Materials Science & Engineering A 558 (2012) 386393

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Materials Science & Engineering A

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

Fabrication of Al/Ni/Cu composite by accumulative roll bonding and electroplating processes and investigation of its microstructure and mechanical properties
Ali Shabani, Mohammad Reza Toroghinejad n, Ali Shafyei
Department of Materials Engineering, Isfahan University of Technology, Isfahan 84156-83111, Iran

a r t i c l e i n f o
Article history: Received 5 June 2012 Received in revised form 4 August 2012 Accepted 6 August 2012 Available online 10 August 2012 Keywords: AlNiCu composite Accumulate roll bonding Electroplating Mechanical properties Microstructure

a b s t r a c t
AlNiCu composite was produced using accumulative roll bonding (ARB) and electroplating processes. Nickel was electroplated on copper substrate for a certain time and voltage. In this study, the microstructural evolution and mechanical properties of the AlNiCu composite during various ARB cycles were studied by optical and scanning electron microscopes, microhardness, tensile and bending tests. It was observed that at rst, nickel layers and then copper layers, were necked, fractured and distributed in aluminum matrix as accumulative roll bonding cycles were increased. Finally, after 11 cycles of ARB process, a completely uniform composite was produced with a homogeneous distribution of copper and nickel particles in aluminum matrix. The results showed that by increasing the number of ARB cycles, the bending strength of produced composite was increased. Also, it was found that when the number of cycles was increased, not only elongation was increased but also the tensile strength of the composite was improved. Microhardness for different elements in different cycles was also evaluated. Finally, fracture surfaces of samples were studied, using scanning electron microscopy (SEM), to reveal the failure mechanism. & 2012 Elsevier B.V. All rights reserved.

1. Introduction Metal matrix composites (MMCs) have played a great part in the materials used in industry for the last several decades. Aluminum based metal matrix composites, because of their specic properties such as low density, good electrical and thermal conductivity, wear resistance and good formability, are commonly used in aerospace, automotive and structural industries [1,2]. Accumulative roll bonding (ARB) is one kind of severe plastic deformation (SPD) process which can produce bulk ultrane/nanograined (UFG) metallic materials and metal matrix composites [3,4]. Also, it should be noted that the majority of the severe plastic deformation processes require expensive tools and complex processes, limiting their commercial and industrial usages. However, accumulative roll bonding process can be used as a new and suitable way for producing multi-layer composites, because of its simplicity and cheaper manufacture process [5,6]. Accumulative roll bonding involves stacking two sheets of the same materials after proper annealing and surface treatments and rolling to a reduction of 50%. The rolled sheet is cut into two equal

Corresponding author Tel./fax : 98 311 3915726. E-mail addresses: ali.shabani@ma.iut.ac.ir (A. Shabani), toroghi@cc.iut.ac.ir (M.R. Toroghinejad), shafyei@cc.iut.ac.ir (A. Shafyei). 0921-5093/$ - see front matter & 2012 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.msea.2012.08.017

halves and this cycle is repeated as many times as needed [6,7]. It had been known that during ARB process, the imposed severe plastic deformation results in grain renement and subdivision from high-angle boundaries to low-angle ones; then the ultra-ne grains with more equilibrium grain boundaries are formed nally [8]. Mostly, during co-deformation of dissimilar layered metal systems, plastic instabilities in one of layers happen earlier than others due to differences in mechanical properties; as strain increases, the harder layer starts necking and early fragmentation occurs between other layers [911]. Lots of works have been performed to produce different composites using accumulative roll bonding process, such as, Al/ Zn [12], Al/Cu [13], Al/Mg [14], Mg/Al/Zn [15], Ti/Al/Nb [16] and Al/Ni [5,17]. Also, studies have been done on particle reinforced metal matrix composites, including Al/Al2O3 [18,19], and Al/SiC [20]. Recently, Jamaati and Toroghinejad produced a metal matrix composite (aluminum/alumina), using a coating method (anodizing) and accumulative roll bonding process. The most important advantage of using coating is producing high-strength and highly uniform composites with ultra ne grain structure [21]. With regard to pervious works, the most incentive behind this study is to combine the goodness of pervious works [5,13,17,21] to produce a composite with a proper distribution of reinforcement in matrix and also good mechanical properties from aluminum, copper and nickel.

