MA TE RI A L S CH A R A CT ER IZ A TI O N 8 6 (2 0 1 3) 3 9 4 8

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Mechanical characterization of copper coated carbon nanotubes reinforced aluminum matrix composites
Adnan Maqboola,b,, M. Asif Hussaina , F. Ahmad Khalida , Nabi Bakhsha , Ali Hussainb , Myong Ho Kimb
a b

Faculty of Materials Science and Engineering, GIK Institute of Engineering Sciences and Technology, Topi 23640, KP, Pakistan School of Nano and Advanced Material Engineering, Changwon National University, Gyeongnam 641-773, Republic of Korea

AR TIC LE D ATA
Article history: Received 6 April 2013 Received in revised form 16 August 2013 Accepted 18 September 2013

ABSTR ACT
In this investigation, carbon nanotube (CNT) reinforced aluminum composites were prepared by the molecular-level mixing process using copper coated CNTs. The mixing of CNTs was accomplished by ultrasonic mixing and ball milling. Electroless Cu-coated CNTs were used to enhance the interfacial bonding between CNTs and aluminum. Scanning electron microscope analysis revealed the homogenous dispersion of Cu-coated CNTs in the composite samples compared with the uncoated CNTs. The samples were pressureless sintered under vacuum followed by hot rolling to promote the uniform microstructure and

Keywords: Aluminum matrix composites CNTs Copper electroless plating Powder processing

dispersion of CNTs. In 1.0 wt.% uncoated and Cu-coated CNT/Al composites, compared to pure Al, the microhardness increased by 44% and 103%, respectively. As compared to the pure Al, for 1.0 wt.% uncoated CNT/Al composite, increase in yield strength and ultimate tensile strength was estimated about 58% and 62%, respectively. However, in case of 1.0 wt.% Cu-coated CNT/Al composite, yield strength and ultimate tensile strength were increased significantly about 121% and 107%, respectively. 2013 Elsevier Inc. All rights reserved.

1.

Introduction

Aluminum has always been an area of interest when reinforced with hard particles and fibers to improve its mechanical performance and making it suitable for numerous structural applications [1]. The aluminum matrix composites (AMCs) possess higher stiffness, hardness and good wear resistance properties while maintaining high strength-toweight ratio. AMCs were widely studied by using various type of reinforcements such as SiC [25], BC [6], Al2O3 [7,8], TiB2 [9] and graphite [10]. During past few decades, carbon nanotubes (CNTs) have attracted much research attention. Especially composite materials, they are predicted as ideal reinforcement for manufacturing of aircrafts and sports goods, due to their high aspect ratio, strength, elastic modulus and low

density [11,12]. Many researchers have used CNTs as reinforcement in the metal matrix such as CNT/Al composites. However, no major breakthrough has been achieved with the CNT/Al composites, because of obstacles related to interfacial bonding between Al powder and CNTs, and unavailability of suitable synthesis techniques for their homogenous mixing at molecular level [13,14]. In addition, their poor wetting property on Al due to entanglement and difference in densities are great hindrances in their uniform distribution for manufacturing of composites [15]. For composites such as Co/CNT, Ni/CNT and Cu/CNT, novel fabrication techniques have been used to obtain outstanding composite powders, because metal oxides (CuO and CoO) can be easily reduced to their respective metals (Cu and Co) [16,17]. Unfortunately, the fabrication of CNT/Al composites is not feasible through solution reduction process.

Corresponding author at: School of Nano and Advanced Material Engineering, Changwon National University, Gyeongnam 641-773, Republic of Korea. Tel.: +82 10 7309 9455; fax: +82 55 262 6486. E-mail addresses: adnanmaqbool247@gmail.com, adnan@changwon.ac.kr (A. Maqbool). 1044-5803/$ see front matter 2013 Elsevier Inc. All rights reserved. http://dx.doi.org/10.1016/j.matchar.2013.09.006

