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ObtencindecermicosabasedecaolnmedianteelprocesodeFreezecasting|GilDurn|RevistaIngenierayCompetitividad

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Inicio>Vol.18,Nm.2(2016)>GilDurn

KaolinbasedceramicsobtainedbyFreezecastingprocess
ObtencindecermicosabasedecaolnmedianteelprocesodeFreeze
casting
SantiagoGilDurn
GrupodeInvestigacinenMaterialesdeIngeniera,EscueladeIngeniera,UniversidadEAFIT.
Medelln,Colombia.
Email:sgildura@eafit.edu.co
E.A.Ossa
GrupodeInvestigacinenMaterialesdeIngeniera,EscueladeIngeniera,UniversidadEAFIT.
Medelln,Colombia.
Email:eossa@eafit.edu.co

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revista
ID IO M A
Escogeidioma
Espaol(Espaa)
Entregar

US UA R IO / A
Nombredeusuario/a
Contrasea

Recibido:Noviembre25de2015
Aceptado:Febrero12de2016
Ejetemtico:MATERIALSENGINEERING/INGENIERADEMATERIALES

Abstract
Freezecastingoffersatremendousopportunitytoobtainbioinspiredsyntheticmaterialsthat
mimicmicrostructuralcharacteristicsofnaturalmaterialslikeboneandnacre.Thesenatural
materialsdisplayhighstrengthandtoughnesspropertiesusuallydesiredinsynthetic
engineeringmaterials.Thefreezecastingprocessinvolvesfourbasicsteps.Theceramicslurry
preparationconsistsoffineceramicparticlesthataresuspendedinafluid.Inthecurrentwork,
waterbasedkaolinsuspensionswerepreparedvaryingthevolumefractionofceramicparticles.
Aftertheceramicslurryisproperlyprepared,theslurryisfrozen.Thesolidificationprocessis
oftenperformedusingdirectionalfreezing,whichcreateslaminarpores,providingthe
microstructuralcharacteristicsofthefinalpart.Whenacrystalisformedthefrozenfrontmoves
theparticlesaroundit,allowingparticlestoagglomeratearoundthecrystal,creatingdifferent
typesofpores.Inthepresentstudy,freezingrateswerevaried.Subsequently,thesamples
havetobelyophilizedinordertosublimatethefrozenliquidphase.Sublimationisthe
transformationofasolidphasedirectlytothegasphase.Asaresultthelyophilizedsamplehas
aporousstructurewithareplicaofthewatercrystalsformedduringfreezing.Asafinalstep,
sinteringofceramicsisperformed.Resultsofthemicrostructuralcharacteristicsofthesamples
revealedthatvaryingthevolumefractionofceramicparticlesandfreezingrateshaveadirect
influenceontheporecharacteristics,changingfromcirculartolaminarpores.
Keywords:Bioinspiredmaterials,freezecastingprocess,kaolin,microstructure.

Resumen
ElprocesodeFreezecastingofrecelaoportunidaddeobtenermaterialessintticosqueimitan
caractersticasmicroestructuralesdematerialesnaturalescomoelhuesoyelncar.Estos
materialessecaracterizanporpresentarunabuenacombinacinderesistenciaytenacidad
propiedadesdeseablesenmaterialessintticosdeingeniera.ElprocesodeFreezecasting
consisteencuatropasos.Primero,preparacindeunasuspensincoloidaldepartculas
cermicas,enestetrabajoseutilizaronsuspensionesabasedecaolnyaguacondiferentes
concentracionesdecaoln.Luegodepreparadaslassuspensiones,serealizunprocesode
congelamientodireccionalquebrindalascaractersticasmicroestructuralesdelapartefinal,
obteniendoporosalineadosdebidoalaformacindireccionaldeloscristalesdeaguaque
muevenlaspartculascermicasalrededordeellos,creandodistintastipologasdeporos.En
estetrabajosevarilavelocidaddeenfriamientodelproceso.Despusdecongeladala
suspensincoloidaldepartculascermicasserealizunprocesodeliofilizacinelcualcambia
lafaseslidadelagua,obtenidadelprocesodecongelamiento,agassinpasarporestado
lquido,permitiendoquelapartemantengalaformadeloscristalesdeagua.Finalmente,se
realizaelprocesodesinterizado.Resultadosdelanlisismicroestructuraldelasmuestras
obtenidasrevelaquelavariacindelaconcentracindepartculascermicasenlasuspensin
coloidalylavariacindelavelocidaddeenfriamientoenelprocesodesolidificacintieneun
efectoconsiderablesobrelamicroestructuraobtenida.Lasmicroestructurasvarandesdeporos
columnareshastaporosesfricos.

