On the other hand, the existence of more fragmented
CNTs can possibly facilitate to the occurrence of nucleating and
growing of new grains due to the effect of heterogeneous nucleation
enhanced diffusion when the sintering temperature is very high and
during dynamic recrystallization, finally acquiring fine and equiaxed
over long time. Al4C3 is a brittle phase, and too much Al4C3 will have
grains [21]. During dynamic recrystallization, nano-sized fragmented
severely negative effect on the mechanical properties of composite. It is
CNTs as the nucleus and promote the nucleating of new grains, which
need to make sure that sintering and extruding can be achieved
makes the distribution of fragmented CNTs changes from grain
smoothly and do not generate too much Al4C3, hence 600 °C SPS and
boundary to intra grain, and the homogeneity of grain size can be im-
500 °C hot extrusion were conducted during the preparation of CNT/Al
proved [21,29]. Therefore, the connection between Al grains has been
composites. The strong interfacial combination can be acquired by
improved owing to intergranular particles transforming into in-
forming appropriate amount of Al4C3, which can promote load transfer
tragranular particles during dynamic recrystallization [30]. The fine
and enhance the fracture elongation of CNT/Al composite [9,18,26].
and equiaxed grains can disperse more stress, so that the deformation is
Guo et al. [20] fabricated the Al-SiC-CNTs composite, and formed dif-
more uniform and does not cause higher stress concentration. In addi-
ferent sizes of Al4C3 rods by different heat treatment temperature, in-
tion, more grain boundaries produced by grain refinement can
dicating that the composite was heat-treated at 530 °C possesses the

Fig. 8. SEM images of fracture surface morphologies: (a) (b) pure Al, (c) (d) composite 2.

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N.Y. Li, et al. Diamond & Related Materials 107 (2020) 107907

Fig. 9. FESEM images of fracture surface morphologies of composite 2.

effectively restrain the propagation of microcracks during plastic de- with a high extrusion ratio. CNT/Al composites obtained good com-
formation, which makes composite less prone to fracture. prehensive mechanical properties balanced strength and ductility.
CNTs in both composites aligned along the direction of hot extru- Especially the elongation (30%) of 2 wt% CNT/Al composite is com-
sion form the bridge connection arrangement, which also play a sig- parable to that of pure Al prepared by the same method, which is
nificant role in restraining the propagation of microcracks during mainly attributed to the firm interfacial combination between CNTs and
plastic deformation. Microcracks mostly originate from the agglom- Al matrix, fine and equiaxed grains and bridge-connected CNTs aligned
erations of CNTs and grain boundaries. For one thing, bridge-connected along the extrusion direction.
CNTs are more favorable to effectively transfer load from Al matrix to
themselves when the stress is concentrated, and prevent form the for- Declaration of competing interest
mation of a high stress concentration in a certain area. For another,
bridge-connected CNTs can restrict the microcracks in a quite narrow The authors declare that they have no known competing financial
space, which can make microcracks be completely inhibited. This fur- interests or personal relationships that could have appeared to influ-
ther confirms that cracks in composite 2 are quite small and dis- ence the work reported in this paper.
continuous, as shown in the fractography [Fig. 8(c) and (d)].
According to Fig. 9(b), it indicates that microcracks are mainly Acknowledgment
originated from the CNTs agglomerations, and this is the negative effect
brought by CNTs. However, small microcracks (≤10 μm) with dis- The authors acknowledge the supports from the Science Foundation
continuous distribution means the cracks had been restrained com- of the Yunnan Provincial Science and Technology Department (grant
pletely in the process of propagation [Fig. 8(c) and (d)], and bridge- 2018FB085) and the Rare and Precious Metal Materials Genome
connected CNTs, fine and equiaxed grains play significant roles in re- Engineering Project of Yunnan Province [grant 2018ZE007,
stricting the propagation of microcracks, which can effectively elim- 2019ZE001-3].
inate this negative effect brought by CNTs agglomerations, and have a
greater contribution to the improvement of elongation. Hence, the high References
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