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Materials and Design

journal hornepa ge : wwur. eJse vier. corr, i oc arelinatd€s

A comprehensive microstructural analysis of AI-WC micro- and

nano-composites prepared by spark plasma sintering
W.-*r".0

Amir Pakdel n'*, Agnieszka Witecka b,

Caulthiel l{.ydzek ", Dayangku Noorfazidah Awang Shri '
t' t*situte ofFuruiarnentd fechtrologtco/ R esearcb, Palish Anr)enry oJSrien.es. Wanaw, Polaild

' i:artfiry of Nlecltarticfii Ingtneenng, tJniye$iti Malaysit Pnhorrg Pelorl Pahanq, lulttl{ttsia

t-llcHLrcl,r ]'s C iiA P I-I I IA I- A B SI'R A C1

' Alurrinum rnJtrix colriposites contain-

i]lg i-10wt.% WC uricro*, nano- and Press{re
birnodai-particles are consoLidated bV ":.:1.-,-
spark plasnra sirltering (SPS). 7
. lhe higirest and lol.i'e st densifiration
levels are obrained in 1 Ht.7. i i........ ...... I
micr"oc::mposites (99.82J ancl 1{l lvt.?;l it. lFon*det ,i
i

nanorr:mposites ( 94.4%), r espectively. i .*-t--*-*-]_... i

. tl
Hai.dr.iess irtcleases bV SPS ternperaillre
.,.'.'.'''\
(400 * 500 "C) in 5 and 10 wt.?i l\
u:ir i-ocomposites, but slightly decreasrs
i-*
I
:":**-B-ir:"!-ql
5 10
in 1 nt.id microcomposites. PreSsure .. ,
wt-% of WC
. Nanocornpo-sites achicve largest ha|d- SBark pleeft:a $1*iering of
rless at 5 rvt.'Z WC concentration, but Ai-Wd composites -':.ffi
ic t0structilr*$
Mechanical pr*pe*l*s
rnicro- arrd biriroddi.ror)ipoiitcs ;re
hdrdcst aI l0 wt.'; \vL (onccntl.]tioll.
. Interplay betlveer] WC paiti.les dish-i-
buLiort honrogerreiry ar:d (ornposrtL
cornpressit:i1ity during SirS dictate rhe
irardening level acirievabie i;t the con:-
posites.

ARTICLE INFO ABSTRACT

Artide histotlJ: l'here have been mairy investigations on metal matrix microcourpositcs produced by conventional casting
Receive{l 4 Nlovembfr 201 6 routes; horrever, in the past decade, the focus has shilted more toward uanoconiposites produced via solid
Received in revised forrn I !i January 201 7
siate routrs. 'l'o have a realistic view of perfonnance plediction and optimul)r design of such composites,
Atcepted 21 Jaouar'\i 201?
in this work Ai rnatrix composites (AN,lCs) reinforced with WC micropariir:les, nanoparticies, and bimodal
Available online 25Januir-1/ 20i7
micro-inano-particles were prepared by spark plasn"la si11(ering.]'he effects ofparticle size a1ld {olrce1ltration,
Kewoils: and process v.rriables (i.e. sintering temperature, duratiou, and pressure) on the evolution ofmicrostructure,
Composite der.rsity and hardness of the conrposites were studied con"iprehensiveiy. Full densification olAMCs with lrigh
N.rnoparticle particle concentration was problematir because ofceiamic cluster filrmafions in lhe rnicrostructur-e. "lhis effect
i\,'liciopar tirie was niore cnrphasized in AMCs contain jng nanoparticles. AI\{Cs with mic|oparticles were inore easiiy diflsifieri,
Pswder rnetaliurgl/ but theil hardness benefits were inferior". On the other hand, tlie mixture of rnicro- and nano-particles in AI-WC
bimodal conrposites led to better matrix reinfbrcement iutegr"ity and an overall improvelnent in the
fulicrostftrcture microstructural propertics. L-inaily, incrcasing the sintering temperalure irnproved thc micrcstructur"al features

* Coileslronding authsr.
f-mail cddress: PAKDEL.Alrrir(qrrlins.gojp (A. Pakdel)

h{tp:,/r'dx.doi.oryr1 i). I 01 lj,,j.nr:rder.20 i;.t1.064

4284-.1275:O 2A17 Elsevier L{.i. Aii rigilfs reserued.
 A. Pakdel et al. i Marerid$ ond Design 1 l9 {2A17) 225-234

and hardness oFthe conrposites (more enhanced in higlr wt.% samplesj, but sinrering dur"ation.lnd pressure did
not have a big iarpact oll rlle composite properties"
o 201? Ersevier Ltd. AIr rights rcse,.r'e.i.