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The literature has suggested that CNT/Al composites have been actively studied among CNT/metal composites due to possible application in the next generation materials for automobile, sports and aerospace industries. Bakshi et al. reported a comprehensive review on CNT/metal composites [18] and CNT/ Al composites [19]. CNT/Al composites have been synthesized by several routes, such as plasma spray coating [20,21], electrodeposition [22], squeeze casting [23], conventional ball milling [14,2428] and high energy ball milling process (HEBM) [2939]. In most of these studies, various combinations of consolidation and post-sintering routes have been suggested such as spark plasma sintering (SPS) [3743], spark plasma extrusion [31], hot extrusion [3436,44] and hot rolling [32,33]. Due to better dispersion of CNTs, HEBM process shows improvement in mechanical performance, but strengthening ability of CNTs is still below the expectation due to damage of the CNTs. Kwon et al. fabricated CNT/Al composites by dispersion in natural rubber and a combination of processes of SPS and hot extrusion to get highly densified CNT composites [40,41]. Deng et al. performed isostatic pressing, followed by hot extrusion process. They distributed CNTs on the surface of 2024-Al powder by mechanical mixing assisted with ultrasonic shaker and fabricated composites which showed increased tensile strength, hardness and Young's modulus [2426]. Liao et al. fabricated CNT/Al composites by mixing the composite powder in the roller mill followed by SPS and hot extrusion [4244]. Laha et al. fabricated CNT/Al composites by plasma spray forming process. They utilized AlSi eutectoid composite to produce a thin layer of SiC on the surface of CNTs which enhanced the interfacial bonding and wettability of CNTs with Al matrix [20,21]. He et a1. developed in-situ synthesis method by coating 1 wt.% Ni nanoparticles on Al powder and direct CVD growth of CNTs on Al powder to fabricate 5 wt.% CNT/AlNi composite [45,46]. Recently, Nam et al. utilized 4 wt.% AlCu powders to prepare CNT/AlCu composite by mechanical alloying [38,39]. CNT/Cu composite powders fabricated by molecular level mixing process and Al powders were mixed by HEBM process. As Bakshi et al. [19] and Nam et al. [38] summarized the strengthening mechanism in CNT/Al composites, homogenous dispersion of CNTs and strong interfacial bonding between CNTs and Al is necessary for higher strength in composites. Therefore, such a process is required which can establish a strong interface between CNTs and Al matrix without damaging the CNTs. In this study, we have synthesized CNT/Al composites to achieve uniform dispersion of CNTs in Al matrix. CNTs were coated with Cu to improve the wettability and interfacial bonding between CNTs and Al. Furthermore, the effects of Cu-coated CNTs and uncoated CNTs on the mechanical behavior of composites were investigated. The grain size is also a contributing parameter in determining the performance of composites. In addition, the influence of Cu coating on CNTs and grain size was also ascertained for the properties of composites.

Co. Ltd., China) and multi-walled carbon nanotubes (Sun Nanotech Co. Ltd., China, purity > 90%, diameter 1030 nm) were used in the present study. Two processes: electroless plating and ultrasonic assisted mixing with N2 purging were utilized for the uniform distribution of CNTs. For the enhancement in interface bonding of Al matrix and CNTs, a Cu/CNT precursor was prepared by using an electroless plating process and then mixed by ball milling with Al powder. Cu-coated and uncoated CNTs were used as the reinforcement in the Al matrix. To get rid of the metallic particles and other impurities, purification and functionalization of CNTs were carried out by acid treatment in conc. HCl, H2SO4 and HNO3. Purification of CNTs was done in conc. HCl (37%), sonicated at 30 C for 5 h and were then soaked for 12 h. Functionalization of purified CNTs was done by mixing conc. HNO3 (65%) in conc. H2SO4 (98%) in the ratio of (1:3).

2.2.

Ultrasonic-assisted Electroless Plating

Two-step sensitization and activation method was performed for CNTs. After this, CNTs were exposed to catalytic treatment of mixing with CuSO45H2O bath for 2 h at room temperature to suspend the CNTs in the solution. Formaldehyde was added in order to reduce the copper in the bath for 20 min. The bath composition was adjusted for the fixed Cu-CNT (1:1) wt. ratio i.e. for 50 mg CNTs, bath composition was adjusted according to copper content in the bath. The plating solution composition was CuSO45H2O (196 g), Na3C6H5O72H2O (532 g), NaOH was used to adjust pH equal to 12 and formaldehyde (1 ml) was added drop wise in the solution.

