Mesias a Desig 31 (2010 3880-3856 Contents lists available at ScienceDirect Materials and Design ELSEVIER journal homepage: www.eisovi com/loeata/matdes = Short Communication Mechanical properties of tri-modal Al matrix composites reinforced by nano- and submicron-sized Al,0; particulates developed by wet attrition milling and hot extrusion M. Tabandeh Khorshid, S.A. Jenabali Jahromi*, M.M. Moshksar igure of Maur Sconce and Enghesng Selo gern, ShiazUniray,FIRGESHISE Shr. ran ARTICLE INFO ABSTRACT ice sory Heceed 2 fay 2010 Accepted 25 Febery 2010 ‘Arvong al meal maria‘com poses, luna ithe most widely wand marx due ois low den ay coe ‘led with high tifiness In this study, aluminum matrix composites erinforced by two sizes of alursing ‘Barices (35m and Om) ate prepared hy wee attston ming and ot onward extrusion process, ‘The effect of che ratio af the nano: w submicron-sired particles (2:8, 3:7,4:6.5:5, and 6 in weight per ent) on mechanical properties oF te conspostes is evaluated Dy microhardness and tense (ests. iS ond that by increasing Mhe nanopaetcles content, the Misdnoss ad strenath of the composites Must ‘increase and then decree when the amount ofthe nanopartiieenceeds 4 wi The ens faccure sur {oces areal observed by Scanning ectron miceseagy. |. Introduction Metal matrix carmposites (MMCS) are promising materials fora ‘umber of specific applications in aerospace, defense, and aukoma- bile industries. Aluminum alloys are one of the most widely used ‘materials in MMICS as matrix from research and industrial View points [4] This is due to their outstanding properties, suchas light weight high strength. bigh specific modulus, low thermal expan- sion coeficieat, and goed wear resistance (2) tis well established that metal mintrix composites cam be rein. forced by particles and fibers. Continuously reinforced campasite: offer better specific strength than other carapasites: however. the production of high stength fers is costly, limuting thei industtal applications, In section, cantinuos fer reinforced compasites {0 not usually allow secondary forming processes, which limits their chaps used fn the original form, As a mecalt in recent years ew researches on non-contimously reinforced composites have been canducted. Compared to cantinnausly reinforced compares, the composites with noa-contiauous veinforcements present lav= fr production east, more adaptable processing methods, accent- able performance, relatively higher thermal stability, and better wear resistanoe [1 Amang all particulate reinfarced eompasites ‘ihe most interest is clbeervedl for those reinfarcel with hare! cera ‘ig particles due ro the possibiliy af controlling thelr mechanical properties Iny optimising the wolume fraction, size, ane distriba thon of the reinforeing particles in the matrix [3], Reinforcing the fuetile aluminum matrix with stronger and stiffer secand!-phase srgng ha Te #8917 513 1535: Gs 8 701230 72, man agree [sto raseruramacir (SA ne a2 30588 se oer maser ©2000 Beer Lt As reseed 1 areenedecomnna aA (© 2000 Esevier Le All right rxenved. reinforcements ike oxides, carbices, borides, andl nitrides provides 4 combination af properties of the metallic matsix and ceramic reinforcement components, leading to the improvement in physi- cal and mechanieal properties af the camposite [4 Composites reinforced by cares. barates. nitrides, and oxides havebecn successfully fabricated by powder metallurgy (P/M) and casting methads [3-7] The P/M process usualy invaves the maix= lng of powders ofthe mats alloy with the reinfoccing particles. follamued by cormpacting and solid-state sintering. This allows using lower temperatures than ather altemative processing methods With Jess interaction between the matrot and eeintarcemant. eis notable that some types of compasites cannat he made by other alremative routes (1. Concerning aluminum matix composites, PIM is ane of the most widely used processing mettwxds, due ta Its law processing casts coupled with its high versacily. ‘Annumber of BM techniques have been evelaped for praca ing metal matrix nanocomposites (MININCS), including mechanical alloying with high energy milling [8}. ball milling [9], nana-sinter- Ing [10], and wet mixing process [11]. Nonetheless, to obtain a desirable microstructure and to imprave mechanical properties. it is essential for all the particles to be homogeneously distributed in the mixture [1/4], However, due ta their poor wetability in the metal matrix and a large surtace-fo-Valume satio, the uniform dis pevsion of nano-siaed ceramic particles in metal matrix 4s a majar challenge, Hecate of this, wet attrition process that wtilfges a wet ‘medium is employed in this research. Aa atrifor consists af 3 ver tiealcumawith 2 series of impellers inside it haf filled with era balls ris known chat wet grinding is more efficient than the dry condition