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The present work is the rst of its kind that focuses on producing AlCuNi composite using accumulative roll bonding and electroplating process. Manufacturing a high strength aluminum matrix composite with a ne and uniform distribution of reinforcement in the matrix is the most attractive aim of this study. So, the microstructure and mechanical properties of produced composites were investigated at different cycles of ARB for a certain wt% of its elements.

strong joint. Also, to prevent signicant re-oxidation of the prepared surfaces, the strips were rolled as soon as possible. 2.4. Accumulative roll bonding process ARB process here consisted of two steps as shown in Fig. 2. In the rst step, the electroplated strip was laid between the prepared surfaces of the two annealed aluminum strips. The three strips were stacked over each other and fastened at both ends using steel wire. Then they were roll-bonded to 66% reduction to attain a strip with 1 mm thickness. This was cycle named as cycle zero. In the second step, the produced strip was cut into two halves, surface prepared, fastened and roll-bonded to 50% reduction. This process was repeated up to 11 cycles. The 50% reduction at room temperature was quite enough to bond the sheets and no fracture at bonded boundaries was observed during the experiment. Repeating this process to 11 cycles was done to get a uniform distribution of reinforcement particles in the matrix, remove porosities from the interfaces between the layers, and obtain an ideal strength and elongation for the produced composite. The roll bonding process was carried out with no lubrication, using a laboratory rolling mill with a loading capacity of 20 t. 2.5. Investigation of structure and mechanical properties Microstructure of the AlCuNi composite in rolling direction (RD) and normal direction (ND) was observed by optical microscope (OM) to investigate the effects of the number of ARB cycles on distribution of copper and nickel particles in the matrix. Also, scanning electron microscopy characterization was performed to investigate the fracture behavior of the surfaces after the tensile test. Vickers microhardness test was done under a load of 100 g and time of 15 s on composites RD-TD plane on aluminum

2. Materials and experimental procedures 2.1. Materials Materials included aluminum and copper commercially pure strips with the specications shown in Table 1. Strips 200 mm long, 50 mm wide, and 1 mm thick were cut from cold rolled sheets parallel to the original rolling direction (RD). Aluminum and copper strips were annealed at 663 K and 773 K for 2 h, respectively, to ensure consistent specimen hardness. 2.2. Electroplating process After the annealing treatment, nickel was coated on the copper strips by industrial electroplating process. Electroplating on the copper sheets was done after the required surface preparation which involved degreasing and acid cleaning. Chemical composition of industrial electroplating bath for coating nickel on copper consisted of 350 kg nickel sulfate (Ni2SO4), 50 kg nickel chloride (NiCl2) and 45 kg boric acid (H3BO4) in 1 m3 of bath. Electroplating was done under an applied voltage of 8 V for a certain time (120 min) that was the optimum time to approach the best bonding quality between the layers with regard to our previous work [22]. Fig. 1 is the schematic illustration of nickel electroplating on copper. The thickness of the nickel layer obtained by the electroplating process was determined by scanning electron microscopy. Average and standard deviations of about 30 measurements were calculated. The thickness of nickel coating on the copper strips after 120 min of electroplating was 30 mm and so, the produced composite involved 3.75 wt% of nickel. 2.3. Surface preparation To produce a satisfactory metallurgical bond by accumulative roll bonding, it is essential to remove the contamination layers upon the surfaces of the two metals to be joined [23,24]. The surface preparation processes used here included degreasing of aluminum and copper surfaces in acetone bath for at least 30 s, and scratch-brushing the intimate surface of strips by means of a circular steel brush with 50 mm radius and 0.25 mm wire diameter. The surfaces were scratch-brushed at peripheral speed of 2000 rpm at least for 60 s, parallel to the rolling direction. However, for the strips with nickel coating, only degreasing in acetone bath for 30 s was adequate. It is important to avoid touching the clean surface because grease or oil by hand contamination on the faying surfaces may impair the formation of a

Fig. 1. Schematic illustration of nickel electroplating bath.