2.3.

Ultrasonic Mixing and Ball Milling

Ultrasonic assisted mechanical mixing of the Al and different compositions of uncoated and Cu-coated CNTs named by CNT addition (0.25, 0.50, 0.75 and 1.0 wt.%) were performed in ethanol. To facilitate uniform distribution and mixing of CNTs, mixture was sonicated at 60 C. Nitrogen gas was bubbled from bottom of the beaker by a glass rod that further enhanced the dispersion of Al powder with CNTs by avoiding powder sedimentation, process details are given in another study [47]. The process was continued until the thick slurry of the CNT/Al mixture was obtained. Then, 12 g of mixed powder was placed in 250 ml stainless steel mixing jars together with the stainless steel balls of 8 mm (). The ball to weight ratio was also adjusted to (10:1). The jars were filled with argon gas and planetary ball mill was used for the mixing of powders at 200 rpm for 1 h. Ethanol was used as the process control agent (PCA) to minimize the cold welding of particles and to avoid sticking of powder with balls and walls of the jar. Uniaxial cold compaction of ball milled powder at 600 MPa was done by hydraulic press in 13 mm high-speed steel die. Pressureless sintering in the quartz tube was performed in the tube furnace at 550 C for 3 h under high vacuum at 10 4 mbar.

2.
2.1.

Experimental Procedures
2.4. Fabrication of CNT/Al Composites
For the preparation of CNT/Al composites with uniform dispersion of CNTs, different combinations of powder metallurgy processes were utilized. Hot rolling of composites was

Hot Rolling

For the fabrication of the composites, gas atomized Al powder (99.84% pure, with 10 m average particle size, Angang Group

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done at 480 C with 0.25 mm per pass reduction. For CNT/Al composites with regular orientation of the CNTs, thickness of the samples reduced up to 40 and 80%. In order to relieve the stresses and improve the tensile properties, hot rolled composites were undergone in the annealing process. All the samples with 80% reduction in thickness were annealed at 500 C for 6 h.

2.5.

Characterization

X-ray diffraction (XRD) (Philips Panalytical X-pert, Model PW 3710) with Cu K radiations, was used to obtain the diffraction patterns. Olympus B061 microscope was used to reveal the microstructure of samples. In order to reveal the CNTs and grain boundaries, the Al matrix was preferentially etched. Etching was performed at room temperature in a solution of 2 g NaOH, 4 g Na2CO3 and 94 ml of H2O [31]. Scanning electron microscopy (SEM) was used to examine the distribution of CNTs within the CNT/Al composites. Microhardness was evaluated with Vickers Hardness testing machine. To measure the microhardness, Vickers microindenter was used at a load of 100 gf. Each hardness value datum was the average of 3 samples, whereas hardness of each sample was determined from a minimum of 10 indents. Tensile loading unloading tests were performed using the Instron model-8501 universal testing machine with crosshead speed of 0.2 mm/min. The specimens gage length was 9 mm and width was 2 mm, according to the ASTM E8.

3.
3.1.

Results and Discussion

Powder Materials

SEM micrographs of the Al powder, as received and functionalized CNTs are shown in Fig. 1a,b and c, respectively. Al is in the form of fine spherical powder with average particle size of 10 m. CNTs are in the form of agglomeration and have the diameter of 1030 nm. It can be seen that, as received CNTs are highly tangled together and in the form of agglomerates. Impurities get attached with the walls and ends of CNTs in the form of nanoparticles during the production process. So, impurities are removed after functionalization which improved the dispersion of CNTs in the matrix. This resulted in the better mechanical properties of composites.

Individual CNTs

3.2.

Electroless CNT/Cu Plating

Fig. 1 SEM micrograph of (a) pure aluminum powder having spherical morphology, (b) as received CNTs showing high entanglement and (c) functionalized CNTs showing individual CNTs after the acid treatment.

