jnanor.21.29age hardening behavior of carbon nanotube reinforced aluminum nanocomposites
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8/13/2019 JNanoR.21.29Age Hardening Behavior of Carbon Nanotube Reinforced Aluminum Nanocomposites
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Age Hardening Behavior of Carbon Nanotube Reinforced AluminumNanocomposites
N. Saheb1,2,a, A. Khalil1,b, A.S. Hakeem2,c, T. Laoui1,2,d, N. Al-Aqeeli1,2,e, A.M. Al-Qutub1,f
1Dea!tme"t of Mecha"ical #"$i"ee!i"$
2%e"te! of #&celle"ce i" Na"otech"olo$'
Ki"$ (ahd )"i*e!+it' of et!oleum a"d Mi"e!al+, Dhah!a"-121, Saudi A!abia
a"oua!i/kfum.edu.+a, babdulkhaa/kfum.edu.+a 0co!!e+o"di"$ autho!,ca+hakeem/kfum.edu.+a, dtlaoui/kfum.edu.+a, e"aqeeli/kfum.edu.+a,
f aqutub/kfum.edu.+a
Keywords: Alumi"um "a"ocomo+ite, %a!bo" "a"otube+, A$e ha!de"i"$, Diffu+io"
Abstract. In the present work, age hardening behavior of CNT reinforced Al6061 and Al2124
nanocoposites, prepared b! ball illing and spark plasa sintering, was investigated" The effect
of CNT content, annealing tie and teperat#re on the age hardening behavior of the
nanocoposites was eval#ated and copared to the onolithic allo!s prepared and age hardened
#nder the sae conditions" It was fo#nd that CNTs have a negative infl#ence on the age hardening
of the allo!s" The allo!s displa!ed standard age hardening behavior i"e" a sharp increase in hardness
d#ring initial aging followed b! a stead! decrease in hardness" $hereas the nanocoposites did not
onl! displa! initial softening d#ring aging b#t also showed red#ced age hardening efficienc!" The
hardening efficienc! was fo#nd to decrease with increasing CNT content" The coplicated behaviorof nanocoposites was e%plained in ters of dislocation recover!, large theral isatch between
atri% and CNTs and b#lk icrostr#ct#re of the coposites"
Introduction
Age hardenable al#in# allo!s find iportant applications in a#toobile and aerospace
ind#stries" Age hardening &also called 'precipitation hardening( of soe al#in# allo!s belonging
to )***, 6*** and 2*** series, res#lts in the precipitation of etastable phases &depending
#pon allo! coposition( which offer resistance to dislocation oveent and hence strengthen the
allo!" The details of icrostr#ct#ral changes and strengthening echaniss which occ#r in these
allo!s d#ring age hardening are well doc#ented +1-."Al#in# etal atri% coposites &Al//Cs( have been proved as a proising sol#tion for
vario#s engineering applications where the light weight of al#in# allo!s is re#ired with
increased strength" The reinforceent phase which a! be in the for of particles, whiskers or
fibers and is #s#all! ceraic in nat#re, act as a barrier to dislocation otion and hence iparts
s#perior echanical properties to the atri%" t#dies have been e%tended to e%aine the age
hardening behavior of Al//Cs to take the d#al advantage of the e%ternal reinforceent phase as
well as the internal phases which a! be developed b! an appropriate heat treatent" atnaparkhi
et al" +4. showed that hardness of Al2124 allo! reinforced with 3 ol"5 iC whiskers can be
increased b! 10 7 thro#gh age hardening" 8an et al" +3. have deonstrated that significant
iproveent in wear resistance of Al2124 allo!, containing iC particles, is possible in the over
aged condition" Appendino et al" +6. reported an increase in hardness fro 900 7 to ore than1400 7 in Al6061 allo! containing iC particles" Increase in hardness b! alost 100 for
Al2024 allo! containing 20 ol"5 iC particles thro#gh age hardening was shown b! Abargho#ie
et al" +)." alvo et al" +:10. reported siilar res#lts for Al6061 allo! reinforced with iC and
Journal of Nano Research Vol. 21 (2013) pp 29-35© (2013) Trans Tech Publications, Switzerland doi:10.4028/www.scientific.net/JNanoR.21.29
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al#ina particles" ong et al" +11. also showed that wear resistance of Al6061 and Al2014 allo!s
containing iC particles can be considerabl! enhanced thro#gh age hardening" It has also been
reported +12,1-. that the age hardening efficienc! of h!brid coposite of Al allo! containing iC in
both partic#late as well as whisker for is #ch higher as copared to a onolithic allo! and the
allo! containing a single t!pe of reinforceent" Age hardening of Al allo!s is also accelerated b!