1. Introduction However, these consoliclation techniques may have some adverse

One of the most common means to evaluate an industry's vitality is
ttt look at its product demand. For conrposite materials, the picture is
promisirig as den:and for encl products reached $22.2 billion in 2015,
with rhe lop market segments in lransportationlautomotive, construc-
tiort. aerospace. ano pipe and iank applicatiorrs [] J. Thc cornmon aim
in designing and using contposite materials is to go beyond propelty
boundaries attributed to common classes of materials. In this regard, a
big irrterest has been given to the development of metal ntatrix compos-
ites (MMCs) in which rigirl ceramic reinforcements entbedded irr a duc-
tile metal or alloy matrix can result in high strength and toughness as
well as excellent, resilience and hardness. Aiuminum matr ix composites
(AMCs) are a good example in this case as they benefit tiom excelient
ductility, corrosion resistance, recyclal-,ility, ancl fornrability of alumi-
num as well as high stiffness, strength, hardness, and wear resisfance
of the ceramic component l2 j.
Among the ceramic materials implentented to reinforce the AMCs so
far, carbides (SiC, TiC. WC, TiC) l3- 14], borides (f iBr, Al82) [ I 5-1 8].
nitrides (SirN4, AIN) t19 241, arrd oxides (Alr03, SiO_2) 125-31 I have
been more commonly investigated. However, there are several
chalienges associated with the introduction ofthese particles into the
metallic nratrix. For exanrpie, liquid-state processing techniques (such
as stir casting, sqlreeze casting, infiltration, and die casting) [32"33j
sufler fronr poor weltabiliry oF the ceramic reinforcements by the
molten metai, as the rnelt has a very high surface tension (of the order
of -1000 mJ m 2) [34]. Also the specific weight of the ceramics ancl
molten metals are oiten considerably different. As a result, non-
uniform distributian, agglomeratio!r, and weak irrteriacial bonding of
the particles in the metallic matrix are often unavoidable 135-351. In
addition, in the case of carbicle and oxide particles in molten aluminum
unwanted and brittle phases ofAl4C3, Al(OH):, and Si niay form due to
processirlg at high temperatures !40,411.
An effective soh,rtion to overcomirrg the aiorenlentionecl problerns in
MMC manufacturing is the application of solid-state processing tech*
niques. For instance, the use of mechanical milling followed by consoli-
dation techniques, such as hot pressing, extrusion, forging, rolling, and
cold isosfaric pressing, can lead to more uniform disrribution ol rhe
hard ceran:ic phase into the relatively soft metal matrix [39,42-48 j.
effects on tlre composite properties as well. For exanrpie, the applied
high temperatures and long sintering time can lead to unfavorable
interfacial reactions, oxidation, and grain growth that can deteriorate
the mechanical properties [49-51J. Recently, spark plasma sinterins
(SPS), a no;.t-conventional sintering process, has proved itself as an
excellent technique fbr the consoiidation of micro-.and nano-
composite powders. In this method, uniaxial pressure and pulsed DC
current are applied to the powder sin-rultaneously, as schematically
showrr in Fig. 1(a).The urriaxial pressure can greatly redrice (or i:ven
completely eliminate) porosity and .rlso break up the otherwise intrr,r-
sive bxide layer on aluminum particles [52.53], while the applied cur-
rent heats the powder rapidly viaJoule effect alld pronrotes enhanced
diffusion rate of the elements [54]. Moreover, short processing time in
SPS can minimize microstructural coarserring, and effective boncling
between particles can enable the synthesis of highly ciense materials
t53-571.
Civen these beneficial traits, this research aims to conduct a compre-
hensive study on the SPS consoiidatior-r of AMCs reinforced with tung-
sten carbide (WC) particles, and to analyze the effect of process
variables (SPS temperature, pressure, and rirne) as well as ceramic
particle size (nanc, micro,.rnd mixed) and volune fr,action on the
microstr-ucture and hardness of the conrposites" In tl-ris work, WC parti-
cles were the material of interest for re inforcement due to theii remaik-
able harclness and stiffness as well as their good wettability by
alunrinum and capability to undergo snrall amount of plasticity i3l.
Furthermore, there has rarely been a systematic study on the inter-
relationship belween particle size/quantity and rricrostructural charac-
tcristics and nrcch.rnical propeftics olAl-WC cornposites.
2. Materials and nrethods
The pnwders empioyed in this work were aluminum (Wal<c Fure
Chemical Inc[lstries, Ltd., Japan, average size *44 prn) and tungsten
carbide (Clobal Tungsten & Powdels Colp., USA, average size -200 nm
and -20 pun). Micro- and nano-composites collsisting of 1,5, and
i0 wt.% of WC were fabricated by blencling and mixing the rnatrix and
reinforcement powders in an agate mortar for 30 nrin to get a homoge-
neous nrixing lollowed by sparl< plasma sintering (Dr. Sinter 1080,

' lvrt€r-{ocled *l*ilrsdr

Graphite 5Da.e.5

'> 6rmFh:te pun{h

, 10
6ra,rhitedie

OB

> Varu0fi clrmber

.9 --
$.c

an Al-UlC mic.oconlposite.
 A. Pakdel et nl. I Materials and Design ] 19 (2017) 225-234

Sllmitomo Coal Mining Co. Ltd.,Japan) under argon gas fbr consolida- wt.% WC {rnicro}
tion. The 1, 5; and 10 wt.9J WC san.rples consisted of I g of aluminum
powder ancl l 0 mg, 50 nrg, and 1Otl mg ol WC powder, re spectively.
-*Al-10
Al-10 wt.o/o WC (nans)

