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This document is downloaded from DR‑NTU ( Nanyang Technological University, Singapore. Friction stir processing of Al‑CNT composites Du, Zhenglin; Tan, Ming‑Jen; Guo, Jun‑Feng; Wei, Jun 2015 Du, Z., Tan, M. ‑J., Guo, J. ‑F., & Wei, J. (2016). Friction stir processing of Al‑CNT composites. Proceedings of the Institution of Mechanical Engineers, Part L: Journal of Materials: Design and Applications, 230(3), 825‑833. © 2015 Institution of Mechanical Engineers (IMechE). This is the author created version of a work that has been peer reviewed and accepted for publication by Proceedings of the Institution of Mechanical Engineers, Part L: Journal of Materials: Design and Applications, IMechE. It incorporates referee’s comments but changes resulting from the publishing process, such as copyediting, structural formatting, may not be reflected in this document. The published version is available at: []. Downloaded on 26 Jun 2021 09:04:06 SGT

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    Friction stir processing of Al‑CNT composites

    Du, Zhenglin; Tan, Ming‑Jen; Guo, Jun‑Feng; Wei, Jun


    Du, Z., Tan, M. ‑J., Guo, J. ‑F., & Wei, J. (2016). Friction stir processing of Al‑CNT composites.Proceedings of the Institution of Mechanical Engineers, Part L: Journal of Materials: Designand Applications, 230(3), 825‑833.

    © 2015 Institution of Mechanical Engineers (IMechE). This is the author created version of awork that has been peer reviewed and accepted for publication by Proceedings of theInstitution of Mechanical Engineers, Part L: Journal of Materials: Design and Applications,IMechE. It incorporates referee’s comments but changes resulting from the publishingprocess, such as copyediting, structural formatting, may not be reflected in this document.The published version is available at: [].

    Downloaded on 26 Jun 2021 09:04:06 SGT

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    Special Issue

    Friction stir processing of Al–CNTcomposites

    Zhenglin Du1, Ming-Jen Tan1, Jun-Feng Guo2 and Jun Wei2


    Friction stir processing (FSP) is a solid-state process with the ability to refine grain sizes and uniformly disperse particles

    to improve the mechanical properties of the base material. In this study, FSP was performed on AA6061-T6 with and

    without additions of multi-walled CNTs. For FSP on monolithic Al plates, dendrites were broken down and dispersed

    uniformly with the increase in number of passes. As for FSP of Al–CNT composites, the CNTs have been successfully

    dispersed with three FSP passes. Dispersion is more uniform with increasing number of passes. The Vickers hardness and

    tensile yield strength were found to have improved after performing FSP with the addition of CNTas compared to FSP of

    AA6061-T6 without CNT.


    Friction stir processing, nanocomposites, carbon nanotubes, mechanical properties

    Date received: 28 August 2014; accepted: 18 December 2014


    Friction stir welding and friction stir processing

    Friction stir welding (FSW) was invented by TheWelding Institute (TWI) of UK in 1991.1 It is asolid-state joining technique used to weld two piecesof metal together without melting. Much research hasbeen done on the welding of aluminum due to its rela-tive low melting pointing and low weldability usingtraditional welding techniques.

    The basic working principle of FSW involves anonconsumable tool with a threaded pin and shoulderbeing plunged into the abutting edge of two sheetsand transverse along the direction of the line ofjoint. The friction between the tool and the plate gen-erates heat which softens the work piece. The rotationof the tool moves the material from the front to theback.2

    The working principle of friction stir processing(FSP) is based on FSW. Work is done on a singlework piece instead of joining two pieces together(Figure 1). Friction stir processing technique wasfirst reported by Mishra et al.3 for localized micro-structure modification to achieve certain desirableproperties and has attracted much attention eversince.