the presence of ceraic fibers as reported elsewhere +14." The concept behind accelerated agehardening of Al//Cs is the increased dislocation densit! developed d#ring sol#tion treatent d#e
to isatch between the coefficient of theral e%pansion &CT;( of the soft atri% and the hard
reinforceent phase" This increased dislocation densit! prootes the n#cleation of strengthening
precipitates and th#s accelerates the aging of the coposite +13,16."
Carbon nanot#bes &CNTs( have been one of the candidate aterials to ipart high strengthlow
weight characteristics to al#in# allo!s" /an! papers have been p#blished on the effect of CNTs
on vario#s ph!sical and echanical properties of al#in# allo!s" owever, the literat#re
regarding the age hardening behavior of AlCNT nanocoposites is scarce and onl! recentl! the
age hardening behavior of Al2024 allo! containing CNTs was investigated b! Choi et al" +1). who
fo#nd that age hardening efficienc! is increased with increasing CNT content" It was proposed that
CNTs act as a pathwa! for diff#sion of copper atos which sti#lates the foration of precipitatesnearb! to CNTs" It was also proposed that the high dislocation densit! at the tips of CNTs a!
sti#late the precipitation kinetics" ence, these nanoscale precipitates a! for coherent or sei
coherent interface str#ct#res with the atri%, res#lting in significant increase of hardness"
The ai of this work is to investigate the age hardening behavior of CNT reinforced Al6061 and
Al2124 nanocoposites prepared tho#gh ball illing and spark plasa sintering"
Materials and Methods
The Al6061 and Al2124 preallo!ed powders #sed in this st#d! were s#pplied b! the Al#ini#
8owder Co" <td", =>" CNTs having an average diaeter of 24 n and a length of few icrons
were #sed as reinforceent" Al2124 and Al6061 nanocoposite powders containing 0"3 and 1 wt"5 CNTs were prepared b! sonication followed b! wet ball illing" /ore details on the cheical
coposition of the powders and preparation of coposites can be fo#nd elsewhere +1:." A f#ll!
a#toated &?CT s!ste, @eran!( spark plasa sintering e#ipent odel 8 3 was #sed to
sinter the saples +19." canning electron icroscope &;/( was #sed to characteriBe the
icrostr#ct#re of sintered speciens" ?or st#d!ing the age hardening behavior, sintered saples
were sol#tion heat treated at 320 0C for 10 ho#rs in a f#rnace #nder an inert environent and
iediatel! water #enched at roo teperat#re followed b! annealing at 1600C and 2000C for ,
1, -, 6 and 10 ho#rs" A 7#ehler //T- digital icrohardness tester was #sed for eas#ring the
hardness of the speciens with an applied load of 100 gf and indenter dwell tie of 12 sec" The
eas#reents were taken at 10 different locations on the specien and the arithetic ean of these
10 readings was reported with a standard deviation"
Results and Discussion
?ig#re 1 shows ;/ icrographs of sintered speciens" 8orosit! is evident in the coposites,
however, the onolithic allo!s do not reveal an! porosit!, this is in agreeent with the densit!