ta produce Finer-ground products, hecau'se the: solvent molecules are adsorbed on the newly formed surfaces of theCr thor a ano at sie 1 (2000) R803 = particles and lower their surface energy. The less-agglomerated condition of the pawider particles and accordingly better nano: sized particles dispersion in the wet condition is alsa useful fac~ ter [12). There are a number of papers in the literature Facusing an the: ‘iceostouctuce and mechanical poaperties af Al~AlyO, caunpasites [13-16], Among them. Kang and Chan [11] showed that by increas ing nanametric particulates cantent t0 4 vaLE, the strength af Al- ‘Al.Os nanocomposites increases; nevertheless, when the content fecteeds 40, the strength dows not vary due to agglomeration ‘of the nanoparticles. In the preseot work, Al;0y particles with ‘nanometer and submicron sizes ave employed as rekaforcement fan Al matrix, named as trismodal metal matrix composites ‘The effect of the weight ratio of the nano- to sulymicron-sized par ticlesion mechanical properties af the tr-madal composites ise: uated. To the best of cur knowledge. no systematic work has beer eeparted oa this subject to date. 2, Experimental procedures ‘The primary materials air atomized commercial pure aluminum ppowtler with a mean partele size of 45 jm and spherical pure ak Dha-Albty powiiers with average particle sizes of 3 nm (Nano-~ structured & Amorphous Materials, Inc) and 03pm (AMPCO}, ‘The PIM process was used to produce the composite materials, ‘At first, the nanometric AlsOx powder was deagslomerated by uutrasonic agitation in ethanol slury for 1h, Then, the resultant Slurry and the submicrometric Als0s powder were poured ints an attritian mil container. after Th attrician mulling te alumi ‘num powelers were added to the milled materias,in-which hard- fenod steel balls with 2 diameter af § mm were used a abrasive ‘media. The rotational speee! of 480 spm andthe bal-ta-powderr3 to (BRR) of 15:1 fw} were conducted with # h-milling time. The coraposite powders were dried at 150°C for 89 min. The resultant powders were ches subjected fo uniaxial single action compaction at 140 MPa pressure ta prepare billets. Final clensification process ‘was accomplished by hot ferward extrusion peocess.at 600 °C with the reduction ratio afapproximatcly 20:1 ta praduce dense rodsaf Genm in diameter. Hot forward extrusion is a common powder ongolidation route to praduce highly dente products without sin tering [17} In this process, the press ram pushes the compacted bbller rough a die ta produce the product. An all the specirnens, the total weight percent af the Al,O, reinforcement were LOWE. To investigate the effect af the nano-sized reinforcement addition on mechanical properties of the composites different r3 tos of the nanometric AlsOy powder to the subamicrometric AlpOy poweler were tested, including 23, 3:7.4:6,5:5, and #:-4in weight percent Polished surfaces of the samples were niserved by a scanning election enicrescope (SEM, Leica Cambridge S360}. The density of the specimens was measured by Archimedes water immersion ‘method. The theoretical density af the composites was qaicu- lated based on tte mixture rule; the density of the pure Al and ALO, peawrders was supposed! to be 2,7 ancl 297 gicr, respectively. Mechanical properties of the compasites were determined by ‘micro-hardness and uniaxial tensile tees. The micro-hardaess test ‘was performed with the load of 25 g and dwell rime of 15, The ‘micro-hardness cost was done on fine points for each sample, ‘The specimens forthe tnizxal tensiletests were machined paral fo the extmsion direction accoming to ASTM EB, with a guge Tength of 20mm, The tensile tests were conducted with Instron tensile testing machine and the crosshead speed af O.05em ua at mam temperature. For ractography studies, the Fracture surface Df the teneile specimens vs obeerved! by SEM. Fig 1. SUM icra oft sample wah the ato of the ato subir ‘ed parker af Ga cote at the wrows uncate the aplomeation a ‘Som partes 3. Results and discussion ‘The SEM micragraph af the sample with the ratio of the nano- tw submicron-sized particles of 6:4 Is depicted in Fig 1. The bright regione represent the alumina particles dispersed in the das alu- ‘minum matrix, Since the amount of the nanopartieles in this cam- ple is higher than that for the other specimens, a partial agglomeration of the alumina particles has occurred, 3s shown with avrows in the micrograph. Fig. % demanstrates the relative density of the consolidated samples, measuted by Archimedes water Immersion method. BY increasing the ratio of the nana- to subenicean-sized particu lates. the density first inereases slightly and then decreases, The: reinforcement pacticles which are smaller than the matric pati- cles situate among the matrit particles filling pares. This causes 2m increase in the density af the