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Palabrasclave:Caoln,freezecasting,materialesbioinspirados,microestructura.

1.Introduction
Materialshavedifferentfunctionsinnature.Forinstance,boneisusedinstructuralapplications
whereasnacreisusedasaprotectivematerial.Bioinspiredmaterialsarematerialsthatmimic
oneormoreaspectsofnaturalmaterials(Meyersetal.,2013Chenetal.,2012Meyersetal.,
2008Launeyetal.,2009).Inordertoobtainbioinspired(syntheticmaterials),scientistshave
exploreddifferentmethodsofmanufacturing,byinvestigatingthescientificreportofMalsheet
al.(2013)itispossibletofindalargelistofotherprocessesaimedtomimicnaturalmaterials
features.

Contador
OPENJOURNALSYSTEMS

TA M A O D E FUE NT E

Freezecastingoffersatremendousopportunitytomimicsomenaturalmaterialswithsynthetic
materialsthatcouldleadtothedevelopmentofnovelstructuresforengineeringapplications.
Therehavebeeninitiativesusingfreezecastingtoproducebioinspiredmaterialsforbone
replacement(Devilleetal.,2006Yangetal.,2010Pawelecetal.,2014).Additionalstudieson
freezecastinghavebeendevotedtothemanufactureofpartsmimickingsomecharacteristicsof
nacrewithhighstrengthandtoughnessbyinfiltratingthestructureswithasecondface(Munch
etal.,2008Sinchuketal.,2013Liuetal.,2014Shagaetal.,2015).
Ingeneral,thefreezecastingprocessconsistsoffourbasicstepsillustratedinFigure1.i)The
slurrypreparationconsistsofanymaterialintheformofparticlessuspendedinafluid,usually
water,campheneandtertButylalcoholbased,eachofthemproducingdifferentporestructures,
leadingtodifferentcharacteristicsofthematerialproduced.ii)Solidification,theslurryis
frozen.Dependingonthesolventusedintheslurrypreparation,thecrystalsformedduring
freezingwillhavedifferentshapes.Thecrystalsareformedusingdirectionalfreezing,which
createslaminarpores(Deville.,2008).Watercanbeusedasasolventtoproducedendritic
shapedcrystals,resultinginellipticporeswithlengthsbetween30umand500um(Fukasawaet
al.,2002).iii)Sublimation,thesampleshavetobelyophilizedinordertosublimatethefrozen
liquidphase.Sublimationisthetransformationofasolidphasedirectlytothegasphase.Asa
resultthelyophilizedsamplehasaporousstructurewithareplicaofthecrystal'sshapeformed
duringfreezing.iv)Finally,sinteringisperformedinafurnace.
Figure1.Thefreezecastingprocessconsistsoffourbasicsteps.1.Ceramicslurrypreparation
2.Freezingtheceramicsolventsystem.3.Sublimationofthefrozensolvent.4.Sintering.

Applicationsofmaterialobtainedbyfreezecastingmayincludeceramicsforgascleaning
(Kitaokaetal.,2004),catalystssupports(PhamHuuetal.,1999),drugdeliverysystems
(Szepesetal.,2007),soundabsorbingceramicmaterials(Franketal.,2011),amongothers.A
recentreviewarticlebyHammeletal.,(2014)givesagoodsummaryofdifferentapplications
ofporousceramics.Theaimofthecurrentstudyistoevaluatetheeffectsofkaolinvolume
fractionandfreezingratesonthemicrostructureofthesinteredpartsobtainedbyfreeze
casting.