Each powder sample was placed in a high strength graphite die that a -
containecl graphite foils to line the die wall and punches. They were
tlien heated at d rate of 100 l(/nrin using pulsecl DC current. Peak tt
sintering tenrperafures were 400 "C, 450 'C and 500 "C, and the speci-
mens were held isothermaliy fbr: 5 nrin before furnace cooling to roont 4,
d
temperature. Higher ten-rperamres were not used to avoid the possible o o r1
tJ U U
oxidatiorr of WC powder that can readily staft at >520 "C [58"59]. Flow- 3 TJ Lr
ever, lhe authors may recommend using higher sintering fenrperafures 3 3
it the SPS pfocess can be performed under very high varuum levels. A
uniaxial pressure of 50 MPa was maintained throughout the complete
SPS cycle. The manufactuied disc-sh.rped specimens hacl a nominal
'10 z0 30 40 50 60 70 80 s0
diameter and thickness of 10 mm ancl 4 mm, respectively (Fig. 1(b)). 2S (degree$)
Characterization of the sintered samples included the chemical anal-
ysis, micrcstructural imaging and measurenrents of density and hard- Fig.2- A compadson lleiweeu ahe XRD patterns ofAl\{C micro- and nauo,composifes
sintered at 500 'C.
ress. The initial chemical analysis of the niicro- and nano-composites
was pefolmed in arr X-ray diffr'actometer (Altima III" Rint 2000, Rigaku
matrix as well as sharp peaks ofWC from (U01 ), (100), and (101) planes
Corporation) using Cul(u radiarion. The microstructure of the speci-
and small peaks of WC from (111), (102), and (201 J planes. However, in
mens was obselyed with a. field-emission ultra-high resolution scan-
the XRD pattem of the nanorjomposite [he majorWC peaks din.iinished
ning electron microscope (5U8200, Hitachi, Japan) equipped with an
antl widened while the minor peaks disappeared.'I'he XRD patterns of
energy-dispersive spectrometer (EDS) and an energv-filtered back-
both micra- and nano-composites confirm that no new phases formed
scattered electron detector. The density olthe specimens'was measured
during the SPS processir.rg at 500 'C. That is, the leiatively low process-
using the Archimedes' principle according to ISO 2738 standarcl. The
ing tempelature successfully avoided the forn'ration of harrrrful phases
nteasured densiry was compared to the value calcuiated lrom a rule-
(such as Al4C:) that could clereriorate the mechanical properties ofthe
of-mixtures approach tcr determine the volume lraction of porosity. ,-'omposites.
I'he hardness values of the specimens were measured by a Rockwell H
hardness tester Llsing a ball inclenter (Wilson Rockr,nrell 2000, Buehler,
a division of Illinois Tool Works hrc., lllinois, USA). In each case, the 3.3, Dcnsitl, n?('usul?mcnfs
average value was calculated from the measurements on 3 specimens.
Each specimen was tested 4 times on 4 different spots. The WC concentration and consolidation temperature had an
imnrense influence on the relative density and porosity level of the
3. Results and discussiorr microcomposites. Fig" 3(a) shows ihe variation of the microcomposites