composites compared with the ure alurninum. Hawever, the increase in agglomeration of the pacticles wich increasing the nano-sized Aly particulaes leads tw the decrease of the density, It would be worth mentianing thar nanoparticles are prone to agglomerate and poses rerained in the agglomerated zones, witch causes to decrease. the density. The results of the micro-hardnes tests are presented in Fig. 3 ‘The results reveal that the addition oF the reinforcement te the AL mati generally inereases the mniceo-hardness value of the com posites, This increase fsa cansequence of dispersion af the ALO, Daticles in tke marcis. The mlcra-hardaess of the composites frst increases to apprmximately 83 Hy for the sample comtaining 4 wt nanoparticles, Howeves,for the specimen containing the nanapa— ticles more than 4 wet the micra-hardiness is reduced, Fig. epresents results of the tenite tests. The specimens con- taining the alwmina particulates exhibit higher yield anc! tensile strengths compated to the monolithic alurninurn In addition, sim= ilar ta the micro-hardness behavinr the strengths af the eanspas- ites fist inccoase with the nanemetric pacticulates content. however. wien the content of the nanopartilates. exceeds 4 wt the strengths eeerease, The strengoh ofthe alloys corresponds to the particulate-disio- cation intersetion acrording ta the Onrwan bowing mechanism, After dislocations pass the particles, residual diclacanion. Loops ane left around each particle. increasing the materials strength [ 8). af che particies are assumed to be equiaxed, che strength increment (Ac) is estinaated as hor 26bAL where L Osel2a waap Mr: Khost ea Mavs ana Design 1 (2010) 3880-388 Weight percent ofthe ubmiconsized ALO, 3” Ems gs» Bas ‘Weigh percent ofthe nanosized ALO, Fig 2 Relative density of the Weight percent ofthe submiconsized ALO, ‘Vickers Microhardness (Hy) ‘eit psc of the nanosized AO, Fig 3 Vickers micro-hanness ofthe alumina and comport, ‘Weight percent of the submicron sized AL,0; “Alvi ateth ‘Weight percent of he nanosized Al,0, ‘where Gis shear modulus.Lsthe interparticle spacing. b isthe Bur- gev’s vector, Vis the volume faction, and isthe grain diameter of the reinforcements [15]. On the other hand, the difference in coef- ficient of thermal expansion between aluminum and AlsOs leads to the generation of dislocations. The dislocation density generated (9) a function of reinforcement size (d, volume faction (V), the product of the thermal mismatch (AC) and the temperature change (AT), The strength (ng) can be estimated by the following reation- ship 119] ca—2Gbp' where p — 12ATACK/bd 2) where G is the material's shear modulus, b ig the Burger's vector and 2 is a constant between 05 and 1, According to the Orowan bowing mechanisiy and thermal mismatch between the matrix and reinforcement particles for MMCs [19-21], by decreasing par~ ticulate size the strength increases. Note that since the particles in this work are small enough (<1 jim), the Orowan bowing mecha- nism can be used to justify this behavior 19], On the other hand, since the difference between the processing and test temperatures {is large enough, the contribution of the thermal expansion coef cient mismatch to the strengthening is considerable, in this work, the decrease in particle size is equivalent to the increase in the amount of the nanoparticles, resulting to the increase in the strength. ‘A decrease inthe micro-hardess and strengths of the compos- ites was observed wien the nanoparticles content exceeds 4 wt. It has been found that when the amount of nanoparticles increases, tthe uniform dispersion of the particulate becomes difficult and consequently agglomeration occurs. The agglomeration reduces tthe relative density ofthe composites and accordingly the micro hardness and strengths by providing sites for crack initiation from Pores in the middle of the agglomerations. Moreover, when the agglomeration occurs, the actual interparticle distance becomes larger than the theoretical distance, causes to decrease the strength based on the Orowan mechanism. Apart from the agglomeration effect, when the nanoparticulate content exceeds 2 critical value, ‘the grain boundaries would be saturated with the nanoparticulates [11]. This gives rise to the formation of a continuous brittle phase along the grain boundaries, diminishing grain boundary pinning ‘and weakening the strength of the composites This suggests that {the effect ofthe agglomeration and the formation of a continuous brittle phase along the grain boundaries on the mechanical proper~ tes prevails over that of the strengthening mechanisms illustrated above, Iis noteworthy that the results ofthis work are in agreement with previous studies. I was found that in Al-Al:0, composites possessing nanoparticles more than 4 vol%, the increase in the reinforcement has no considerable