2.Materialsandmethods
Freezecastingrequiresasetofmaterialstopreparetheceramicslurry.Inthecurrentstudythe
aqueousmediumusedwasdistilledwaterasithasbeensuccessfullyusedinpreviousstudies
(Launeyetal.,2009Liu,2011).TheKaolin(Al2Si2O5(OH)4)employedwasobtainedfrom
ProtokimicaS.A.Swithaverageparticlesizeof17.886mandspecificsurfaceareaof0.569
m2/g(Mastersizer2000).TheslurrywasthenpreparedwithdifferentKaolincontent(10,30and
50%Weighted).Theproceduretopreparetheceramicslurryconsistedofweighing(Mettler
ToledoML204/1,d=0,1mg)thepreciseamountofdistilledwater,kaolin,andanorganic
defloculant(polyvinylalcohol,1,4wt%ofthekaolinpowder,341584ALDRICHPoly(vinyl
alcohol),Mw89,00098,000.Theorganicdefloculantwasaddedtorisethestabilityofthekaolin
suspensionviaadsorbedorganicmoleculesaroundtheparticlesurface(Chaiwong&Nuntiya.,
2008).Further,Poly(vinyl)alcoholworksasabinder,increasingthestrengthofthegreenpart
(Launeyetal.,2009).Afterweighting,thedistilledwaterandorganicbinderweremixedat700
RPMinamagneticstirrer/hotplate(CorningPC420D)at80oCfor12hourstodilutethe
Poly(vinylalcohol).Whenthisblendreachesroomtemperature(20C)theceramicpowderis
addedgraduallywhileitiskeptunderconstantmixing.Toensureagooddispersiontheslurry

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mustbemixedforabout24hours(Liu.,2011).ThekaolinslurrywasleftatitsinnerpH6.0
becauseitwasmorestableatsuchvalue(Chaiwong&Nuntiya.,2008).
Thefreezingapparatususedisdescribedby(Liu.,2011).Threedifferentfreezingrateswhere
usedtofreezetheslurry(e.g.:0,019(V1),0,025(V2)and0,081(V3)mm/sec)tostudyits
effectsonthefinalmicrostructure.Thekaolinslurrywaspouredintoaprecooledacrylicmould
of10mmindiameter,50mminlengthandthicknessof20mm.Afterfreezing,thepartwas
freezedriedfor12hourstoallowtheicetosublimate(Preissetal.,2012)(VirTisBenchTop4K,
16mTorrat80C).Sinteringwasthenperformedinaconvectivefurnace(NaberthermLT
15/13/P330)at1300Cforthreehours.Theporosityofthesampleswasassessedbyoptical
microscopyonreflectionmodetostudytheporemorphology(ZeissDiscovery.V8).Finally,the
bulkdensityofthesampleswasmeasuredusingparaffincoatingandtheArchimedes'method.

3.Resultsanddiscussion
ResultsshowedthatthesamplesdisplayedthreewelldefinedzonesasshowninFigure2,each
havingdifferentporemorphology.Thebottomofthesamplewhichisindirectcontactwiththe
cooledsurfaceshowsadensercellularstructurewithnovisiblemacroporosity.Thisisthe
resultoftheinitialsupercoolingeffectsofpouringtheceramicslurryoveracoldsurface,
leadingtoanotsteadyfreezing(Waschkiesetal.,2011).Justabovesuchzone,thereisa
transitionwherethealignedporesbegintogetformedwhichisproducedbytheinstabilityof
thewatercrystalswhilechangingfromcellulartolamellarstructures(Devilleetal.,2006).
Finally,towardsthetopofthesampleappearwelldefinedlamellarmacroporesthatgetwiderin
thedirectionoftheupperregion.Theporesarealignedtowardsthefreezingdirectionwitha
branchlikestructure.Lamellarmacroporesaretheconsequenceofslowerfreezingfrontatthe
topofthesampleresultinginahomogeneousicenucleation(Schoofetal.,2001).Thepore
gradientcharacteristicsreportedherehavealsobeendescribedbyseveralauthors(Moritz&
Richter.,2007Sofie.,2007Waschkiesetal.,2011).Aslamellarporesarethemostimportant
featureexpectedfromfreezecasting,thesubsequentanalysiswillbeconcentratedonthis
region.
Figure2.Distinctivesamplescharacteristics.Threetypicalzoneswithlengthdependenton
slurrysolidcontentandfreezingrates