    For friction stir processing, the constituent phasematerial in the process zone is being mixed and refinedby the tool due to the intense plastic deformationduring the FSP. The true strain during FSP isapproximately 40.4 Mishra et al.3 studied FSP withthe addition of SiC and observed an increase in

    surface hardness as well as uniform distribution ofSiC particles in Al matrix. An investigation on theeffect of rotation speed on FSPed AZ31–Al2O3 com-posites, found that an increase in rotation speed led toenhancement in the particle distribution and createdfiner nanoparticle agglomeration.5

    Metal matrix composites

    High elastic modulus and wear resistance of particu-late-reinforced metal matrix composites (MMCs)have drawn the attention of the aerospace, automo-bile and defence industries. Furthermore, additions ofsmall amount of nano-sized particles significantlyenhanced the material properties.6–8

    Guo et al.9 studied the evolution of grain structureand mechanical properties of AA6061 alloy reinforcedwith nano-Al2O3. Slurry of nano-sized Al2O3 particlesand a volatile solvent was used to preplace reinforcingparticles in an array of cylindrical holes on the surfaceof AA6061 plate. Multiple FSP passes were applied toimprove the dispersion of the particles. In the study,particle dispersion improved with increasing number

    1School of Mechanical & Aerospace Engineering, Nanyang Technological

    University, Singapore2Singapore Institute of Manufacturing Technology (SIMTech), Singapore

    Corresponding author:

    Ming-Jen Tan, School of Mechanical & Aerospace Engineering, Nanyang

    Technological University, 50 Nanyang Avenue, Singapore 639798.

    Email: [email protected]

    Proc IMechE Part L:

    J Materials: Design and Applications

    0(0) 1–9

    ! IMechE 2015

    Reprints and permissions:

    DOI: 10.1177/1464420715571189

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    of FSP passes, and finer grain size was produced withthe addition of composite. Also, the final grain size forone pass and three passes were similar, as the finalgrain size is dependent on welding temperature.10

    Liu et al.11 studied FSP of Mg–Li–Al–Zn underwater and reported fine equiaxed, recrystallizedalpha (hcp), and beta (bcc) grains. Superplasticitywith ductility of 300% at 100 �C and more than400% under high strain rate at 225–300 �C wasachieved.

    To the best of the author’s knowledge, no one hasreported on CNTs reinforcement using friction stirprocessing. However, a study by Liao and Tan12

    was conducted on the addition of CNT to aluminummatrix. CNTs were mixed with aluminum powder andsintered before hot extrusion and hot rolling. The spe-cimens were then tested for mechanical properties. Itwas observed that the presence of CNTs in the alumi-num matrix slowed fatigue crack propagation bycrack-bridging, CNT frictional pull-out, and breakagemechanism. Al–CNT composites showed significantlyimproved densification, nano-indentation modulus,hardness, tensile strength, and fatigue resistance.However, the CNTs were not well dispersed andagglomerated in clusters. FSP is able to achieve a uni-form dispersion of many particles, hence the aim ofthis study is to use FSP to obtain uniform dispersionof the CNTs in the aluminum matrix and study itsmicrostructure and properties.

    Experimental details

    There are various methods of applying particles onthe substrate before performing FSP. Mishra et al.3

    prepared Al–SiC surface composites by applying amixture of SiC powder suspended in methanol ontorolled 5083 aluminum Alloy surface. Holes, orgrooves can also be made on the surface of the base

    material to contain the reinforcement particles.13

    Billets made from cold compacting and sintering amixture of metal powder and composites can also bedone prior to FSP.14 Cross rolling is then done on thecast alloys to obtain a flat surface for FSP.15

    In this study, CNTs were applied onto an AA6061-T6 rolled plate of 300mm length and 100mm width(rolling direction). An array of 960 cylindrical holeswith diameter of 1mm and depth of 2mm weremachined in an area of 240mm� 50mm (Figure 2).Acetone was used to degrease the plates before airdrying. The multi-walled carbon nanotubes(MWCNTs) are of outer diameter ranging from 10to 20 nm, length ranging from 10 to 30 mm, andpurity of at least 95%. The nominal volume fractionof CNTs produced by FSP is 0.5%. A friction stirwelding robot capable of generating a maximumdownward force of 12 kN was used to carry outFSP. The tool used to conduct FSP was a threadedconical probe welding tool with three flats. The toolhas a shoulder diameter of 12.5mm, probe length of2mm, and a probe base diameter of 5mm. An add-itional 1mm thin sheet of AA6061-T6 was placedabove it prior to performing FSP, using a rotationalspeed of 1800 r/min, travel speed of 8mm/s, and tiltangle of 3�.

    Metallographic samples were then sectioned trans-versely from the plates after FSP was performed.They are then polished using conventional mechanicalpolishing method and viewed under field emissionscanning electron microscope (FESEM) equippedwith electron backscattered diffraction (EBSD).EBSD was performed with step size of 0.5lm andmaps were used to plot misorientation angle histo-grams using Channel 5 software by HKLTechnology. A minimum of five points were sampledfrom the cross section surface using Vickers hardnesswith 50 gf loading. Tensile testing was conducted in

    Figure 1. Schematic and actual illustration of FSP.