Table 1 Chemical composition of materials used. Al (%) 99.713 Cu (%) 99.86 Si (ppm) 730 Si (ppm) 30 Fe (ppm) 1640 Fe (ppm) 600 Mn (ppm) 70 Mn (ppm) 34 Ni (ppm) 17 Ni (ppm) 84 Zn (ppm) 160 Zn (ppm) 20 Ti (ppm) 150 Sn (ppm) 170 Sb (ppm) 14 Pb (ppm) 73 V (ppm) 90 Cr (ppm) 20 Cu (ppm) 0.00 Al (ppm) 206 Cr (ppm) 0.00 S (ppm) 34

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Fig. 2. Schematic illustration of the principle of the ARB process.

matrix, copper layers and nickel particles for different cycles of ARB. Eight tests were performed for each sample, then the abnormal, off points were deleted off and the rest points were averaged to report the sample microhardness. Three-point bending tests were performed on composites with different numbers of cycles as shown in Fig. 3 and bend strengths of samples were calculated from Eq. (1) [25]

Fig. 3. Schematic illustration of three-point bending test.

6FL 4WT

MPa 2

where F is the bending load, L is the distance between the two supports, and W and T are the samples width and thickness respectively. The tensile test samples were machined from the

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ARBed strips, according to the ASTM E8M standard, to get oriented along the rolling direction. The gauge width and length of the tensile test samples were 6 and 25 mm, respectively. Tests were done at room temperature. Also, for bending and tensile tests, three samples were tested for each condition and the average values were reported.

3. Results and discussion 3.1. Microstructure evaluation Fig. 4 illustrates microstructure variations of Al/Ni/Cu composites on RD-ND plane during different ARB cycles. It is obvious that nickel coating was fractured locally in cycle zero (Fig. 4a) by increasing the numbers of cycles nickel fragments distributed uniformly in aluminum matrix. This is one of the advantages of using electroplating process, because fracture of nickel layer happened at primary cycle and a composite with highly uniform distribution of particles could be produced. Also, it is evident that copper layers were uniform just in the primary cycles of ARB, and then they were initiated to neck and fracture locally in subsequent cycles (Fig. 4b and c). It can be seen that as ARB process proceeded, strain was increased and thickness of copper layers was decreased. Finally, copper layer separation was observed in the seventh cycle. Also, after eleven cycles of ARB process, an aluminum matrix composite with a homogeneously distributed copper and nickel fragments in the matrix was achieved (Fig. 4d). Generally, during plastic deformation of dissimilar metals, plastic instabilities caused by different ow properties and differences in mechanical properties of layers caused the emergence of necking and fracture in the harder layer [13,16,26,27].

The hardness of aluminum, copper and nickel before rolling were determined as 25, 50 and 150 HV, respectively. Therefore, in the primary cycles of rolling, pressure of rollers resulted in both elongation of sample along rolling direction and fracture of nickel layer. Also, the copper layers were necked and fractured after the third cycle due to mainly increasing the hardness and decreasing of owability. Therefore, it was seen that while pure aluminum layers sealed their coherency in most regions during the ARB processing, nickel and copper layers would be necked and ruptured nally. Also, it was observed that nickel and copper layers were fractured nonhomogeneously in the form of small parts in aluminum matrix because of the difference in mechanical properties of the three dissimilar layers. Consequently, by increasing the number of cycles, a homogeneous distribution of copper and nickel layers inside the aluminum matrix would be obtained. Fig. 5 shows the variation of average thickness of copper layers versus the number of ARB cycles. A rapid decrease in average thickness of copper layers at primary cycles was seen. However, by proceeding ARB process, the rate of decreasing in thickness is reduced. Decreasing in copper layers thickness is due to the enhancement of the strain by increasing the number of ARB cycles. However, the fracture of copper layers after third cycle caused a reducing in the rate of copper thickness decreasing. Also, it was observed that after eleven cycles of ARB copper, layers were separated in the matrix, and a completely uniform distribution of particles in matrix was achieved. 3.2. Mechanical properties 3.2.1. Hardness test Microhardness variations of aluminum, copper and nickel layers at different cycles of ARB process are shown in Fig. 6. It is