Thelengthsofthethreemainregionsaredependentonthefreezingratesandsolidfraction
content.Toassessthesecharacteristics,thelengthofthelamellarmacropores(topofthe
sample)respecttothetotallengthofthesamplewasanalyzed,asshowninfigure3.In
general,slowfreezingratespromotetheformationoflamellarstructureswithinthesample,
resultinginlongerlamellarstructures.Asfreezingratesincrease,thelengthofthelamellar
structurestendstodecrease.Thelamellarstructureformsasaresultofparticlefrozenfront
interactions.Slowfreezingratesproduceaslowfrozenfront.Then,thecrystalsthatare
formingwhilethefreezingfrontisadvancingareabletomovetheparticlesaroundthem,
allowingtheformationoflamellarstructures.Ontheotherhand,highfreezingratesdonot
allowtheparticlestobemovedaroundthecrystal,finishingtrappedwithinthewatercrystals,
hencenotpermittingtheformationoflamellarpores(Rempel&Worster.,1999Rempel&
Worster.,2001).Therefore,selectingtheappropriatefreezingratehasadirecteffectonthe
formationoflamellarstructureswithinthesample.Particlesizeisanimportantfeaturetotake
intoaccountwhenanalyzingthemicrostructureobtained.Forinstance,Devilleetal.,(2009)
noticedthatusingsubmicronparticlessizeresultsintheformationofcracklikedefects
affectingthecompressivestrengthofthesamples.
Figure3.Lamellarzonelengthwithrespecttototalsamplelengthatdifferentfreezingratesand
solidfractions.Theerrorbarsindicatestandarddeviation