res#lts reported elsewhere +1:, 19." ?ig#re 2 &a( and &b( shows the age hardening behavior of
Al6061 onolithic allo! and Al6061DCNT coposites at an annealing teperat#re of 1600C and
2000C, respectivel!" At 1600C, the onolithic allo! reached its peak hardness after annealing for 1
ho#r whereas peak hardness was achieved within ho#r at 2000C" This is e%pected beca#se a
higher teperat#re will accelerate the diff#sion of atos res#lting in earlier foration of coherent
precipitates which are ainl! responsible for strengthening the aterial" ?or the coposites, it can be seen that CNTs do not onl! retard the age hardening rate b#t also red#ce the age hardening
efficienc! of the allo!" At lower annealing teperat#re, the coposites reached their peak hardness
in 6 ho#rs whereas at higher annealing teperat#re, peak hardness was achieved after - ho#rs"
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/oreover, it can be seen that for all aging ties, the hardness reained lower for the coposites as
copared to onolithic allo! and the coposite containing 1 wt"5 CNTs displa!ed a lower
hardness as copared to the coposite containing 0"3 wt"5 CNTs" A siilar trend was displa!ed
b! onolithic Al2124 and Al2124DCNT coposites as evident fro ?ig#re -"
Fig 1 ;/ icrographs of 8Eed Al6061 containing &a( 0 &b( 0"3 &c( 1 wt"5 CNTs and 8Eed
Al2124 containing &d( 0 &e( 0"3 &f( 1 wt"5 CNTs
An iportant observation in case of coposites is the decrease in hardness d#ring initial aging
stage" As can be seen in ?ig#res 2 and -, the coposites displa!ed decreased hardness d#ring the
first ho#r of aging" This shows that soe softening echanis occ#rred in coposites d#ring initial
aging" An e%actl! siilar trend has been reported b! <in et al" +1-. who st#died age hardening of
Al2024 allo! reinforced with iC nanoparticles" The average siBe of reinforceent particles was -3
n" This decreasing trend of hardness d#ring initial stage was attrib#ted to the dislocation recover!,
which is ore predoinant in the initial stage #ntil which the F phase has not fored" As the aging
tie increases, F phase fors at a higher rate beca#se of the presence of a high dislocation densit!,
which are considered favorable sites for F phase n#clei foration, which is responsible for peak
hardening of the allo! +20." Altho#gh the F phase foration is ore specificall! related to C# based Al allo!s, the CNT containing Al6061 allo! displa!ed a siilar trend" The aging kinetics in
the presence of nanosiBed reinforceents is th#s cople% and ore research is needed to f#ll!
concept#aliBe this aspect" Another iportant finding is that the presence of CNTs res#lts in red#ced
age hardening efficienc! as well as retardation of the age hardening rate in Al allo!s" It has been
proposed +21,22. that the densit! of #enchedin vacancies is saller in the coposite owing to the
greater densit! of sinks &dislocations, atri%reinforceents interfaces( and since vacancies are
needed to n#cleate @8 Bones, the precipitation kinetics in the coposite is slowed down" It is well
known that Al allo!s containing /g and i are sensitive to age hardening owing to the possible
foration of /g2i precipitates" The coplete ageing se#ence in the allo! s!ste isG
s#persat#rated solid sol#tion H @8 Bones or partiall! coherent J needles H partiall! coherent F rods
H incoherent &/g2i( discs" The last two stages correspond to over aged conditions +9." In the presence of CNTs, the foration of @8 Bones or J phase a! be s#ppressed as CNTs a! act as
an ip#rit!, inhibiting the reaction between /g and i" In a siilar wa!, the foration of F phase
a! be inhibited in Al2124DCNT coposites" The coposites displa!ed a%i# age
a
d
cb
ef
1 !m
1 m
1 m
1 m
1 m
1 m
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hardenabilit! for the aging ties of - and 6 ho#rs at the annealing teperat#res of 200 and 160 0C,
respectivel!" This increase in hardness is d#e to the contrib#tion of phases precipitated inside the
atri% onl! and apparentl! there is no contrib#tion of CNTs" The decrease in hardness of
coposites after achieving a%i# hardness a! be attrib#ted to the coarsening of precipitates,
especiall! near the atri%CNT interfaces where the dislocation densit! is high" This will decrease
the coherence between the atri% and the precipitates res#lting in red#ced hardness +1)."It has been shown that CNTs displa! a negative coefficient of theral e%pansion &CT;( in the
teperat#re range of 30 to 600 > &22- to -2)0C( +2-." Also, the val#e of CT; for CNTs in this
teperat#re range was fo#nd to be of the order of 10 % 106 > 1 as copared to al#in# for
which CT; is D22 % 106 > 1" Altho#gh, the sol#tion treatent teperat#re #sed in the present
work i"e" 3200C is well be!ond this range, the annealing teperat#res i"e" 160 and 2000C lie within