3.1. DensiJtcatiofl process und sirrfenngph enolnena 100

As SPS is a relatively new cor-rsolidation iechnique, the whole physi-

cal phenomena promoted by the pulsed continuous current is not fuily B<

understood yet. The general idea of plasn'ra formation pioposed by

Tokita [6n] is still an open debate l6:,621. However, it is generally 6s6
c
believed lhat during SPS a high temperature is attained in the contact {,
area of the powders, which may even exceed their melting point.'Ihis or ^,
>v4
can locally melt the powders and lead to excellent interparticle bonding
s(l +Al-1 M.cA WC (micro)
iS3l. lt is worth mentioning that such overheatir"rg is localized on the *sz
surface of the particles, sirice the teniperatllre gradient along the parti-
+-Ats wt.0,6 wfr (rnicrol
+ Ai-'l 0 vrt.{o WC {micro}
cle radi us is very steep. Thus, rhe bulk of the parricle is practically unaf-
fectrri l:y the sr:iface phenomena lG4l. 400 45S 500
SPS Temperature {"C}
Fig. 1 (c) shows a typical SPS pr"rnch displacement of an Al-1 wt"% WC
microcomposite versus tir-r-re. The densification process can be catego-
rized into three indicative stages with the following sequence: ( 1 ) the
initial cold packing stage during which sliding and rearrangement of
particles resulted in small densification; (2) the warm packing stage
dur-ing which tlre powders rearrange further, pores get connected and x""
-oR
surround the particles; tlrus, mediocre densification was obtained; and ut
(3) the hot packing stage during wl.rich the pores berween the particles o
can be sealed offand lead to high densif,cation. After the end ofthe final
>YO
stage of densification, no noticeable displacentent of the punches was {s
observed although high pressure and temperature were kept for several (,
adclitional minutes.
u *-..* AI-WC {nano)
- *- AI-WC {micro}
94
j.2. X-ray tlifrraction 1 $ 10
ry1,7q of WC
The XRD patterns of Al con-rposites reinforced with 10 wt.% WC
Fig.3" ia ofsintedng temperature oil the density of dre microcomposires reirrforced
I EUect
micro- and nano-particies sintered at 500'C are illustrated in Fig.2. with and i 0 wt.ii !,VC nticroprraicles. (b) A contparison berween the dersiry vari.ttion
1. 5,
The XED pattem of the microcomposite showed large peaks of the Ai oi the naDocornposites and ilicrocomposites witb WC (orcltiltratiorl.
228 A. Pakdtl et eL ! lt(aferieh flnd D€sign 1 19 QA17) 225-2i4
density as a function of SPS ternperature. To avoid the possible oxidation
of the WC particles, the maximunt sintering temperature was set to
500 "C which was sufficimt to achieve full density (i.e. relative
density > 99.8%) only in one ofthe speciniens. The highest level ofden-
sification was obtained tbr Al-i wt.% WC specimens with relarive den-
siiies of 99.8%, 99.0?4, and 97.5?{ at SPS temperarures of 500 'C, 450 "C,
and 400 'C, respectively. This temperature dependenry oIAMC densifi-
cation could i:e attiibuted to thernral softening and betrei formabiliW of
the niatrix powr.ler at higher ten-tperatures. When the concentration of
WC microparticles increased to 5 wt.z; the densification !evel sliglrtly
clinrinished (as compared to that of Al-1 wt.% WC specimens) wirh rel-
ative density values between 98.97i and 95.77.. By further increase of the
microparticle concentration to 10 wt.% a stronger emphasis to this trend
r,vas observed. 'l'he highest relative densify for Al- 10 wt.,'{ WC speci-
mens was 96.6% at the sinrering temperature o1500 'C, and this value
fell to 92.173 for the specimens sinterecl at 400 'C. Overall, tlie effect of
SPS femperature on tlie clensification levei of the microconrposites
was more pronounced in specimens with higher ceramic particlr
conc*nffation.
Since the microcomposites consolidated at 500 "C had the highest
density vaiues, the nanocomposite specimens were onlv sintereC at
500'C (and not iower temperatures). fig.3(b) shows the variation of
der-rsity as a fuuctiotr of WC nanoparricle concenlration. For comparisor,
reiative density values of nticrocomposite specirnens are presented as
I
weil. At low WC concentraiion i wt.%) both micro- and nano-
composites exhibited full density values. hor,^rever as the WC concentra-
tion increased the density ofthe nanocomposites dropped nrore drastical-
ly tlian those of rhe microcontposites. That is, the composite specimens
with higher reinforcement content smaller WC particles were less ef-
"rnd
fectively densified. lhis is partly due to the greater strengrhening eflect of
the nanaparticles as canrpared to that of rhe microparticies, which arises
from the plastic constrairrts ofthe nratrix caused by the hard elaslic parti,
cles- In other wor"ds, while the applied pressure was high enough for the
piastic deiorm.rtion of the metal, the rigid non-plastically-deformed pafti-
cles hinclered the plastic flow of Al powder toward densification. In an
MMC with a specific wt.% of reirrforcement, decreasing the particle size
(i.e. inrreasing the nun-rber of particles) leads to a gre.lter rrumber of con-
straints against the plastic flow ofthe ductile maffix, and consequently
less effuctive densification. Similar trend has been reported for isostatical-
ly plessed of Al-SiC microcomposites,,uvhere decreasing the particle size
required higher pressure for achieving a given densification level 1651.
As will be shown in the next section, another reason for the decline
oi rhe compnsitcs compressibility wirh increasing rhe hard particle
1wt.%
400 "c
500 "c
50 gm
I
Fig.4. Low nt:gnificatioo backscatlered electrsn iiniges 01'the AMCS reinforced with 1,5, and 10 wt.%WCmicroparricies sirtered at400 "C (a-c) and 500 "C
content is the clustel formation in the matrix. The consequent interpar-
tjcle friction can hinde{:the honrogeneous distribution ofthe applir:d
load lE6l. Numericai simulations also tonfirm that the local rearrange-
ments of particles strongly influence the resistance to densification,
and as a lesult the relative density can drop with increasing the rein-
lorcement content in MMCs {67J.
3.4. Microstrut turol rrnfl lysis
Low nragnification SEM images conrparing the general microstruc-
tures of the AMCs reinforced with 1, 5, and 10 wt.7,j WC microparticles
and sintered at 400 "C ancl 500 'C are shown in Fig^ 4. The microgr.rphs
of the 1 wt.7; WC specinrens showed snrall agglomeranons of the ceram-
ic particles mainly occurring at Al particle interfaces. Tlrere also existed
microvoids in the uratrix, especially in the specimens sintered at400'C.