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Waschkiesetal.,(2011)studiedtheinfluenceofparticlesizeandfreezingratesonthe
microstructureusingdifferentaluminaparticlesizesinawaterbasedpolystyrenemedium.
Resultsshowthatwhentheparticlessizeisaround2mlamellarstructuresareobtainedina
widerrangeoffreezingrates(11000m/s).However,whenlargerparticles(15m)areused,
lamellarstructuresareonlyformedatfreezingratesbelow3m/s.Resultsfoundinthecurrent
studyarenotinagreementwiththosebyWaschkiesetal.,(2011).Here,theslowestfreezing
ratewas19m/susinganaverageparticlesizeof17,886m.Lamellarstructureswere
obtainedonlyaftercompletingtheprocess.AsmentionedbyDeville,(2010)oneofthemain
challengesofcomparingfreezecastingresultsisthattheporemorphologycanbevariedby
usingdifferentadditives.Forinstance,Zhangetal.,(2009)observedthattheporemorphology
andsizeissignificantlyaffectedbytheadditionofgelatintotheceramicslurry.Fuetal.,(2008)
addedglycerolwatermixturesandconcludedthattheglycerolproducesfinerpores.Thus,the
resultsobtainedheremightnotmatchwiththeonesbyWaschkiesetal.,(2011)becausethe
ceramicslurrywerepreparedusingdifferentbasematerial,mediumandadditives.
Solidfractionalsohasadirecteffectonthelengthofthelamellarstructure.Forinstance,
sampleswithhighsolidfractionstendtohavealongerlamellarzoneatslowfreezingrates,
whereasathighfreezingratestheyshowthetendencytohaveshorterlamellarzones.For
particlefluidmixturesthethermalpropertiesdependonparameterslikethermalconductivityof
thebasefluidandparticles,volumefractionandtemperatureofthesystem,amongothers
(Wang&Mujumdar.,2007).Thethermalconductivityofkaolinclay(0,3W/mK)(Etuketal.,
2003)islowerthanforwater(0,59W/mK).Asaresult,highersolidfractionsendupinalower
thermalconductivityoftheceramicslurry,whichslowsthefreezingfrontthroughthesample,
resultinginafasterhomogeneousicenucleationwhichcreateslongerlamellarstructures.
AccordingtoDevilleetal.,(2007)solidfractionshigherthan80wt%makethatthelamellar
structuregetlostandtheporesarenotinterconnected.
Figure4showstheporemorphologiesatdifferentfreezingratesandsolidfractions.Thefreeze
castingprocessishighlyreproducible,givingtheopportunitytocontrolstructureformationby
simplytuningthefreezingratesandsolidfractionsoftheslurry.At10%solidcontent(figures
3a,3band3c)thesinteredkaolinpartbarelyformscrystals.However,atslowfreezingratesit
wasfoundalamellarstructure.At10%solidcontentduringfreezedrying,approximately60%
ofthepouredsamplelengthcollapsedduetothelackofinteractionsbetweenparticles.The
remaining40%ofthesampleshowedthecharacteristicspreviouslydescribed.Devilleetal.,
(2007)alsopointedoutthatatlowceramiccontentthegreenbodybecomesweakerand
difficulttohandle.Nonetheless,itcanbeimprovedbyincreasingthebindercontent.Thelength
andsizeofthelamellarporesatslowfreezingratesat30%and50%solidfractionsare
noticeableincreasedasobservedinfigures3d,3e,3gand3h.At30%thelamellarporesare
welldefinedalongthesamplewitharemarkableporosity.Higherfreezingratescertainlydonot
promotetheformationofwelldefinedcrystalsatanysolidcontent(figures3c,3f,and3e).
Resultsofdensityofthelamellarzoneatdifferentfreezingratesandsolidfractionsareshown
infigure5.Overall,forhighersolidfractionsareobtainedhigherdensitiesofthelamellar
structureofthesamples,aswellasslowfreezingratesgivetimetotheparticlestosediment,
thusthedensityofthetopofthesampletendtobereducedexplainingthelamellarzone
characteristicsatdifferentfreezingratesandsolidcontents.
Figure4.Lamellarzonecharacteristicsatdifferentfreezingratesandsolidcontent.a.10%solid
contentat0,019mm/sec.b.10%solidcontentat0,025mm/sec.c.10%solidcontentat0,081
mm/sec.d.30%solidcontentat0,019mm/sec.e.30%solidcontentat0,025mm/sec.f.30%
solidcontentat0,081mm/sec.g.50%solidcontentat0,019mm/sec.h.50%solidcontentat
0,025mm/sec.i.50%solidcontentat0,081mm/sec.

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Figure5.Densityofthelamellarzoneatdifferentfreezingratesandsolidcontent.Theerror
barsindicatesthestandarddeviation.

4.Conclusions
Thefreezecastingprocessisahighlyreproducibleprocessgivingtheopportunitytocontrolthe
porousstructureformationbysimplytuningthefreezingratesandsolidfractionsoftheslurry.
Astudyofthemicrostructuralcharacteristicsofthesamplesrevealedthatvaryingthesolid
fractionofceramicparticlesandfreezingrateshaveadirectinfluenceonporemorphology.
Ingeneral,slowfreezingratespromotetheformationoflamellarstructuresatthesolid
fractionsevaluated(10%,30%and50%).Nonetheless,thesamplesshowedalowerdensity
duetothesedimentationtimegiventotheparticlesduringthefreezingprocess.Thebest
definedandlongerlamellarporeswereobtainedat30%solidcontentatslowfreezingrates.
Whenthesolidfractionisincreasedto50%therearestilllamellarstructuresbutthesamples
showedahigherdensityandthelamellarporeswerenotwelldefined.At10%solidfractionthe
samplespresentedseveralproblemsduringfreezedryingduetothelackofparticle
interactions,asaconsequencetheinitialpouredsamplelengthwasreducedabout60%after
thefreezedryingprocess.Thus,solidcontentsaslowas10%arenotrecommendedinfreeze
castingprocessesunlesssuchcharacteristicsaredesired.Finally,higherfreezingratescertainly
donotpromotetheformationofwelldefinedlongercrystalsatanyofthesolidcontents
evaluatedandthesamplesshowedhigherdensity.

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