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Developmentofa3DPrintingMethodforProductionofDentalApplication

LiYanga,ShanshanZhanga,GustavoOliveirab,BrentStuckera
a
DepartmentofIndustrialEngineering,J.B.SpeedSchoolofEngineering
b
DepartmentofGeneralDentistryandOralMedicine,SchoolofDentistry
UniversityofLouisville,KY,40292
Abstract
Traditionally,themanufacturingofdentalrestorations,includingcrowns,veneersand
otherstructuresmadebyceramics,isalaborintensiveandtimeconsumingprocess.
Additivemanufacturinghasthepotentialtosignificantlydecreasethetimeandcost
associatedwiththisprocess.Thisworkperformedpreliminaryinvestigationforthe
feasibilityofdentalrestorationpartsprintingusingtheExOneMLabsystemwitha
commercializeddentalporcelainpowder.Theporcelainpowderswerecharacterized,
andtwomeasurements,includingpresinteringandadditionofflowagent,weretaken
intheattempttoimprovetheprocessabilityoftheoriginalpowderfeedstock.The
resultsshowedthatwhiletheadditionofflowagenthasmoresignificanteffectsin
improvingtheflowabilityofthepowderused,thepostsinteredpartsexhibit
considerableshrinkageandresidualporositythatnecessitatesfurtherinvestigation.

Introduction
Overthepastdecades,therehasbeenatrendofusingmetalfreerestorationsinthe
dentalfield(DenryandHolloway,2010,Guessetal.,2011).Ceramicdentalrestorations
havebeenincreasinglyusedduetotheiroutstandingaestheticfeaturesandresistivity
tochemicals(Conradetal.,2007,Kelly,1999).Traditionally,thedentalceramicswere
producedbyhotpressing,sinteringorslipcastingprocesses(DenryandHolloway,2010),
whichingenerallacksufficientflexibilityintheaccuratecustomizationoftheparts.
Machiningwasusedaswell,butoftensuffersfromthehighhardnessandlow
toughnessoftheceramicfeedstock.Inrecentyears,aCAD/CAMbasedmethodwas
developedtoproducedentalrestorationswithgeometriesaccuratelymatchingthatof
thepatients(Filseretal.,2003,Guessetal.,2011).Thebasicproceduresofthisprocess
involvesthepresinteringofceramicblocksfollowedbyaCNCmachiningprocessthat
producesaccurateshapes,thenthegreenmachinedpartsaresubjecttoadensification
sinteringprocesstogeneratethefinaldensitiesaswellasmechanicalperformance.The
useofthetwostagesinteringhelpsreducetheissuesassociatedwithmachiningofhard
ceramics,thereforeincreasingtheefficiencyoftheprocesswithlowercost.However,
duetotheshrinkageinthesecondsinteringstage,theaccuracyofthemachiningcould
besignificantlyreduced,whichcompromisesthebenefitintendedtobeprovidedvia
machining.Inaddition,therelativelycomplicatedproceduresalsoresultinlonger
manufacturingtimeandhighercost.

WiththeabilityofmanufacturingpartsdirectlyfromaCADmodelwithadequate
accuracyandminimalwaste,additivemanufacturingholdsgreatpotentialforthefuture
productionofcustomdentalrestorationparts.Severallasersinteringbasedstudies
havebeenpresentedintheattempttofabricatedentalrestorationswithvarious
materials(Lietal.,2000,Hagedornetal.,2011).Theuseofalaserforthedirect

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sinteringofceramicsenablesonestepprocessingforthemanufacturingoftheseparts,
andprovidesthepotentialfordirectmanufacturingofceramicovermetaldentalparts.
Ontheflipside,thermalcrackingisacommonissuefortheseprocesses(Wilkes,2010),
andthefeatureresolutionisalsooftenlimitedduetothepartialsinteringofthe
surroundingceramicpowders(Hagedornetal.,2011).Recently,adirectwritebased
printingprocesswasinvestigatedforthefabricationofzirconiadentalprostheses(Ebert
etal.,2009).Theprocessselectivelydepositsazirconiabasedsuspensionongraphite
substrates,followedbyapostsinteringprocesstoachievethefinaldensity.The
resultingpartsexhibithighgeometricalaccuracyanddensity,aswellasgood
mechanicalstrength.Inthisworkitwasalsoreportedthepotentialissuewiththenozzle
clogging(Ebertetal.,2009).
Inthisstudy,theExOneMLabwasusedinanattempttofabricateceramicpartsfrom
offtheshelfcommercialceramicpowdersusedfordentalapplications.Whilethe
systemisrelativelynew,therehavebeenstudiesthatutilizebinderjettingtomake
ceramicparts(Cimaetal.,1995,Uhlandetal.,1999).Thisprocessofferssomepotential
advantagesinceramicprinting,suchastheflexibilitywithdifferentceramicmaterials,
therelativelyhighfeatureresolution,andeasyprocesscontrol;thereforebinderjetting
wasadoptedforthisstudywithfuturedevelopmentsinmind.Thegoalofthisstudyisto
identifythefeasibilityofthesystemforquickandaccuratefabricationofcomplex
shaped,3Ddentalrestorationparts.Basedonthepreliminarystudy,futureworkcanbe
determinedintheefforttoproducehighqualitypartswithminimaldefects.