Faneis (b)*(c) and (e)-(f Fig.4 illustrate that with increasing rhe WC
concentration, larger ceramic clusters formed in the composites. That
is, the rlistribution of the n:icroparticles became less hcmogeneous in
the specirlens with higher reinforcemenl concentration. An overall
comparison between the n:icrocor"ltposites sitltered at 400 "C and
500 'C reveals that cluslerillg of cer-amic particles was in fact r:ot influ-
cnced muth by rlrc sintering rcmpcr.tturc; br.rr. marrix porosiry
improved with the SPS temperature.
A more detailecl inspection on the effectS ofreinforcement contenf
and SPS temperature on the nricrostructure ofthe nlicrocomposites is
provided in Fig. 5. The h igi: magnification backscatterertr electron r.nicro-
graphs of Fig. 5(a) and (b) indicate that during the compaction and
sintering of the i wt.?l WC microcomposites sever cracl<ing and breal(-
age of the WC particle occr:rled. That is, during the initial ccld densifica-
lion stage (and n-raybe even the warm dens!fication stage) larger
particles tendecl to fragment probably due to stereoiogical factors
(such as proximity with other particles and reiative shape) ancl stress
concentration. This is a particular feature that has rarely been reported
and discussed in SPS processed MMCs, and needs further investip;alion
to assess possible limitations on SPS processing of large-size
inicroceranrics in MMCS. Panels (b) and (c) in Fig. 5 show that the conr-
posites sintered at 400 "C suf,fered ftom pniosity ancl nticrocavity forma-
tion at sonre interfaces between the ceramic particles aild the matrix.
Moreover, the large cluster of WC pafiicles in Fig. 5(c) further contrib-
utes to higher ievels ofporosity in that specimen. Panels {ej and (f) in
Fig.5 der::onstrate tharby increasing the SpS temperature to 500 'C bet-
ter interfacial features and iess microvoids were obtained (also evi-
denced by the highcr densification levels shown in Fig. 1). Tl.ris is due
5 wt.% 10 wt.%
ld-q.
 t\,.ljokd?l €t al.
1wt.%
400 "c
500 "c
lractu{e:s \ycll as lrit:rol,oids are uoticed in the microstmctures.
to the matrix soflening aspects aclive at higher temperatrires which
allow a more facile penetration of the matrix around and betlveen the
ceramic particles. ln other words. by increasing the SPS temperature
to 500 "C the flow stress of the A1 matrix was lessened to a level that
the applied pressure was slfficient to force Al to pr355 through and
encapsulate WC particles. There{bre. the porosity .rssociated rryith
small ceramic clusters as well as nratrix microvoids were diniinished
clue to the higher sintering ternperature. However, this phenomenon
was not completely effective for the elimination of iarge cluster,
associated porosity; since in this case, the nretallic nratrix could mainly
surroLlnd the cutel layer" thereby leaving the inner ceramic core
(Supporting infbrn-ration Fig. S1 ). This ceranric core consists of non-
deformable particles, and acts likr: a parous medium because of gas
entrapnlent between the particles. Moreover, it can create a localized
increase in electrical resistivity that can cause a more acute diversion
ofcLlrrent dudng SPS and adversely aflect theJoule heating and densifi-
c.rtion process, as .iepicted in Fig. i:. To be mole precise, when the elec-
trical potential is applied to graphite punrhes during rhe SPS process, a
high energy electric spark is created. The discharged spark can remove
the surface contaminants from powders and form a solid cohesive
Jaule heating .::,,.',a S{rtacg higl temperature
Discharge i..: Laeelized max temp€rature
Fig. 6. A schematic iliustratior ofthe 5PS piocess.
i Nlaterials nnd Design 1 !9 QA17.j 225"234 I ?C)
5wt.% 10 wt.7+
mass. Immediateiy after the sparl(, the current is continued for a few
sr''conds and flows through the conductive Al matrix: Consequently,
the powders are heatecl up quickly with different mechanisms; for in-
stance, Joule heating of the powders in conlact, or the electrical dis-
charge between powders in a close disrance. However, when the
current reaches the non-conductive WC particle cklsters it gets diverted
around lhcse Al*WC*Al junctions. As a resr"ilt, the Iocalized Joule-
heating and densilication level in those spots decline.
Fig" 7 shows the microstructurai assessment of the nanoconrposite
specimens. Low- and high-magnification SEM images ol 1, 5, and
-10
wt.?6 WC nanocomposites demonstrate fhe spreading of WC nano-
particles in the boundaries and interspaces of Al particles.'lypical EDS
eiemental maps showing the spatial distribution of Al. W, and C irr the
nano- and nricro-conrposites are prrvided in Figs. 52 and 53 of the
Supporting information. Fig. ? depirls that similar to the case of the
microcomposites, by increasing the concentration ofthe ceranric parti-
cles in the nanocomposites more agglomeration and larger-sized clus*
ters of WC were formed. However, a conrpa|isori between the
backscattered SEM images in Figs" 5(a)-(f and 7(a)-(c) reveals that
the distribution olWC nanoparticles was more efficient than the case
of WC microparti{:les, as ihe observed ceranric clusters were less iie-
quent and smaller-sized in the nanoconrposite specirriens. High-
magnification micrographs in Fig. 7(g) and (h) contrast the formation
of particle agglomerations and micrcvoids in the microstructure, as
well as the intragranular dis(ribution of the nanoparticles. That is,
while ther"e was a network of WC nanoparticles within the intergranular
spaces of the Al matrix, some nanoparticles were also spread through-
out the Al grains. Therefore, the nanocomposite specimens yielded a
better particle distribution as compared to the microcomposites.
j.5. Bimoclal micro- ltnno- composite s
l'o benefit fiom both the better densification and less porosify ofthe
microcomposites as well as the nrore homogeneous particle distribution
of the nanocomposites, bimodal (mixed) micro- and nano-WC powder
mixtures were incorporateal into tlie Al rlatrix. Low magnification SEM
images comparing the general mtcrostructures of the bin"rodal AMCs
reinforced with 1,5, and 10 wt.% \{/C particles and sinteled a( 500'C
are shown irr panels (a)-(c) in lig. 8. It is noticed that the bimoclal
micro- and nano-particles in 1 wt.% WC composites were ntainly
clisnibuted throughout the microstructure alnrig the boundaries of the
Al particles. Similar frend existed in 5 wt.% WC coniposites; however,
230 A. Pakdel et aL i l,4ateriab and Design 1 i9 QA1?) 225 2:4