Fig. 4. Optical micrographs of longitudinal cross-section of ARBed Al/Ni/Cu composite: (a) after primary sandwich preparation, (b) after 3 cycles, (c) after 7 cycles and (d) after 11 cycles.

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Fig. 5. Thickness variations of the copper layers during different cycles of ARB of Al/Ni/Cu multilayer composite.

could be resulted in generation of new dislocation at the component interfaces, i.e. Al/Cu, Al/Ni and Cu/Ni interfaces. This process could increase hardness of composite and phases in the last cycles of ARB process, Fig. 6. In addition, it can be seen from this gure that hardness for eleventh cycle for copper, nickel and aluminum is 4.1, 3.8 and 3.4 times greater than initial foil or coating, respectively. This difference in the rate of increasing hardness can be attributed to the different rate of strain hardening of element during deformation process. It is suggested that the difference in the rate of strain hardening is attributed to the dissimilarity of stacking fault energy of elements. The stacking fault energy determines the extent to which unit dislocations are dissociated into partial dislocations. Such a dissociation, which is promoted by a low value of stacking fault energy, hinders the climb and cross slip of dislocations, which are the basic mechanisms responsible for recovery [30]. Stacking fault energies of copper, nickel and aluminum are 78, 128 and 166 mJ m 2 [30], respectively. It is expected that copper layers go through more strain hardening than nickel and aluminum, corresponding to the result of hardness tests. So, the less the stacking faults energy, the more the strain hardening rate and therefore, the more rate of increasing in hardness during ARB process.

Fig. 6. Microhardness variation for individual aluminum, copper and nickel layers for ARB processed Al/Ni/Cu composite.

obvious that by proceeding ARB process, microhardness of aluminum matrix and reinforcing copper and nickel particles was increased. The many investigations performed on variations of phases microhardness during ARB process illustrated that the rapid microhardness increase of different phases after primary sandwich preparation can be attributed to the strain hardening as a result of high dislocation density [13,14,17]. Fig. 6 shows that after one pass of rolling (cycle zero), remarkable increases can be observed in the microhardness values, which were 2.1, 1.9 and 2 times greater than primary layers of aluminum, copper and nickel, respectively. The increasing rate of hardness in primary cycles of ARB is because of the high rate of strain hardening as a result of high dislocation density. The hardness increase, with lower rate for the following cycles (2nd5th) can be attributed to the reduction of strain hardening rate during plastic deformation. In addition, it has been reported that difference in coefcients of thermal expansion (CTE) between matrix and reinforcements can inuence the hardness variations of different phases in composites produced by ARB process [28]. Generally in ARB process, sample temperature increases due to plastic deformation and also friction between roller and sample [8]. Therefore, with respect to the difference in CTE of aluminum, nickel and copper, 23, 13 and 50 mm/mK [29], respectively, the temperature rise