MaterialsandMethods
TheprimarymaterialusedforthisstudyisVITAVM13Base(VitaZahnfabrik,Germany),
whichisaleucitereinforcedglassceramicwidelyusedfordentalpractice.Thechemical
compositionandbasicpropertiesofthepowderprovidedbythemanufacturerisshown
inTable1(VitaVM13,2009).

Linearcoefficient
Flexural
Chemical
Powder
Particlesize
ofthermal
strength
composition(wt%)
expansion
SiO2:5963%,
VM13
Al2O3:1316%,
~120MPa
~18m
13.614x106K1
Base
K2O:911%,Na2O:
46%
Table1GeneralinformationofVM13Base

Theoriginalpowdersexhibitsignificantaggregationwhichmadeitunsuitableforthe
process.Preliminaryparticlesizeanalysis(MicrotracS3000)indicatedthatthe
characteristicsizeoftheaggregationwasaround100105m,asshowninFig.1.Two
factorswereconsideredtocontributetotheaggregation.FromFig.2,itcouldbeseen
thatthepowdershaveaveryirregularmorphologyandaratherwidesizedistribution,
whichcouldsignificantlyreduceitsflowability.Inaddition,thelargesurfaceactivityof

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thesilicapowdersalsomakesthempronetoclumping(Bagweetal.,2006).Therefore,
Presinteringandflowagentadditionwereimplementedinanattempttoimprovethe
issue.

Fig.1ParticlesizeanalysisresultsfortheVM13Basepowder

Fig.2MorphologyoftheoriginalVM13powder

Throughapreliminarytrialitwasfoundthatatabout600Cofsinteringtemperature,
significantdensificationdoesnotoccurforthepowder.Therefore,600Cwaschosento
bethepresinteringtemperatureinordertoachievefasteffects.Theholdingtimefor
presinteringwaskeptat30minutes,followedbyfurnacecooling.
SurfacemodifiedR972SiO2powder(COSMOSPlastic&Chemicals)wasusedastheflow
agent.Thepowderiscomposedof>99.8%fumedsilicatreatedwith
dimethyldichlorosilane(DDS),withanaverageparticlesizeof16nm.Theflowagentwas
addedtotheoriginalVM13powderandmixedbyhanduntilsatisfactoryimprovement
offlowabilitywasobserved.
Theflowabilitywasevaluatedbytheangleofreposefortheoriginalandtreated
powders.Inaddition,micrographsweretakenforthepresinteredpowdertoevaluate
theevolutionofpowders.Afterthetreatment,theprocessablepowderswereusedto

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printsamplecrownpartsusingtheMLab.Thebinderusedfortheprocesswasthe
ExOnePMBSR104,anethersolventbasedbinder.Afterprinting,thegreenpartswere
driedintheovenat70Covernight.Theschematicofthepostsinteringprocessis
showninFig.3.Thegreenpartswereheldat500Cfor1hourtoburnoutthebinders,
followedbyatwostepsinteringsequenceat700Cand850C,respectively.The
dimensionsofthefinalpartsweremeasuredwithcaliperbeforeandaftersintering,and
resultswerecomparedtoevaluatetheshrinkage.Thecrosssectionalmicrostructureof
thesinteredsampleswerealsopreparedandobservedusingopticalmicroscopy.

Resultsanddiscussion
Presinteringdidnotseemtohavesignificanteffectontheflowabilityofthepowder.
Fig.3showsthemorphologyofthepowdersafterthepresintering.FromFig.3itcould
beclearlyobservedthatsignificantsinteringoccurredwhichresultedinthegeneration
oflargepowderaggregations.Ontheotherhand,theflowagenthadamoresignificant
effectontheflowabilityofthepowderattheratioofapproximately7%involume.Fig.4
showstheanglesofreposeforeachsample,andTable2showstheresultsofthe
measurement.Presinteringwasusedforceramicpowderswithfineparticlesizesin
previousstudiesusingselectivelasersintering(Harlanetal.,1999).However,fromthis
studyitseemsapparentthatwithhighlyirregularpowders,evenifthepresintering
couldreducethetotalsurfacearea,theincreaseofparticleirregularitywillcanceloutall
thebenefitsandpotentiallyresultinthereductionofflowability.Itwasexpectedthat
theadditionofflowagentcouldimprovetheoverallpowderflowabilitybyservingasa
lubricationinterfacebetweenthelargeVM13powders,whichwasverifiedbythe
study.