1wt.% 5 wt.% 10 wt.%

lg) r{ggioneratir:n ofWC nJnoparticles iorergranularlv iDd ilrl rheir intragranular distribution witlrin the A1 grains.

smail agglomerarion of WC partides was noticeable through the rlicro-
structure. With incleasing the WC concentration ro 10 wt.%, larger WC
clusters formed and the distribution of rhe bimoclal pafiicles in the nra-
trix bec.rme less r-rniform. Higher magnifiration SEM images in i;ig. S(d-
f) indicate a Eiood interfacial bonding berween the particles .lnd rhe
matrix (no obvious microvoids or microclacks), and encapsulation of
the nano- and micro,Wc particles bv the metallic niatrix. Panels
(e) and (f in Iig. I particr,rlarly show the distribution of smallerWCpar-
ticles not only around the larger particles (i.e., forming ch-rsters) but also
spleading through the Al nratrix. In contrast to some prevrous repofis

7wt.% 5 wt.% 1*wt.%

 A. Pukdel et al. I Materials and Design I 19 {2017) 225-234
bE
Fru
o when the SPS pressure was raised from 50 MPa to I00 MPa- WC clusters
o in fig. 10ib) indicate rhat doubling the
E imnrense effect on the distribLltion of the ceramic particles in tlie metal-
.$ *u
(8
E -.* AI-WC {nano)
d - r- AI-WC {miffo)
--*-* AI-WC (bimodal)
94
1510
wt.% of WC
Fig- 9. A compaliso0 betweeu tlle effect of WC pirticle concentratioit in
b inrodal-.coirrposites.
l3 j. no trace of chemical
interafiions between Al and WC, dissoh.rtion, or
fomration of an interfacial microlayer was detected in our specimens.
Fig- ! compares the relative density of micn:-, nano-, and birnodal-
composite specimens. lt indicates the better densification ol bintodal
coriiposites corlpared to nanocontposites, with relative density values
close to that of the microcomposites. In general, considering tlte better
matrix-reinforcement integrity and the ovelali irnprovement in the
microstructural properties of the AI-WC bimodal composites, they
could be expected to have superior nrechanical properties than micro-
and nano-composites.
3.6. FJfen of SI\ duratiott and prcssure
There are plenty ofresearrh works available on optimizing the SPS
parameters for densification af metals, ailoys, and ceramics. However,
the liteiature is insufficient on how the SPS process variables affect
fhe microsil Ltcture, porosity, and rirechanical properties of the MMCs
reinfo[ced wit]r micro- and nano-pafticles. So far the general suggestion
is that the most inf'luential SPS paran-reter on the nricrostructural fea-
tures of the MMCs is ihe sintering temperature. However, the effect of
other SPS parameters seenls to be particularly case dependant
[{rB -71 ]. In previous secrions, the effects of SPS temperature (as well
as reinforcement particle size ancl concentration) an the n-ricrostructure
of Al-WC composites were thoroughly discussed. In this section, atten,
rion will be given on how the SPS pressure and duration could affect the
AI-WC corlposites" Fig. 10(a) shows the SEM micrcgraph of an Al-
i0 wt.TaWC bintodal romposite held fbr 10 min at500'C (twice longer
rhan the SPS duration of the specin.rens in Fig. B).There was not a big dif-
ference in agglornelatiorr elin-rination oi porosity level of these samples
as compared to those sintered for 5 min at 500 "C (the relative clensities
in both cases were -96?{). This suggests that the thermally activated
500 "c,50 MPa, 10 min
ljig" 10. Effefi oflil the SPS dur.rtion artd (b) the 5l'5 pressure on the n]icrostructurc
diffusion/flow mechanisnrs during the hot pacl<ing stage (SPS stage lll)
were conrpleted in a short period oi tinre (<5 min); thus, further
irnprovenrent could not be achieved by keeping the conrposite speci-
mens at 500 'C for longer periods^
The microstructure of the i-:omposites was neither influenced greatly
S[)S prbssure did nor have an
lic n-ratrix. There was only a slight inclease in the relative density of the
specimens (^96.3%), which should be relateci to better elimination of
interlacial microvoids under the higher compressive stress levels. But,
the ceramic agglorneration-related porosity could not have been affect*
ed rnuch by increasing the SPS pressure. In short, it can be confirmed
that, unlike the SPS tenrpelature, the SPS duration and pressuie dicl
not have a considerable effect on tlie microsfucture of the AI-WC com-
posites in the present work.
mirG, nano, and
3.7. H ardne ss me asllre men ts
The effect of sintering temperature and WC parficle size on the buli<
hardness ofthe conrposites is shown in Fig. 1 1. ltwa$ noticed thatthe
sintering tenrperature influenced the hardness of the microcomposites
in dissimilar ways (Fig. 1i(a)). In order to interpret the hardness data,
the microstructural differelrces in the specimens need to i:e highlighred;
that is, with increasing the sirrtering temperature: (1) pcrosiiy levels
decreased in all microconrposites, but at diflerent rates; (2) distribution
of the microparricles in the ntatrix was riot influenced significantly; and
(3) grain growth rate in the Al matrix could be accelerated.
fig. 11(a) indicates that in the most dilute microconrposire i1 wt.%
WC) the hardness did not change considerably with SPS temperature,
because the hardening effect gained by porosity elin-rination was com-
pensated by the softening effect driven by grain growth. However in
higher concenli-ation microcomposites (5 and 10 wt.7; WC), hardness
values increased with SPS temperature. It is because the relative density
nf those sanrples escalated more shar"ply with SpS temperature
(Fig. 3(a)). Thus, the associated gains in hardness Brere more than the
simultaneous losses attributed to grain growih. As a net resuit, arr
ascending trend in hardness versus SPS temperature was observecl.
Fig^ 1 1 ( b) shows the variation ofhardness with parricle size and con-
centration. In nanoccmposite specimens, hardness initially increased
with WC concentration r"rp to 5 wt.?{ due to the positive effect of disper-
.10
sion strengthening. But afterwarcls, hardness decreased in wt.%
nanocomposites due tit the negative effect ol an abrupt decrease in rel-
ative density caused by nanoparticle agglomerations (Fig^ 9). fn
microcomposite specimens on the other hand Ihere was a regular
trend of hardness increase with WC coucentrarion; because, in fhis
case the densification level was affected less severely with particle con-
cenlration (fiS. 9). Thus the iower porosity content of the
microcomposites allowecl a continuous ilrcrease of the hardness with
particle concentration. In a similar trend, hardness of the bimodal
500 oc, 100 MPa, 5 min
oiAl-l0 wt.%WC hiinodal composites as revealed bySE[,l nricrographs
232 A, Pakdel et al.
il, --** Ai-1 Yvt.o,ri
+At"5w1.%
, --r-,At-10 wt.% wc
:I75
----/ --"-lil
u d.-
I T
n tu
,n
o |/-
*-----'' -" .- *-
-"
*os
t6o
Micro-cornposite
with l0 wI.% WC.
composites was also amplified with increasing rhe wt.Z; of the WC
micro- and nano-parlicles.
In addition, these measurenlents demonstrated that all the nano-
composites and l:imodal cornposites reinforced r,vith difterent cerarnic
contents were harder than their corresponding microcomposites.
Fig. 11ic)*(e) depicts a conrparison befween very low magnificatiori
SEM images of these three types of composites. A clear difference in
the distribution ofthe nanoparlicles along the AI grain boundaries and
the agglomeration and cluster fonnation of the micropafiicles in the ma-
trix can be noticed. Although nanoccmposires had higher porosiry levels,