this range" #ch large difference in CT; val#es co#ld be another iportant reason for the observed
trend" $hile annealing, the atri% particles #nderwent e%pansion whereas CNTs e%perienced
contraction" This will not onl! res#lt in decreased adhesion between the atri% and CNTs b#t will
also create icroscopic gaps between CNT cl#sters at a few locations and the atri% particles" The
#ltiate res#lt will be the degraded hardness of the coposite"
The res#lts of this work are contrar! to that obtained b! Choi et al" +1). where CNTs were fo#ndto have a positive ipact on the age hardening efficienc! of Al2024 allo!" Choi et al" #sed
nanocr!stalline atri% powder whose grain siBe was red#ced b! ball illing the powder for 24
ho#rs" It is known that the n#cleation and growth of precipitates a! progress #ch faster when
grain siBe is red#ced beca#se the fine str#ct#res ca#se enhanceent of aging kinetics +24." At the
sae tie, the grain bo#ndar! diff#sion will be higher in the case of saller grains d#e to an
increased densit! of grain bo#ndaries" Also, the nanocr!stalline atri% will posses a greater degree
of coherence with the CNTs d#e to coparative siBe" $hereas in the present work, as received
icron siBed atri% powders were #sed having a lesser degree of coherence with the CNTs d#e to
large difference of siBe" These aspects co#ld be the possible reasons for contrasting res#lts"
Altho#gh it has been proposed that addition of foreign particles iproves the age hardening rate
and efficienc! of the aterial d#e to increased dislocation densit! and conse#entl! increased
precipitation kinetics +414., this siplified stateent ight not be applicable to the aterials
containing nanoparticles s#ch as CNTs" It is a well established fact that aggloeration of CNTs
cannot be totall! avoided d#ring processing d#e to the high s#rface energ! of CNTs +23-1." This
aggloeration hinders proper densification of the atri% and hence the pores are developed inside
the aterial, as alread! shown in ?ig#re 1" These pores can be considered as acroscopic defects
inside the aterial which degrade the echanical properties of the aterial" These defects cannot
be copared with the point vacancies and atoic level dislocations which are considered as
precipitate accelerators d#ring age hardening" The pores or acroscopic defects, developed
priaril! d#e to CNT aggloeration, wo#ld rather decelerate the aging kinetics d#e to incoplete
diff#sion of atos which is andator! for aterial strengthening" Also, it is known that thestrengthening of aterial in the presence of second phase is governed b! the relationG
where τ is the !ield stress, K is the interparticle spacing, G is the shear energ! of dislocation and b
is the dislocationEs b#rger vector" igher porosit! in atri% eans an increased val#e of K, which
eans red#ced strength of the aterial" ence increased porosit! d#e to CNT aggloeration can
slow down the aging kinetics"
The res#lts of this work indicate that age hardening of Al nanocoposites is cople% and cannot
be e%plained p#rel! in the conte%t of conventional age hardening theories" Altho#gh process odels
have been developed +-2,--. which describe the aging phenoena in Al allo!s to a reasonablee%tent, the aging process in coposites and nanocoposites is far ore cople% and f#rther
research is needed to #nderstand and odel the age hardening response of Al etal atri%
coposites and especiall! the nanocoposites"
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Fig 2 ardness of Al6061 and Al6061DCNT coposites as a f#nction of aging tie at an annealingteperat#re of &a( 1600C and &b( 2000C
Fig 3 ardness of Al2124 and Al2124DCNT coposites as a f#nction of aging tie at an annealing
teperat#re of &a( 1600C and &b( 2000C
Conclusion
The present e%perientation reveals that carbon nanot#bes &CNTs( retard the age hardening kinetics
in Al6061 and Al2124 al#in# allo!s" The CNT reinforced nanocoposites showed softening
d#ring initial aging which was attrib#ted to dislocation recover! before the foration of coherent
precipitates which are responsible for strengthening the aterial" ?or higher aging d#rations, the
nanocoposites displa!ed age hardenabilit! d#e to the sole contrib#tion of the atri%" The hardness
of nanocoposites reained lower than that of the onolithic allo!s for all aging ties d#e to the
wide difference between the theral properties of CNTs and atri%, scarcit! of #enchedin
vacancies, and an increase in the interparticle spacing ca#sed b! CNT aggloeration"
Acknowledgement
The a#thors wo#ld like to acknowledge the financial s#pport for this work fro >ing Abd#l ABiB
Cit! for cience and Technolog! &>ACT( thro#gh research proLect n#ber A82:122"
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