    2 Proc IMechE Part L: J Materials: Design and Applications 0(0)

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    accordance to ASTM E08-04 standards at test speedof 1mm/min. A minimum of three ‘‘I’’-shaped rect-angular sub-sized samples with gage length of 25mmand width of 6mm in the reduced section were used(Figure 3). A fractography was done using scanningelectron microscope (SEM) on the fractured sites.

    Results and discussions

    Particle dispersion

    Large dendrites as well as Si particles were observed inthe as-received AA6061-T6 (Figure 4(a)). FSP hasbroken up some Si particles and aluminum dendritesand dispersed them uniformly into the aluminummatrix. Finer particles as well as a more uniform dis-tribution of the particles were observed with increasednumber of passes (Figure 4(b) and (c)). The stirredzones of the FSP were free of porosities.

    Similar observations were seen in the Al–CNTSEM images. From SEM, clusters of CNTs werefound in the sample with one pass (Figure 4(d)). Inthe sample with additions of CNT and three passescondition, there were no visible CNT clustersobserved (Figure 4(d) and (e)). It is believed that theCNTs were broken up by the stirring and mixing byFSP.

    Grain structure evolution

    The EBSD results of the friction stir processed sam-ples showed significant grain refinement compared tothe base material (Figure 5). It was also observed tohave sub-grain boundaries present in several slightlyelongated grains. More sub-grain boundaries wereseen in the stirred zone. This is in agreement with

    the continuous dynamic recrystallization, whichoccurred with the introduction of continuous straincoupled with rapid recovery and migration of sub-grain boundaries during friction stir processing.16–18

    Hence, severe deformation was caused by the intensedislocation generation experienced by the material inthe stir zone. The stored energy in the dislocationresulted in the dynamic recovery and recrystallizationprocess.

    For samples without CNT, the average grain size is4.49lm for samples that underwent one pass and5.04lm for samples that underwent three passes(Table 1). This slight variation is in agreement witha previous study that found grain sizes are similar andindependent on the number of passes.19 And, dynamicrecrystallization is a strong function of the flow stressand not the temperature during deformation.20

    Hence, the grain sizes were somewhat similar here.However, studies have also showed that grain sizesof the stir zone are a function of the welding tempera-ture.10,19,21 In this study, the processing parameterswere kept constant for the different passes, resultingin a constant flow stress and processing temperature.

    For the samples with CNT, the average grain size is2.11lm for samples that underwent one pass and4.67lm for samples that underwent three passes(Table 1). Interestingly, samples with CNT thatwent through three passes had larger grain sizes ascompared those that went through one pass. Thiscould be due to higher temperature experienced withthe increase in number of passes with the presence ofCNTs. For Al-CNTs with one pass, the average grainsize is smaller than those without CNT. This couldonly be the result of adding CNT as the processingparameters are the same; particle stimulated nucle-ation may occur when Al-based metal matrix

    Figure 2. (a) AA6061-T6 plate with an array of 720 holes with 1 mm diameter, 1 mm in depth, and spacing of 4.2 mm; (b) AA6061-T6

    plate after FSP.

    Du et al. 3

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    composites were friction stir processed.22–24 However,particle stimulated nucleation did not occur as it isonly possible when dislocations accumulate at theparticles during deformation and CNTs are smallerthan 1 lm. Therefore, it is believed that Zenerpining effect by CNT has resulted in finer grain sizesby retarding the grain growth of the matrix. The rate

    of grain growth in the recrystallization of metalswith dispersed second phase particles can bedescribed using equation (1) according toHumphreys et al20


    dt¼M P� Pzð Þ ¼Mð

    ��bR� 3FV�b

    2rÞ ð1Þ

    Here, Fv is the volume fraction, M is the boundarymobility, P is the driving pressure from the curvatureof the grain boundaries, Pz is the Zener pinning pres-sure, R is the radius of the grain, r is the radius of thepinning particles, a is a small geometric constant, and�b is the boundary energy.

    When P¼Pz, grain growth will stop

    ��bR¼ 3FV�b


    Figure 4. FESEM image of AA6061-T6 samples (a) as received with �1000 magnification; (b) with one pass condition with �1000magnification; and (c) three passes with �1000 magnification; FSP Al–CNT composite with (d) one pass with �5000 magnification and(e) three passes with �5000 magnification.