their better distribution in the marrix (i.e. borh intergranularly along the
grain boundaries and intragranularly through the grains) resulted in
higher harclness values. Agglomeration of microparticles and formation
of clusters reduces their efficient interaction with dislocation glide;
thus, plastic deforrnation ofthe matrix cannot be hindered effectively.
The bettei distributed nanoparticles, on the otlier hand. pin the dis-
locations, impecle their movemerrt, and consequently render lesser
compressibility and superior harclness. Fig. 1 1 (c)-(e) indicates that in
case ofthe bimodal composite, both clustering and intergranular disrri-
bution of the micro- and nano-particles coexisted.'Ihat is why the hard-
ness values of the 1 and 5 wt.){ WC bimodal composites were between
those of the micro- and nano-composites. However, the 10 wt.% WC
bimodal composite had the highest hardness among all the samples;
probably due to its higher density as compared to the corresponding
nanocomposite specimen.
4. Conclusion
Spark plasma sintering has recently gained n"ruch interest for the
fablication of nletal matrix composites. To have a realistic view of the
assets and liabilities of this rnethod, in this work Al matrix composites
reinforced with WC particles of various sizes and conceittrations were
prepared under different sintering conditiotis, and their nticrostructural
features were studied comprehensively.
WC parricle clirstering and inhomogeneity in particle distribution
increased with WC concentration in tiorh nano- and nricro-contposites.
However, the overall number of clusiers and their size were sntaller in
i Materials flntl Design 1 19 QA17) 225 234
wC {micro} {b}
WC (micro)
($rioro)
:E 7q
oIU
,h
{,
€uu
$
roo --.*- AI-WC {flano}
--**,Alwc (micfoJ
"-*- AI-WC (bimod€l)
10
Nano-romposite Bimodal-composite
the nanocomposites as colupared to the nticrocomposites. BuL the poros-
ity levels in 5 and 10 wt % nanocomposites were higher than those of the
microcomposites. When micro- ancl nanc-powders of WC were mixed to
fabricate birnodal conrpr:sites, a general imprcventent in particle distribu-
tiorr and interfacial features between Al and WC were obtained {no clear'
microyoids or microcracks) as compared to micro- and nano-composites.
Increasing the sintering temperature slightly improved the WC
particle distribution in the miclostlucture and also resultecl in
Iower porosity levels. However, enhancing the compaction pressure
and sintering duration did not have a large effect on the microstruc-
ture of the conrposites.
Rockwell H hardness measurements showed rhar the hardness
of 5 and 10 wt.% microcomposites increasecl witli sintering femper-
ature, while the hardness of the 1 wt.% specimens did not change
considerably. Moreover, the hardness of binrodal and nanocom-
posites was superior to that of microcomposites in all WC concen-
trations. In bimodal and microcomposites, there was a regular
trend of hardness increase with WC concentration, bur the h.rrd-
ness of the nanocomposite specimens initially increased with WC
concentration up to 5 wt.% and then decreased due to the negative
r,ffects of nanopart;cle clusrering.
Acknowledgement
'Ihis collahorative research was performed in fhe National Institute
for Materials Science (NIMS; Tsukuba,Japan), Insriiure of Fundamental
Technological Research of Polish Academy of Sciences (Warsaw,
Poland), and Universiti Malaysia Pahang (Pekan. Malaysia). The authors
acknowledge the financial support of the lnternational Cer-rter forYoung
Scienrists (ICYS; Tsr"rkuba,Japan) ancl theJapan Society for the Prorno*
tion of Science (JSPS; Tokyo, Japan).
Appendix A. Supplementary data
Supplementary data to this article can be found online at hfrp:/ldx.
doi.orgll 0. 1 * 1 6/j.nratdes.2fi 'l 7.01 .064.
 A" Pakdel et {il. i h4aterials and Design
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f47l W. Ztrang. My.Qt:,D7.V.iat1X. ZK. Y;o, rciling.Itii iunealing textures oi a SiC\,V/A1
r{Ilposire, Ivlarer. Lrrt. 56 i2004) 3414-3418.
i48l A. Pakalel" l-{. i:arhangi, M. llirrarrlr. Iifect rif gxtmsici: process $i] t]u*illi]r anc!
F:r:lLiure EellavioI oi SiCPr,,A.luminunl Allov fonlprs;te!. pro.rfdings si gtll
lrrtrrr::iilnai frncrrre CLlltiffen.e, Yil{liz'Iechniral tJni,/*rsiry, lsaJnbul. l-urkey,
t0 '".
L49j !i. Viswandtban, T. khn, I(. Bai:fli. A. Agalrjl, j. Seal. t hallenges anii ,ldvinces iil
nau0composite pmcessir:g techr:iques. I\4;1rer. S.i. Eng. il 54 (Z00ij) 111,295.
[50] Ii. lanaka, N. iyi, {,.riytypes, grJin-grDwtlt,,nd frnc{ut-tougltnrss r}fnreral boriCt
l-,,1: tifillate 5if (omposites, J. ,{nr. feram. 5o.. 78 i.19tj: 1)21.. 12'i9.
l5ll l'",1.a;upfJ,'l'.5.5rivdtiJB,i\,{ifilstrtcture.:ndgniugrorlthi;;}:*viorofanalurriitu0t
alloSi mrtnl DJtri: ronposire prs#ssed ltv dirintetrated lrflit depr-)sition, I. N{nfer.
llriS. Feilbrnr. I (19931
'i13..478.
l52l C.Q.Xie,0.Ohaslri,M.H.5ong.k.Ftruyr,'l.trtorla,B:lravlornioxiilefilrtrttltrir?
'Lci1;rs lletweeit p.l-licles in siirtered.rl powders hv pulse riectric a[nent sitlicrjl]g.
tu1rtail. &,lnllr."trians. A 14 {:00]) rjg8--?01.
I53l C.Q. Xie, O. Ol:asl:i, N. \'dmaguchi. &,i.C. -tlng, I(. M'{$u;rhi t(. Furuya, t'. Nodi,
l}i:avior oi axide fi lnt ai i rterta(e betlveru p"lrticles oi Al Mg d llfly p*tvrlrr cont."
parts prc;:;red bli pulsf tjrrtrir (nrrsrit sinrering,Jpn.J. Appl. piry5.42 iZflfjj)
4725- 4.1 ;8.
[54] N. Chenn*ufi, C. Majkic, Y.C. Ciietl, Ii.srlitri,'fcntperrrlllr,.unent. i*d he.tt loss
{listribuli.}ns ir reduced electrother!ual lo,cs:paric pltsnr: sirter!ng. \,ietali. &,,idL-i.
'll?ns. A 40 r20091 240 I
-2409.
[55] K. llash, n. ChJir;, llf. flav, lyrithesis Jnd cha.n(trri2:irion 0falun:injuln-rlumiira
rritr* ar:d naur-r*i:rpcsites bt, spark plasnra sintering, Maaer. Res. fJull. 4g
i2Ai3t 25'35 2542.
[56] .].T. Zl)an8, H.i.5'ri, i\.1,(, Cai, L.i. Liu, P.C. Zhri, ihe dyrldrri( lrr8perries ol Sjft]iAl
.ompositcs labricrted hv sparl< plasi:ra sintering h.ith pr:rrders preparerl by ire,
rhanical alloying process, MaI, sci. t:ng. A-Srrucr. 52? i2\.j?9) 215-)24.
[57] R.Orru,li.Li{hed,A.tul.Lorci,A.Cinrotti,{.C.Cas,Crnsolida{ionrs}ittiresisoinlar*-
ri:ls L:I,electric cdrreirt d.tiyifed./nssiste(l sioteri:1g, fu1;ter. S[i. tin.]. [ 6l (Zf.ii]g)
121 2:d,1 .
[58] A.5. tiuiiov, A.tr.6u5rv, Eff'ect Blparticl€ _cizr ol] the {lxidition r:fwc pou,,ders during
heatir:g, Inor^g. Nlatet, 47 (2\)t i\j 1 38. t]3
[59] A.E. Ncwkirk, lhe oxidalisn oL tllugsrer cz.hide, l. Am. aeranl, ,S,rr. 7? i1355)
4571.,,4522.
160] lU. lrlkira, Developrrent of largr-sizr tefnmicr,mr{,ll bulk igrl iabrir;ted by spark
plasma sii:tering, [,1ater.Sci. {roru$ 308-]!j f1!J99) Bl-.86.
i6 l I J.ll. Crrzr, ir.1. 6;r.;a, J.A. 5chi:eider. SrL.fr.e eiilcts in fiekl-.issisted s!naerlng, J.
Mater. lles. li:; i2$11) 28ij-)92,
[62] i].&4.{-iillbflt.A.As{lers".J.Anderssrn,[J.t.,lve!nia,A.]<.Mukhrtjee,Adiscnssion
on the nbsence o{ pid$nla in spnrl( piJsn}a sinteii.Jg. S(r. i!4jt.r. 60 (2t09 I 835- [i]9.
[63] XY.5orrg.X,M.l-iu,J.X.Zhailg,l\r(l{fomtarionnrxlreil:*djusringi:recharrirnroinetk
g.olvtlr ol.(orducting p$wdei s in sp.trk plJsma risteriitg, j. Aiil. CrraJ:r. Sor. 6g
i:a\b') 494-5aa.
[64] 5. Diour, A. Mslinni, Dri]sifi(atisll n:eciranisrr-c ir spirk plasma sinteriltg: efle.a oi
parLicls -{ize nlrd ptrsrure. i)owdri itch*Dl_221 i20l?.\ 22A-)-)}
l65l l. Srklhar, N.A. {.'ie(k. Yieid bfl},t"iour of.old cermpalted conlpitite powders, Arti
h,later. 48 (20001 314, ..3?52.
234 A. Pakdel $ aL i MoiericJs flnd Design 1 t9 (201?) 225--234