3.2.2. Bending and tensile test Mechanical behaviors of multilayer produced composite were evaluated for different cycles of ARB using three-point bending test. The results of the bending tests for different cycles are given in Fig. 7, plotting the force versus the vertical displacement. It can be seen that the bending force of the composite is improved by proceeding ARB process. Fig. 8 illustrates the variations in the bending strength of the Al/Ni/Cu composite versus the number of ARB cycles. It is obvious that the bending strength is increases in the composite by increasing the number of ARB cycles. It can also be seen in Fig. 8 that after three cycles of ARB, the bending strength achieved 573 MPa from 505 MPa, showing the rate of 22.7 MPa increase per cycle. However, this rate was decreased to 10 up to nine cycles, and by proceeding ARB process, this rate again was increased to 20 up to 11 cycles. Also, in order to study the effect of ARB cycles on the mechanical properties of Al/Ni/Cu composites, tensile test was conducted. The engineering stressstrain curves are presented in Fig. 9. It is shown that yield and tensile strengths of composite are increased by proceeding ARB process. As it is observed in the stressstrain curves, the Al/Ni/Cu composite showed a signicant

Fig. 7. Three-point bending tests results.

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Fig. 8. Variation of bend strength with the number of ARB cycles.

Fig. 10. Variation of tensile strength and elongation with the number of ARB cycles.

Fig. 9. Engineering stressstrain curves for sandwich sample and Al/Ni/Cu composite within different cycles of ARB process.

enhancement in strength with increasing ARB cycles. The maximum tensile strength of composite was reached to 346 MPa at the eleventh cycle. As can be seen in Figs. 7 and 9, the elastic modulus of samples subjected to one and more cycles are slightly more than the one with zero cycle (primary sandwich). It should be noted that the primary sandwich consists of three layers (Fig. 4a), whereas after applying the cycles, the sample microstructure turns to a composite containing an aluminum matrix with a homogeneously distributed copper and nickel fragments in the matrix. The latter elastic property differs from the former. In the work performed by Eizadjou et al. [13] the same result was observed on the AlCu composite produced by ARB process. The variations in tensile strength and elongation of the Al/Ni/ Cu composites versus the number of ARB cycles for 3.75 wt% nickel are shown in Fig. 10. It is obvious that tensile strength is increased in the composite by increasing the number of ARB cycles. These results are consistent with previous ndings [13,14,17,1921]. As can be seen, the tensile strength of composite is increased from 228 to 259 MPa after 5 cycles of ARB, indicating 14% enhancement in the strength. However, the rate of strengthening after fth cycle is increased and after eleven cycles, the tensile strength of composite reaches to 346 MPa, showing 40% increase in the strength at the second step. In addition, according to Fig. 10, the elongation of composite after production of primary sandwich was 7.5%. It was decreasing as ARB process proceeded, reaching an amount of 5.6% after the third cycle. But it can be seen that after the third cycle, increasing ARB cycles

greatly enhances the elongation of the composite, reaching to 7.9% after the eleventh cycle. It has been declared that variations of strength in severely deformed materials are governed by the two major strengthening mechanisms: strain hardening by dislocations and grain renement [3,4,7,31,32]. Also, it has been showed that strain hardening plays the main role in enhancing the strength within the primary cycles of the ARB process, but at higher cycles, grain renement increased the strength of composite by proceeding the process [3,4,13,33]. In this study, strengthening of MMCs results not only from the mentioned mechanisms but also by following factors: Composite strength is boosted by the reinforcing role of copper and nickel particle in aluminum matrix. Reinforcement particles in the matrix can impede dislocation motion and also cause the generation of additional dislocations around copper and nickel particles. Consequently, motions of dislocations are decreased due to the presence of the reinforcement, which strengthens the composite. The distribution of particles can also affect the strength of composite. Increasing ARB cycles causes the uniform distribution of the reinforcement in the matrix [1921,33]. During plastic deformation, the cracks are initiated in the interfaces of matrix and reinforcements will propagate and link up with other cracks. So, if the particles move independently of one another under the stresses at the crack tip, then the constraint gives rise to very large plastic strains and the crack displays a preference for passing through clustered regions [34]. Thus, the tensile strength of MMC is improved. Also, the bonding between matrix and reinforcement affects the strength of the composite, which has a dual effect. By proceeding ARB process, the bonding between the reinforcements and the matrix becomes stronger due to the greater rolling pressure applied, reducing crack initiation in the interfaces. So the strength of composite is improved. On the other hand, the stronger bonds between the reinforcements and the matrix reduce the tensile strength. It is because the layer aids interfacial sliding (as against debonding) and promotes stress relaxation, thus reducing the tensile strength [34]. Variation of size and shape of reinforcement can also affect the strength of composite. It can be seen from Fig. 4 that by increasing ARB cycles, reinforcement layers changed from elongated shape to small particles, resulting in more and smaller particles which makes more efcient obstacles against dislocation movement. This can increase the strength of the composite being deformed. Variation of elongation during ARB process can be attributed to the following factors: Strain hardening decreases elongation due to the decreasing mobility of dislocation. In addition, uniform distribution of particles can increase elongation of composite. As the particles