    Figure 3. Dimensions of the samples used for tensile test in


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    Zener limiting grain size (a¼ 1) can be obtainedwhen the mean grain radius (D) and the radius ofcurvature (R) are taken to be the same

    Dz ¼4r


    Tweed et al.25 suggested that the interactionbetween the pinning particles and grain boundariesis very complicated. Their study suggested that thehigh energy of the grain boundary of the high-angleboundaries may have curved the boundary planewhen it touches a second phase inclusion. Thisresult in a bypass long before the boundary bentinto a semi-circle as a whole. However, low angleboundaries has lower energy and are more flexibleresulted in a more perturbed plane.

    EBSD analysis was used to further investigate thepinning effect of the CNTs (Figure 6).

    For friction stir processing of Al–CNT with threepasses, the mean boundary misorientation and thenumber of high angle boundaries (>15�) was observedto have slightly decreased with a slight increase in thenumber of low angle boundaries (415�) when com-pared to AA6061-T6 that underwent three passes(Table 2). The reason for this observation is that theCNTs were randomly oriented and very small in size.Hence, there were no significant pinning effect anddifferences in the results.


    The Vickers’ micro-hardness values were measuredon the base material, samples without CNT, and

    Figure 5. Typical grain structures of EBSD image of AA6061-T6 samples (a) as received, (b) with one pass condition and (c) three

    passes; FSP Al–CNT composite with (d) one pass and (e) three passes. For the boundary misorientation: white lines: between 1� and5�, grey lines: between 5� and 15�, black lines: >15�. (The reader is referred to the web version of the article for interpretation of thereferences to colour in this figure legend.)

    Du et al. 5

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    samples with CNTs added (Table 3). The decreasein hardness value was observed when FSP was con-ducted on AA6061-T6. It is also observed thatincreasing the number of passes did not influencethe hardness of the samples without CNT. Thiscould be due to the dissolution of the hardeningprecipitates.26

    For Al–CNT composites, significant improvementin the hardness value was observed when comparingwith those friction stir processed samples withoutCNTs. This is due to the finer grain sizes and theOrowan strengthening caused by the addition ofCNTs. An increase in the hardness value was

    observed with the increase in the number of passes.This could be due to the improved dispersion of theCNTs under three pass conditions.

    Tensile testing

    The tensile stress strain verses strain curves wereplotted as shown in Figure 7. The tensile results ofFSP samples without CNTs showed that a decreasein yield strength compared to a non-FSP sample(Table 4). There is also a significant increase in per-centage elongation-to-failure, indicating an improve-ment in ductility. This is mainly due to the grain












    Misorientation (°)

    Misorientation HistogramAA6061-T6 1 pass

    AA6061-T6 3 passes

    Al-CNT 1 Pass

    Al-CNT 3 Passes

    Figure 6. Histogram showing the distribution of grain/sub-grain misorientation angle by EBSD.

    Table 2. Grain/ sub-grain boundary misorientations.

    Material and


    Mean grain

    misorientation (�)

    Fraction of

    high-angle grain

    boundaries (>15�)

    Fraction of low angle grain

    boundaries (415�)Number of

    samples(1–5�) (0–15�)

    AA6061-T6 1 Pass 23.11 0.50 0.29 0.50 49,871

    AA6061-T6 3 Passes 24.00 0.58 0.26 0.42 39,629

    Al-CNT 1 Pass 31.14 0.74 0.13 0.26 71,873

    Al-CNT 3 Passes 22.75 0.48 0.30 0.52 50,795

    Table 3. Micro-hardness values measurement of the base material, FSP of base material and FSP of Al–CNT composite.

    Materials and

    process AA6061-T6 AA6061-T6 1 Pass AA6061-T6 3 Passes Al–CNT 1 Pass Al–CNT 3 Passes

    HV 109.5 61.7 66.2 80.1 90.6

    Standard deviation 1.38 1.70 0.72 0.93 0.87

    Table 1. Grain size measurements using EBSD.