I66l C.A. Leon, C. }iod:iguez,Or-tiz, E.A. Aguilar-Reyes. foid rortpa(.iolt riiICtJl reranjir i?0] R.5ulr, PA. Ol[irrmbi. i,sigalas.J{iO. Asante,J{. Garrctt, efieri oi sps consolid.rtitu
ilowders in thr prepamti$n of copper base hybri.l ilatrriJls, N.lna. 5ri. Eil{. A-5iru.t. parinetei6 *n,cubmi;r*r Cu .:iltd au-CN]'conrposiles ior therm:1 r:ra0agenrent,
526 (t80!l rOft i 12. !}r:uder Tecl:i:ni. 258 i2C141 1 98-205.
I67l *. Sttrirj:r. ,,1-. La.sson,.olal coarpactioii cfromposite pawdrrs wiih sjzc rntio,.lct; U1l l,V.Y. \'aog, Z.K. Fnn. l.].T. Wang, Z.P. Xie, H.Z. l".1Lro. LN. An, fritrictrtiolt of Si:N.il,SiC
i\'latei, 5: i2804j 1 ti? i..1884. i:;nocoinposites b'!i ,pdfk fjlasrna sinleriilg of antorpllous sicn pslvders deriveil
l68l 5. Pns*hJsi. A.1{. llutr..J. 8urtrs, l. ChJrir, lt.S. Nlishra, Oride riispersisu stre$glhs8ed liorn a poiynreric prerurror.J, Ceranr. Process. Res.7 (200ajj :07 310.
nickr! i:ased ailoys via sDa.k plarnta sintrrisg, Mat.Sci. gng. A,Stllct.610 (2015)
155,i{i9.
l6el l.sulirila, f,. Putyrr, P, Hyiei(.-l-. Tokaisl<i, fliiecr oisps paran]eterr li: drnsifiraiio0
and piopcrties oI steel uatrir rcmpositcs, Adr. lbw.der 1*chrol. 26 i:,01-rl
1152.1161.