Fig.3MorphologyofVM13powderafterpresintering

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(a)Original

(b)Presintered
(c)Flowagentaddition
Fig.4Anglesofreposeforeachtypeofpowder

Powder
Angleofrepose(degree)
Original
64
Presintering
66
7%vadditionofflowagent
56
Table2Anglesofreposeforeachtypeofpowder

Thepowderwithflowagentadditionwassuccessfullyusedfortheprintingofcrown
partsintheMLabandsinteredsubsequently.Fig.5showstheoriginalpartaswellas
thepostsinteredparts.Significantshrinkagecouldbeobserved.Thedimensionsas
showninFig.6weremeasuredforthreesamples,andtheresultsareshowninTable3.
Theresultsarequiteconsistentforeachdimension,andanaverageof25%32%
shrinkagewasobservedineachdimensioncomparedtothegreenparts.Theshrinkage
valuesareconsiderablebutreasonableconsideringthatthepowderishighlyirregular.A
slightdifferenceofshrinkagebetweenthebuilddirection(alignedwiththedimension
H)andtheothertwodirectionswereobserved,whichcouldbecausedbytheburnout
ofthebinder.Thereisalsoaslightdifferenceofshrinkagebetweenthetwoplanar
directionsperpendiculartothebuilddirection,ascouldbeseenfromTable3.Thiscould
beassociatedwiththespecificgeometryofthesesamplessuchaswallthickness.
However,withoutfurtherinvestigation,itisdifficulttodeterminethelikelycauseofthis
phenomenon

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Before

After

Fig.5Greenandpostsinteredcrownparts

Fig.6Measurementofdimensions

Sample

L(mm)
W(mm)
H(mm)
Beforesintering
1
11.50
11.55
6.00
2
11.45
11.55
6.07
3
11.43
11.58
6.03
Postsintering
1
8.80
8.16
4.12
2
8.61
8.11
4.08
3
8.60
8.09
4.13
Linearshrinkage
1
23.48%
29.35%
31.33%
2
24.80%
29.78%
32.78%
3
24.76%
30.14%
31.51%
Average
24.35%
29.76%
31.88%
Table3Shrinkageofthesamples

Fig.7showsthemicrostructureoftheceramicsamplesaftersintering.Ingeneralthe
sinteringseemedtohaveachievedarelativelyhomogeneousdensification.Largevoids
aswellassomelightparticlescouldbeclearlyobserved.Thesizeofthevoidsvariedbut

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wereatthemagnitudeof50100m.Thisseemedtohaveacorrelationwiththesizeof
theaggregationoftheoriginalpowder.Onepossiblecausecouldbethatduringthe
powderspreadingprocess,thelargeaggregationwasdisplacedbytherollerduetothe
temporaryadhesiontotherollersurface,whichresultedinsurfacevoidsonthenewly
spreadlayer.Anotherpotentialsourcethatcouldcontributetothevoidformationisthe
additionoftheflowagent.Themechanismofthesurfacemodificationintheflowagent
wastocreateahydrophobicsurfaceonthesilicaparticles.Sincesufficientwettingis
requiredtoformacontinuousbondingbetweenthebinderandthepowder,the
existenceoftheflowagentcouldpotentiallyaffectthecontinuityofthegreenpart,
leavingvoidsthatbecomedefectsafterthesubsequentprocesses.Furtherstudiesare
neededtoidentifythepotentialimpactoftheflowagentinthefinaldensitiesofthe
parts.Inaddition,theuseof850Casthedensificationsinteringtemperaturewas
largelyduetothelimitationofthefurnace,whileinthereferenceinstructionforthe
VM13powder(VitaVM13,2009),itwasrecommendthatthegreenpartbesinteredat
920C.Thelowertemperaturecouldalsocontributedtotheporositiesobservedinthe
sample.

Fig.7Microstructureofthepostsinteredpart

Conclusion
Inthisstudy,anofftheshelfdentalveneerpowderwassuccessfullyprintedusinganM
Lab.Theoriginalpowderhadsignificantaggregationissues,andtwomeasurements
wereusedintheattempttoimprovetheflowabilityofthepowder.Additionoftheflow
agentofabout7%volumewasshowntobeaneffectivemethodtoimprovetheoriginal
powderflowability.Atrelativelylowsinteringtemperature,thefinalpartsshowed
homogeneousdensificationandcontinuousmicrostructures,althoughlargevoidswere

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presentinthefinalparts.Theshrinkageofthepartsaftersinteringwasaround2530%
ineachdirections,andanisotropicshrinkagewasobservedinallthreedirections.
Furtherinvestigationsareneededtoidentifythecauseoftheanisotropicshrinkageas
wellasthesourceofthelargevoidsinthefinalparts,andadditionalmechanicaltesting
isalsorequiredtofurthercharacterizethequalityoftheprocess.

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