    Material and process AA6061-T6 AA6061-T6 1 Pass AA6061-T6 3 Passes Al-CNT 1 Pass Al-CNT 3 Passes

    Average grain size (lm) 70.04 4.49 5.04 2.11 4.67

    Standard deviation, SD 39.04 3.37 3.53 1.45 3.16

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    Figure 8. SEM image of the fracture site of the FSP monolithic Al plates with (a) one pass condition with �1000 magnification;(b) one pass with �10,000 magnification; (c) three passes with �1000 magnification; and (d) three passes with �10,000 magnification.







    0 5 10 15 20 25 30 35


    ss (



    Strain (%)

    Stress vs Strain

    AA6061-T6 1 Pass

    AA6061-T6 3 Passes

    Al-CNT 1 Pass

    Al-CNT 3 Passes







    3 4

    Figure 7. Stress versus strain plot of friction stir processed samples.

    Table 4. Tensile results.

    Tensile properties of Al base metal and Al–CNT composites produced by FSP

    Materials and process Ultimate tensile strength (MPa) Yield strength (MPa) Elongation (%) Young’s modulus (GPa)

    AA6061-T627 290 240 8 69

    AA6061-T6 1 Pass 220� 4 110� 4 27� 1 71� 1AA6061-T6 3 Passes 206� 2 96� 9 29� 1 71� 1Al–CNT 1 Pass 157� 4 120� 5 3� 1 57� 2Al–CNT 3 Passes 178� 28 112� 2 10� 5 65� 12

    Du et al. 7

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    refinement (Figure 4). A reduction in the yieldstrength was observed when comparing one passand three passes; this could be due to the dissolutionof the hardening precipitates.26

    The tensile results from the FSP with CNTsshowed no improvement in yield strength as com-pared to the parent material (AA6061-T6) withoutFSP (Table 4). However, the yield strength of Al–CNT was superior when compared to FSP withoutany addition of CNTs. For Al–CNT samples, therewas a significant reduction in the percentage elonga-tion-to-failure in both one and three passes.The CNTs could have acted as defects andstress concentrators during the tensile test. Thestrengthening of the material could be attributedto the grain size differences from Hall–Petchequation.9


    The fracture sites of the FSP samples without CNTswere observed under SEM and dimpled appearancesat the fracture sites were observed indicating ductilefracture. In addition, smaller dimples were observedin FSP samples that underwent three passes(Figure 8).

    For the FSP samples with CNTs, larger dimpleswere found on the samples with one pass conditioncompared to three passes. This is in agreement with

    the tensile results earlier indicating three passes ismore ductile than one pass. Some CNTs wereobserved in the SEM (Figure 9).

    Comparing the percentage elongation-to-failure ofthe specimens with and without CNT, the specimenwith CNT had smaller percentage elongation-to-fail-ure. This observation implies that specimens withCNT are less ductile. In addition, some CNTs wereobserved at the fracture site, indicating the CNTscould have acted as defects in the material under ten-sile load. The interaction between the CNTs and theAl matrix may not be strong enough in enhancing ofthe mechanical properties. The appearance of CNTsat the fracture sites of the samples that underwentthree passes also suggested that crack bridging couldhave occurred.12,28


    1. In this work, FSP on monolithic AA 6061 platesand Al–CNT composites were studied togetherwith the effects of different number of passes.For the monolithic Al 6061, the dendrites werebroken down and dispersed uniformly with theincrease in the number of passes. In the study ofFSP of Al-CNT composite, the CNTs have beensuccessfully dispersed with three FSP passes; dis-persion is more uniform with the increasingnumber of passes.

    Figure 9. SEM image of the fracture site of the FSPed Al–CNT samples: (a) one pass condition under �1000; (b) one pass under�10,000; (c) three passes under �1000; (d) three passes under �10,000.

    8 Proc IMechE Part L: J Materials: Design and Applications 0(0)

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    2. The Vickers hardness number decreased withincreasing number of passes for the AA6061 spe-cimens that underwent FSP due to dissolution ofthe hardening precipitates. For specimens withCNTs, the Vickers hardness increased withincreased number of passes. Overall, the speci-mens with CNT have superior hardness valuesthan specimens without CNT that underwentFSP, but inferior to the as-received AA6061-T6specimens.

    3. Grain refinement was achieved using FSP. Theaddition of CNT resulted in further refinementof the grains, improved tensile yield strength aswell as provided crack bridging in the material.The ductility of the material improved withincreased number of passes.

    Conflict of interest

    None declared.


    This research received no specific grant from any fundingagency in the public, commercial, or not-for-profit sectors.


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