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2020 Microstructural, Mechanical and Thermal Properties of Microwave
2020 Microstructural, Mechanical and Thermal Properties of Microwave
a r t i c l e i n f o a b s t r a c t
Article history: Cu nanocomposites reinforced with 0e6 vol% MWCNTs are fabricated using mixing, ball milling and
Received 8 November 2019 microwave sintering techniques. It is found that decreasing the Cu powders size from 65 to 15 mm
Received in revised form significantly enhances the mechanical and thermal properties of the fabricated nanocomposites. In
1 January 2020
addition, the optimal MWCNTs content in such composites is found to be 4 vol%; there exists maximum
Accepted 3 January 2020
Available online 7 January 2020
for microhardness, bending strength and thermal conductivity of Cu- MWCNT composites which rise to
82.2 HV, 155.2 MPa and 380.2 W.mk 1, respectively. However, the nanocomposites properties then fall to
75 HV, 139.5 MPa and 315.4 W.mk 1, respectively, with further increasing the MWCNT content up to 6 vol
Keywords:
Cu-MWCNT nanocomposite
%. Furthermore, the relative density of the pellets is calculated using Archimedes method, demonstrating
Microwave sintering a lower relative density for the composites with higher MWCNTs content. These findings provide a
Microhardness simple and effective sintering method for the engineering of low-cost metal matrix composites.
Thermal conductivity © 2020 Elsevier B.V. All rights reserved.
Relative density
https://doi.org/10.1016/j.jallcom.2020.153675
0925-8388/© 2020 Elsevier B.V. All rights reserved.
2 M. Darabi et al. / Journal of Alloys and Compounds 822 (2020) 153675
as severe plastic deformation (SPD) [29]. In addition, excessive other research which emphasizes the outstanding role of fine grain
grain growth caused by long sintering time at high temperature size of matrix and microwave energy absorption of reinforcement,
could lead to a weakened interfacial strength in the fabricated leading to improved properties. Findings of this research provide a
MMCs [29,30]. Hence, some rapid densification methods including simple and effective fabrication method for the engineering of low-
spark plasma sintering (SPS) and microwave sintering have been cost MMCs.
utilized due to their many inherent advantages over conventional
sintering technique [31e35]. 2. Experiment
Compared to SPS technique, microwave sintering could save up
to 85% of the sintering time as well as 96% of the energy [30], of- 2.1. Cu-MWCNT nanocomposites fabrication
fering lower sintering temperature, lower porosity and lower pro-
cessing cost [36e38]. Using spark plasma sintering, Guiderdoni For the synthesis of Cu- MWCNT nanocomposites, six batches of
et al. [15] fabricated homogenously dispersed double walled carbon copper powders with average particle size of 15, 25, 35, 45, 55 and
nanotubes (DWCNT) in Cu matrix, featuring significantly micro- 65 mm (supplied by Iran Powder Metallurgy Complex, with 99.9%
hardness (103 HV) for DWCNT/Cu composites compared to pure Cu purity) and one batch of MWCNT with a diameter of about 20 nm
samples. Using microwave sintering, Babu et al. [29] investigated (supplied by US nano of America with purity level of >95%) were
the effect of sintering time as well as CNT diameters on the me- used. Copper powders were mixed with MWCNTs in a planetary
chanical, electrical and thermal properties of the synthesized Cu- ball mill using a stainless-steel jar (the mass ratio of ball to powder
CNT composites. The optimal hardness of 80 HV, relative density was 10:1). The powders and MWCNTs were mixed under argon (Ar)
of 91% and electrical conductivity of 47 MS m 1 were obtained at atmosphere for 10 h at 120 rpm, to prevent oxide formation. Then,
60 min sintering time for the CNT average diameter of 20e40 nm the mixed powders were compacted in a uniaxial hydraulic press
[29]. In another research, Duan et al. [30] reported a hardness of 80 under the 450 MPa pressure for 60 s to obtain green pellets (Fig. 1)
HV for the Cu-0.5 wt% CNT composite fabricated by molecular-level with two different dimensions of 40 10 3 mm3 and 10 3 mm2.
mixing followed by microwave sintering technique. The micro-
hardness value decreased significantly from 80 to 55 HV by 2.2. Sintering procedure
increasing the CNT content from 0.5 wt% to 1 wt% which could be
attributed to the aggravated agglomeration in the composite with The green pellets were sintered for 20 min using a microwave
higher CNT content [1,30]. However, limited studies are conducted furnace (900 W, 2.45 GHz, LG Microwave furnace) equipped with Ar
on the role Cu powder sizes, as metal matrix, play on the micro- gas at a rate of 42 C.min 1 (Fig. 1). For higher overall heating rate,
structure as well as mechanical, electrical and thermal properties of the samples were placed in an alumina crucible and immersed in
CNT-Cu composites. Silicon Carbide (SiC) bed. This step provided the green pallets with
In our previous work [39], a simple comparison was conducted a hybrid heating facility as well as reduced the thermal gradient of
between conventional and microwave sintering methods, samples and the atmosphere around them, leading to the fabrica-
observing that a similar mechanical and electrical properties could tion of crack free components. In order to minimize the heat
be achieved in a significantly shorter synthesis time, when the transfer, the crucibles were covered by a layer of glass wool to
samples are sintered using microwave method compared to the eliminate the heat loss. Sintered specimens were then cooled down
conventional sintering techniques. Here, the effect of matrix grain to room temperature (Fig. 1).