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Fig. 11. The SEM micrographs of fracture surfaces of Al/Ni/Cu composite at (a and b) primary sandwich, (c and d) ve cycles, (e and f) 11 cycles, of ARB process.

move independently of one another and the distance between the Al/Cu and Al/Ni interfaces increases, cracks are propagated and linked up with other cracks later. So, the elongation values of MMCs are improved. Finally, bonding quality between the matrix and reinforcement increases the elongation of MMC. This is because the layer aids interfacial sliding and promotes stress relaxation, thus reducing the tensile strength and delaying the onset of catastrophic failure and consequently, increasing elongation.

the size of the dimples is reduced; also, equiaxed dimples are changed to shear dimples and dimples are not as deep as the dimples in the composite of primary cycles. So, it can be said that the fracture mechanism is changed to shear ductile fracture by increasing ARB cycles; however, few brittle fractures in eleventh cycle can be distinguished by considering Fig. 11e and f. Fig. 11 also illustrates that by increasing ARB cycles, the bonding quality between layers is improved.

4. Conclusion 3.2.3. Fractography In order to clarify the rupture mechanisms of composites in different cycles of ARB process, SEM was used. The fractographs after tensile test are shown in Fig. 11. Clearly, the primary sandwich and almost the composite at ve cycles exhibited a typical ductile fracture, showing equiaxed dimples. This rupture model was observed in some other investigations of materials under severe plastic deformation [4,35]. This kind of fracture occurs by formation and coalescence of microvoids ahead of the crack and very limited dislocation activity [35]. However, it is obvious that with increasing the number of ARB cycles, fracture mechanism of composite is changed due to the variation in dimples size, orientation and depth. By proceeding ARB process, The accumulative roll-bonding (ARB) process was used as a severe plastic deformation technique to provide an effective alternative method for the manufacture of high strength aluminum/copper/nickel composite. Also, electroplating process was used to produce a highly uniform composite. The microstructure and mechanical properties of the composite were investigated. The following conclusions can be drawn: 1) ARB process can be used to produce Al/Ni/Cu multilayer composites. It was seen that nickel coating was fractured locally in cycle zero and copper layers were initiated to neck and fracture in the subsequent cycles. After eleven cycles of

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2)

3)

4)

5)

ARB, a composite of aluminum matrix with uniform distribution of reinforcing phases (Ni and Cu) was obtained. Average thickness of copper layers was reduced with increasing the number of ARB cycles, reached to about 7 mm after the eleventh ARB cycle from 1000 mm in the primary layer. Microhardness of different elements and bending strength of produced composite were enhanced by proceeding ARB process. The tensile strength of the composites was improved when the number of cycles was increased, reaching to 346 MPa after 11 cycles, which was 1.5 times higher than that was obtained for the primary sandwich sample. Also, the elongation of produced composite was decreased at primary cycles but improved by increasing the number of cycles. SEM fractograph of fracture surfaces illustrated that by increasing ARB cycles, fracture mechanism was changed from ductile to shear ductile and partially, to brittle fracture in the nal cycles.

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