effect on the mechanical prop- erties, due to the inhomogeneous distribution and agglomeration ff nano-sized reinforcements [1]. Additionally, in Al-SiC nano- ‘composites when the volume faction of SiC particles is higher than abOUE 5%, a decrease in the strength was observed [20]. SEM micrographs of the tensile fracture surfaces are shown in, Fig. 5. There is a large difference between the appearance of the fracture surfaces ofthe pure aluminum and aluminum matrix com- posite reinforced with alumina. ig. 5a and b displays the fracture surface of the pure aluminum in two different magnifications. In ‘these figures, large dimples can be recognized. Voids nucleate fram some inclusions in the matrix, grow and coalesce, This fracture ‘mode is known as the dimple rupture, Fig Se and d depicts the fracture surface ofthe composite with ‘the ratio of the nano- to submicran-sized particle of 3:7 and Fig 5e and f presents that ofthe composite with the rato ofthe nano- to ‘submicron-sized particle of 4:6, In contrast to the pure Al sample, dispersed shallow dimples are observed in Fig. Se-f whereas in the latter micrographs the size of dimples is various due to the differ~ fence in the size of the reinforcements used, The number and dimension of the dimples observed in ig. Sc or d are relatively more than those observed in Fig. Se orf This s due to the fact that ‘the amount of the submicron-sized reinforcements of the sample ‘with the ratia of 3:7 is mare than that of the sample with the rio ‘of 4:6. Note that cracks generally initiate from interfaces between the matrix and reinforcements. By increasing the amount of the nnano-sized particulates, crack nucleation sites increase, When the ‘numerous nucleation sites are activated, adjacent cracks coalesce and fracture accurs before they have an opportunity to grow and ccan form larger size dimples.Cr thor a ano at sie 1 (2000) R803 igs stat musopph afta tenes ature artes “4. Conclusion In this research, aluminum matric composites reinforced by ‘two sizes of alumins particles (aanometric and submicron sizes) ‘were prepared by wet attrition milling are hat forward extrusion processes. It was found that by increasing the ratio of the nano~ {tn submicran-sized particulates the relative density first increases and then decreases, The amount of the mieso-hardaess and ‘strengths of the rrmposites first inemsases andl then deereases by increasing the nanoparticles content. The increase in the mechan fecal properties was explained by the Orowan bowing mechanism {and thesmal mismatch benweea the marax and reinforcement par ticles, Forthe samples havingthe nanaparticles morethan-4 wea doctaase io the strengths was abserved, attibuted ro the agglom- eratioa ofthe nanoparticles and the formation of a contiouous brit tle phase slang grain bourdaries In addition, the dimension af dimples formed in the Fractured surfaces decreases by increasing the nano-sizedl particulates. References oy Toaaina yaaa coxa CE veusco Ff atminu mae compontes: an rere, [ter Paces Pec! 2008 13cau3 (ey zeroth Sate Dapenency ot pyc se mechanical peperes af reectankal aloyed A AsO) composes on rallitg time Mater De: (3) Yoncarcave per A Doorzaten 1A eres. Aanmiae abmufsoun 2 omanum mabe lois mates rstces Ay pee | Ae Mas mecttey supa cot 140 he pore amin ean teal eand he ecmpnsae-nith the sais athe mont sbi ph imo 48 [i] Potbe 8, Saaremaa Cheacesiewion of gh ele L Maidan 8 Syathests and IAA snare pee to ty bghenery rng Nn Si Eg 2 Ist Ltrs Tae. cone nario neal mt cogent | Mater Foves Feces! #805 482712 Fn St 8 oat [10] Gree, BL Sri af meena pnmde, tt | Pome Mel ‘one anso-85" erg ¥€, Slam Sl Tre props of nari ALO. tic ured Slamiean uein conpentes, Marr Ghee Pay! 300 oz) Suryaarovons C Mectonicd atoye: and mung frog Mer 5 (t3) Raza Hest 2 Matinoar HR Sinchi A Aa scvecigaton on GGapresiily af lamnumiaana slanana crmpaste cove peared By ‘Seana semachanscl mling Mater Sa Emg A oor sce 53 Pot ee, Guay AC, Maller ak Fscune toughnes ot mucmaptae ‘As AU parties met mara compoutes Componter 20038 a0. Zsoapad SM, Sajal SA nhkosrucare eahanian of Al Ae compodte froaiced by mecca aoyingenetod. ise bee 2066-7088 8. joo) eet Meee Sima A Se amar Sk Sours coon Suna ‘estas rlling a wnamesns andeacaretnc ADs elrced Almas Ganpoates arersa Eng a snGez¥- 8 or) Cate ie arom Kaucuwan ®, Mack We Consol of ma paar sng the eraser pov | Nan rose ean 002ase er Aho ont: ot sige 1 (2000) m0 se 8) Me 2¥. Us MA tase Bone 8 Te SE Mime. SNA [0 Zag Chen Canin of wen stating fin pare Darieerenirce!alminare comgasite Sows Sci Ene A 1980:208 enforced ‘el utr sanacargesits. Miter Sang 8100844 Dest ‘crabs [19] Miler WS tumphreys F smengthening mecarioms im paricaine metal (21) SHAE 2, Tropa 2 Cabbibe ML vargas E,Sweraeing Sm a WES ‘abc composes, Sols Metall Maer 1994-2808 nage alloy contig Spaces Mater Sc ng A 2007 #2.229-8,