A fabrication approach such as the molecular-level mixing is necessary for CNT/Al composite. Homogeneous dispersion and strong interfacial bonding of CNTs with metal can be achieved by electroless coating [48]. By chemical reaction between functional groups on the surface of CNTs with metal ions, strong interfacial bonding between CNTs and metal was achieved, as shown in schematic representation in Fig. 2a. Cu particles are deposited and distributed uniformly on pretreated surface of CNTs, as shown in Fig. 2b. The size of Cu nanoparticles is less than 100 nm and particles are densely coated on the CNTs. Similar results were reported in many research

studies [49,50]. Optimizing the plating bath to (1:1) by wt CNTs with Cu, thickness of Cu-coated CNTs is reduced to 100 nm, as shown in Fig. 2c. The SEM analysis suggested that the thickness of coated CNTs is uniform. In addition, few open end tips of CNTs are found and it can be concluded that surface of CNTs is completely embedded in Cu particles, which is in accordance with previous results [5153].

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c
Cu coating on CNTs

Fig. 2 (a) Schematic representation of electroless copper plating of CNTs, process steps are showing the attachment of Cu on the functionalized CNTs. SEM micrographs of (1:1) by wt CNTs with Cu coating (b) CNTs are completely embedded in the Cu nanoparticles and (c) thickness of Cu-coated CNTs is about 100 nm.

By mixing Al powder with Cu-coated and uncoated CNTs, a proper mechanical interaction between Al powder and CNTs can be achieved. As the CNTs content increased, more and more powder is covered with the CNTs, which is also suggested by previous research studies [42,43]. The Cu-coated CNTs have provided sufficient wettability with the Al and hence a good bonding is achieved. The composites were fully densified near to their theoretical density.

3.3.

Microstructure

restrain the growth of particles. It is significant to note the critical effect of Cu-coated CNTs to achieve more interfacial bonding with Al matrix. Therefore, small grain size is obtained in the Cu-coated CNT/Al composites compared to uncoated CNT/Al composite, where a little grain growth that resulted in relative bigger grains is observed. Owing to the poor wettability in uncoated CNTs, more Al powders are cold welded during ball milling and pinning effect of CNTs in Al particles is less pronounced during sintering as compared to Cu-coated CNT/ Al composites. Similar grain refinement was also observed in 4 wt.% AlCu composite with higher concentration of CNTs and Cu nanoparticles [38,39].

In sintered composite samples, morphology of Al grains did not change much relative to that of the raw powders, as shown in Fig. 3. It is due to the equal pressure being applied around the compacts, which is beneficial for the plastic forming of the powders in order to reach full density. The grain boundaries are more visible after repeated etching. In the pure Al sample, small grain growth is observed (Fig. 3a) and equiaxed grains are observed in all the composites (Fig. 3b and c). In composite samples, CNTs are homogeneously dispersed at grain boundaries and within the Al particles, as shown in Fig. 4a and b. By comparing the grain size of composite samples (Fig. 3b and c) with the Al powder particles (Fig. 1a), it can be seen that growth of particles is very small. This sintering behavior is due to the pinning effect of CNTs to

3.4.

Phase Analysis

Several studies have shown that after CNTs dispersion in the Al matrix, no peak appeared for CNTs at 2 = 26 XRD pattern, even for rotator mixed CNT/Al powder (i.e., gentle mixing, not SPEX milled/ball milled) [3537]. Representative XRD patterns (for pure Al, 0.75 and 1.0 wt.% of uncoated and Cu-coated CNT/Al composites) are presented in Fig. 5. CNT amorphization has been reported in the high energy milled powders, which ultimately produce the Al4C3 phase in the CNT/Al composites [29,30]. No peaks of Al4C3 and Cu/CNT appeared in the XRD patterns of 1.0 wt.% uncoated and Cu-coated CNT/Al composites. This shows that no interfacial reaction occurred between CNTs and Al matrix.

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a
15.1 m

20 m

b
11.6 m

composites increase as CNTs wt% increases, as shown in Fig. 6a and b, which is in accordance with the previous reports [3236]. The fine grain size and pining effect due to Cu coated CNTs seemed to enhance the mechanical properties significantly. The increase in hardness of composites is more pronounced with the increase in the percentage reduction in thickness. After 80% reduction in thickness, increase in the microhardness of rolled composites is more pronounced in Cu-coated CNT composites. In 1.0 wt.% uncoated and Cu-coated CNT/Al composites, compared to pure Al, the microhardness increased by 44% and 103%, respectively. In case of 1.0 wt.% Cu-coated CNT/Al composite, there is an equal amount of Cu. Therefore, Cu nano particles are present along with the Cu coated CNTs in the Al matrix. The effect on microhardness is more pronounced in the case of 1.0 wt.% Cu-coated CNTs, compared to the uncoated and 0.75 wt.% Cu-coated CNT/Al composites. This is a clear indication of the strengthening effect of both CNTs and Cu nanoparticle.