size on the microwave mechanism, scattering of microwave energy,
and microwave energy absorption was investigated simulta- 2.3. Characterization
neously. In addition, the effect of Cu powder size as well as MWCNT
content on microstructural, mechanical, electrical and thermal Prior to characterization, the samples were mounted and
properties of microwave sintered Cu/MWCNT composites are grounded using 500 to 5000 grit SiC sandpapers, and then polished
investigated. Mechanical properties such as physical properties of with alumina based polishing slurry. The samples then were
fabricated samples were then characterized by measuring relative chemically etched by immersing in an etching solution of CrO3,
density and thermal conductivity as well as investigating the me- HNO3, H2SO4 and H2O, for 10 s. The Archimedes method was used
chanical properties, including microhardness and bending to measure the density of the sintered specimen according to ASTM
strength. Finally, the samples microhardness was compared with B311. The thermal conductivity of the samples was measured by
Fig. 1. The preparation process for fabricating Cu-MWCNT nanocomposites using mixing, ball milling and microwave sintering techniques.
M. Darabi et al. / Journal of Alloys and Compounds 822 (2020) 153675 3
Fig. 3. Interaction of different types of materials with microwaves: a) Transparent, b) Opaque, c) Absorber.
Fig. 4. (a) XRD patterns of Cu-4 vol% MWCNT powders and nanocomposites and magnified view of the main XRD peaks at 2q of (b) ~ 43.3 and (c) ~ 50.4.
circles) to 96.2% and 90.9% (blue circles), for the MWCNT content of for Cu(15 mm)-MWCNT nanocomposite and 66 HV for Cu(65 mm)-
0 vol% and 6 vol%, respectively. Further decrease in Cu average MWCNT nanocomposites. This higher microhardness is attributed
particle size down to 65 mm led to a lower relative density of 95.6% to the higher strength of MWCNT compared to pure Cu matrix. In
and 90.1% (blue rectangles) for the Cu-MWCNT nanocomposites addition, grain refinement as well as strong Cu/MWCNT interface
with 0 and 6 vol% MWCNT content, respectively (Fig. 5). formed during microwave synthesis could result in higher micro-
Higher relative density was reported for the Cu composites with hardness in the fabricated nanocomposites [30]. Increasing the
similar CNT content fabricated by SPS [15]. This lower density of the MWCNT content in the nanocomposites could ease the load
sample with higher MWCNT content could be attributed to the transfer from the Cu matrix to the harder MWCNT, resulting in an
slower densification of Cu powders in the presence of extra enhanced hardness value of the fabricated Cu-MWCNT nano-
MWCNT in the matrix [53]. Due to the higher melting point of composite. However, further increase in MWCNT content to 6 vol%
MWCNT compared to the copper matrix [54], higher MWCNT led to dramatic decrease in microhardness to 75 and 54 HV for the
content resulted in the formation of larger macro voids in the nanocomposites made of 15 and 65 mm Cu powders, respectively
microstructure, and consequently decreased the relative density of (Fig. 6a). This lower microhardness could be ascribed to the for-
the fabricated samples. In fact, increasing the size of macro voids in mation of larger micro voids as well as a greater number of ag-
the microstructure could be the main reason for lower density of glomerates in the nanocomposite with higher MWCNT content
the composites with higher MWCNT content [30]. Similar results [29].
were reported by Babu et al. [29] for Cu-CNT nanocomposites made Fig. 6b presents a comparison of microhardness obtained by Cu-
by 0.25e1.0 wt% CNT. The relative density of the fabricated nano- MWCNT nanocomposites fabricated in this research with similar
composites decreased from 87.1% to 80.8% by increasing the CNTs nanocomposites reported in the literature [55e58]. The micro-
content from 0.25 to 1.0 wt%. However, some materials processing hardness of 82 HV obtained by Cu-4 vol% MWCNT nanocomposites
techniques such as cold rolling could significantly increase the fabricated by microwave sintering technique was the highest value
relative density of these nanocomposites via eliminating these compared to similar reports. In contrast, the Cu-10 vol% MWCNT
macro voids [30]. In addition, for a wide range of MWCNT content nanocomposite fabricated by Shukla et al. [56] demonstrated the
from 1 to 6 vol%, the Cu(65 mm)-MWCNT nanocomposites featured lowest microhardness of 56 HV amongst others. Uddin et al. [55]
considerably lower relative density compared to Cu(15 mm)- reported a 32% increase in microhardness of Cu-0.5 vol% MWCNT
MWCNT ones. In fact, at the MWCNT content of 6 vol% the relative nanocomposite fabricated by hot press technique, compared to the
density of the fabricated samples were 93.5% and 90.1% for pure copper samples, which is in line with 39% increase in hardness
Cu(15 mm) and Cu(65 mm)-MWCNT nanocomposites, respectively. of Cu-4 vol% MWCNT nanocomposite, obtained in this research
(Fig. 6a). Moreover, Wei et al. [58] and Daoush et al. [57] succeeded
in achieving hardness of about 58 and 75 HV by preparing Cu-4 vol
3.4. Microhardness
% CNT and Cu-1 vol% CNT nanocomposite through powder metal-
lurgy technique and electroless deposition process respectively.