3.5.2.

Annealing of Hot Rolled CNT/Al Composites

20 m

c
10.5 m

20 m

Fig. 3 Optical micrographs of etched (a) pure Al, 1.0 wt.% (b) uncoated and (c) Cu-coated CNT/Al composites.

3.5. 3.5.1.

Mechanical Properties Microhardness of Hot Rolled CNT/Al Composites

For the evaluation of the mechanical properties, the strength of composites was investigated by microhardness and tensile test. The samples were hot rolled to promote the uniform microstructure and dispersion of CNTs in matrix. Thus, hot rolling can be very effective to tailor the mechanical properties of CNT/Al composites. The hardness of CNT/Al

CNT/Al composites were highly strain hardened and stresses were produced due to high energy balled milling and severely deformed samples [3236,38]. In order to relieve the stresses and improve the tensile properties, 80% reduced composite samples were undergone the annealing process. A decline in the hardness of the composites has been observed by annealing. Decrease in hardness of pure Al is more as compared to the CNT/Al composites, due to excessive grain growth. Hence, annealing can be very effective to further improve the tensile properties of the CNT/Al composites. The characteristic stressstrain curves are presented in Fig. 7. Strength of annealed CNT/Al composites increased as CNTs wt.% increased. Yield strength and ultimate tensile strength of composites were measured from the stressstrain curves, as shown in Fig. 8a. Quantitatively, the enhancement in strength is not substantial in the uncoated CNT/Al composites as it is in the Cu-coated CNT/Al composites. For 1.0 wt.% uncoated CNT/Al composite, compared to pure Al, increase in yield strength and ultimate tensile strength estimated about 58% and 62%, respectively. Detailed data is presented in Table 1. However, in case of 1.0 wt.% Cu-coated CNT/Al composite, the yield strength and ultimate tensile strength increased significantly about 121% and 107%, respectively. Cu-coated CNTs developed the stronger interfacial bonding and higher affinity with the Al matrix which ultimately resulted in the efficient transfer of load. This shows that better dispersion of Cu-coated CNTs resulted in fine grain microstructure and homogenously embedded the CNTs in the matrix, as revealed from the SEM micrographs of sintered samples in Fig. 4. So, the higher strength of Cu-coated CNT/Al composites is caused mainly by CNTs where they act as high load translation from Al matrix, with Cu acting as a binding material. However, recently Nam et al. [38,39] proposed on the bases of mechanical and microstructural properties that CNT/AlCu composites were strengthened by both the load transfer from the AlCu matrix to the CNTs and by precipitation hardening of the heat treated AlCu matrix. In addition, He et al. [45,46] revealed that remarkable strengthening in CNT/AlNi composite is caused by the homogeneously dispersed CNTs and Ni nanoparticles. Compared to other hard particle reinforcements in AMCs such

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a
CNT concentration at grain boundary

Embedded CNTs inetching grove

Fig. 4 SEM micrographs of (a) 1.0 wt.% uncoated CNT/Al composite is showing the concentration of CNTs at grain boundary and (b) 1.0 wt.% Cu-coated CNT/Al composite is showing the presence of embedded CNTs within the etching grove at grain boundary.

as SiC [25], BC [6], Al2O3 [7,8], TiB2 [9] and graphite [10], the strengthening caused by CNTs reinforcement is the strongest. Fig. 8b shows that the ductility (elongation at fracture) of the CNT/Al composites decreased as the CNTs wt.% increased.

The decrease in the elongation is higher in the Cu-coated CNT/Al composites compared to uncoated CNT/Al composites. However, due to stress relieving during annealing process, sufficient ductility is observed in all the composite

Fig. 5 Comparison of XRD patterns of pure Al, uncoated and Cu-coated CNT/Al composites are showing no phase change and presence of only Al peaks.

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Fig. 6 Microhardness of hot rolled (a) uncoated and (b) Cu-coated CNT/Al composites with 40 and 80% reduction in the thickness.

samples. The characteristic yield phenomenon occurs during tensile testing and CNT/Al composite fracture after proper plastic deformation. Homogenous dispersion and alignment of CNTs along the of Al grains during hot rolling, contributed in the enhancement of the tensile strength, which are also reflected from the enhanced strength as well as enhanced ductility of the composites.

that Cu-coated CNTs are ruptured in fractured samples and few CNTs were pulled out. This suggests that the longer the CNTs embedded in the matrix, the greater is the bonding energy. Hence, it can be concluded that current Cu-coated CNT/Al composites have the strong interfacial bonding as well as good mechanical properties.

3.5.3.

Fractography

4.

Conclusions

SEM analysis was conducted to investigate the fracture behavior of CNT/Al composites after tensile loading. It can be seen in Fig. 9 that the CNTs are uniformly dispersed and embedded within Al matrix. The homogenization of CNTs is essential to improve the performance of composites under tensile loading where CNTs can act as high load translation (as shown from embedded and pulled out CNTs in Fig. 9a and b) and thus enhanced the energy to fracture and the strength of composites. CNTs are embedded in the Al matrix and held at one end, depending upon bonding energy and the extent of the embedded portion [38,45]. In Fig. 9c and d, it can be seen

Molecular-level mixing of Cu-coated CNTs resulted in the homogeneous dispersion of CNTs in Al matrix. The main conclusions are as follows: Optimizing the plating bath to (1:1) by wt CNT with Cu, thickness of Cu-coated CNTs has been reduced to 100 nm. Due to fine grain microstructure, compared to the pure Al, in 1.0 wt.% uncoated and Cu-coated CNT/Al composites, the microhardness of composites was increased by 69% and 136% respectively.

Fig. 7 Comparison of stressstrain curves of the pure Al, uncoated and Cu-coated CNT/Al composites.

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Fig. 8 (a) Yield strength, ultimate tensile strength and (b) % elongation of uncoated and Cu-coated CNT/Al composites.

Due to strong interfacial bonding of Cu-coated CNTs with Al matrix, increase in the microhardness of hot rolled Cu-coated CNT/Al composites is more pronounced at 80% reduction in thickness. Moreover, in 1.0 wt.% uncoated and Cu-coated CNT/Al composites, compared to pure Al, the microhardness increased by 44% and 103% respectively. For 1.0 wt.% uncoated CNT/Al composite, increase in yield strength and ultimate tensile strength estimated about 58% and 62% respectively. However, for 1.0 wt.% Cu-coated CNT/

Al composite, yield strength and ultimate tensile strength increased significantly about 121% and 107% respectively.

Acknowledgments
The authors are thankful to GIK Institute for financial assistance and providing research facilities. They are thankful to Dr. A. Saeed Hakeem, Dr. Basit Yameen and Dr. Hamid Zaigham of the GIK Institute for their technical support and valuable suggestions.

Table 1 Comparison of mechanical properties of uncoated and Cu-coated CNT/Al composites. Sample
Pure Al Uncoated CNT/Al

CNT wt.%
0 0.25 0.50 0.75 1.0 0.25 0.50 0.75 1.0

Hardness Hv
39 44 46 51 56 44% 61 68 71 79 103%

Yield strength (MPa)

86 96 101 134 136 58% 143 148 156 190 121%

Ultimate tensile strength (MPa)

140 170 189 214 227 62% 237 249 261 290 107%

Elongation (%)
31.5 21.5 14.8 10.5 7.2 77% 31.5 18.2 9.7 5.0 84%

Cu-coated CNT/Al

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b
CNT Pull out

Embedded CNTs

Fig. 9 SEM micrographs of fractured composite samples (a & b) 1.0 wt.% uncoated CNT/Al composite is showing the pulled out CNTs in Al grains and (c & d) 1.0 wt.% Cu-coated CNT/Al composite is showing the embedded CNTs and strong interfacial bonding between the Al and CNTs.

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