Fig. 6a shows the Vickers microhardness of pure Cu and Cu-
MWCNT nanocomposite samples with different MWCNT content
from 0 to 6 vol%. Regardless of MWCNT content, the nano- 3.5. Bending strength
composites made of smaller Cu powder size demonstrated a higher
microhardness compared to the samples fabricated by larger Cu Fig. 7 shows the bending strength of microwave sintered Cu-
micro-powders. This lower microhardness for nanocomposites MWCNT nanocomposites as a function of Cu powders size for
made by larger Cu powders could be attributed to a lower level of MWCNT content of 0 vol% up to 6 vol%. Regardless of Cu powders
microwave energy absorption and consequently higher level of average size, the bending strength of the fabricated nano-
micro-voids formed in the microstructure of these nano- composites reached a peak value of 155 MPa at 4 vol% MWCNT
composites, compared to the ones made of smaller Cu powders content, for nanocomposites made of 15 mm Cu powders size. This
[45]. higher bending strength of nanocomposites with high MWCNT
In addition, the microhardness of nanocomposites made by content could be attributed to the high elastic modulus and
15 mm powder size increased rapidly from 50 HV to 74 HV by strength of MWCNT as well as strong interface combination be-
increasing the MWCNT content from 0 to 2 vol% (Fig. 6a). At 4 vol% tween MWCNT and Cu matrix [39]. As a result, the load applied
MWCNT content, the microhardness value reached a peak of 82 HV during the bending strength test could be easily transfer from the
Fig. 6. (a) Microhardness of microwave sintered Cu-MWCNT nanocomposites made of Cu powders with 15, 25, 35, 45, 55 and 65 mm particle size as a function of MWCNT content.
(b) A comparison of microhardness obtained by Cu-MWCNT nanocomposites fabricated in this research (15 mm particle size) with similar nanocomposites reported in the literature.
6 M. Darabi et al. / Journal of Alloys and Compounds 822 (2020) 153675
Fig. 8. FESEM micrographs of fracture surface of Cu-6 vol% MWCNT nanocomposites made of 65 mm Cu powders.
M. Darabi et al. / Journal of Alloys and Compounds 822 (2020) 153675 7
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Declaration of competing interest of carbon nanotube buckling on the reinforcement of CNT/Cu composites,
Compos. Sci. Technol. 79 (2013) 28e34.
The authors declare that they have no known competing [21] J. Liu, U. Khan, J. Coleman, B. Fernandez, P. Rodriguez, S. Naher, D. Brabazon,
Graphene oxide and graphene nanosheet reinforced aluminium matrix
financial interests or personal relationships that could have composites: powder synthesis and prepared composite characteristics, Mater.
appeared to influence the work reported in this paper. Des. 94 (2016) 87e94.
[22] P.-C. Tsai, Y.-R. Jeng, J.-T. Lee, I. Stachiv, P. Sittner, Effects of carbon nanotube
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CRediT authorship contribution statement behaviors of carbon nanotube/copper composites, Diam. Relat. Mater. 74
(2017) 197e204.
Marjan Darabi: Data curation, Formal analysis, Investigation, [23] H. Ghodrati, R. Ghomashchi, Effect of graphene dispersion and interfacial
bonding on the mechanical properties of metal matrix composites: an over-
Methodology, Visualization, Writing - original draft. Masoud view, FlatChem 16 (2019) 100113.
Rajabi: Conceptualization, Methodology, Supervision, Writing - [24] B. Chen, S. Li, H. Imai, L. Jia, J. Umeda, M. Takahashi, K. Kondoh, An approach
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Validation, Visualization, Writing - review & editing. [25] A. Radhamani, H.C. Lau, S. Ramakrishna, CNT-reinforced metal and steel
nanocomposites: a comprehensive assessment of progress and future di-
Acknowledgement rections, Compos Part A Appl Sci Manuf 114 (2018) 170e187.
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The authors are grateful for the research support of Iran National of thermal conductivity in copper matrix composites, Scr. Mater. 63 (4) (2010)
Science Foundation with this research work. 375e378.
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