添加填料合成SiC(Al)纖維的先驅(qū)體聚鋁碳硅烷

1、226Vol.22No.6December2008200812CHINESEJOURNALOFMATERIALSRESEARCHSiC(Al)(CFC410073),.:46%,10082436,SiSi;N265%,400,120069%;SiSiSiCSi,SiAlCO2.1GPa,Ar1800SiC(Al).,SiC,TQ3431005-3093(2008)06-0623-06PolyaluminocarbosilanepreparedwithllingsasprecursorsforSiC(Al)bersZHAODafangLIXiaodongZHENGChunman(KeyLabof

2、CeramicFiberandComposites,NationalUniversityofDefenseTechnology,Changsha410073)*SupportedbyNationalNatureScienceFoundtionofChinaNo.59972042andSupportedbyNationalDefenseFundamentalResearchFoundationofChinaNo.9140C820820506KG0102.ManuscriptreceivedFebruary18,2008;inrevisedformApril10,2008.*Towhomcorre

3、spondenceshouldbeaddressed,Tel:(0731)4576421,Email:xdli0153ABSTRACTPolyaluminocarbosilane(PACS)wassynthesizedbyareactionbetweenpolysilacarbosilaneandaluminumacetylacetonateatambientpressureinN2.Areactorwithahightemperaturepyrolysisequipmentwhichwaslledwithllingswasused,soPACScanbepreparedforshorterr

4、eactiontime.ComparingwiththePACSsynthesizedwithoutllings,itsincreasedfrom1008to2436,itsmoleculardistributionwasnarrower,anditsSiSibondscontentdecreased.Moreover,ceramicyieldoftheobtainedPACSat1200inNfrom2wasincreasedfrom65%to69%whenitwassynthesizedwithllings.ItissuggestedthatthetranslationSiSibondst

5、oSiCbondswasfacilitatedwhenthellingexisted.ThePACSisspinnability.Lowermasswasgottenduringaircuringprocess.ThetensilestrengthoftheobtainedSiAlCOberis2.1GPa.AdensiedSiC(Al)berwasobtainedafterbeenheatedat1800inAr.KEYWORDSinorganicnon-metallicmaterials,Polyaluminocarbosilane,SiCbers,preceramicpolymerPCS

6、,PCB3.(Polycarbosi-,SiSi,lane,PCS),(Polydimethylsi-,lane,PDMS)1,23.,.SiC(Poly-.,Yajima1300,borodiphenylsiloxane)SiCO,.,*:(1)599720429140C820820506KG010246.;(2)2008218;2008410.SiC:,71011,12.TyrannoSA7,624220022,(Polyaluminocar-(Ultravioletvisiblespectrum)bosilane,PACS)PCS(Aluminum.,200-400nm.PACSacet

7、ylacetonate,Al(AcAc)3)110.1g/L.HMKPCS.(Polysilacarbosilane,PSCS)Al(AcAc)3NETZSCHSTA449CN2(ThermogravimetricAnalysis,TG),/min.PACS13,14,10TC436N/O,SiSi.PACSO,AlPACSSiC(Al).YG002,.SiC(Al)PACS,30.12.1,PACS1.1PACS,58h33h.,PACS,PDMS.PDMS4005001PSCS.PSCSAl(AcAc)3,58h31h,(400550),.PACSF1.10.5PACSC,(10),0.7

8、3m3/m3.(4004502h),PACSF2(PACSFPACSF2PACS,PACSF.).SiC,1PACS,1.2PACSC.PACSF1PACSC,PACS,33h(PACSF2)FTIR(Nicolet),4cm1.SiCH3PCS:PACS.,4004000cm1.H1360cm1SiCH2SiC.1400cm1CH1,PACS,(ASiCH2Si/ASiCH3),2950cm1CHSiCH2SiSiSiCH22100cm1CHSiH,1400cm1SiCH315.Waters1515,1250cm1CH2(Gelpermeationchro-1030cm1SiOSiCmato

9、graphy,GPC),.,830cm1,1.0mL·min1,.PACS.SiH.BrukerDRX,TMSPACS,5001HNMR(1HnuclearmagneticPACS.PACSFPACSCresonancespectroscopy)ASiH/ASiCH30.670.7,CDCl3.UV2800PACSSiH.1PACSTable1PropertiesofPACSobtainedundervariousconditionsReactiontime/h583133Yeild(%)505149100820762436Softeningpoint/120110125Chemic

10、alAnalysisAl0.990.720.91O6:SiC(Al)6251PACSCPACSF2PACSCPACSFFig.1FTIRspectraofPACSCandPACSFFig.2UVVisspectraofPACSCandPACSF3PACSC,PACS-FPSCSGPC(a)(b)Fig.3GPCcurves(a)anddierentmolecularweightcontentsof(b)PACSC,PACSFandPSCSASiCH2Si/ASiCH1,GPCPACSFSiCH2Si16,(3b).PCS,LPS,PACSFSiSi,PACSP

11、ACSC,(.,PACSFPACS1).SiSi15.2,PACSF2.2,(200nm280nm)PACSC,4,200PACSCPACS-FSiSi.PSCS,(3a),;400,PSCSSiSiSiCSi14;600800,;3,CH3SiHCHPACSGPC(3a),;800,PSCS,;PACS16,17.PACSCCPACSFGPC,PACSF,PACSF400.,PACSC.LgMw3(WL,PACSF,Mw1000),LgMw4.00.PACSF120069.2%,(WH,Mw10000),3LgMw4.00PACSC(65%).6264PACSFPACSCTGFig.4TGc

12、urvesofPACSFandPACSCPACS,PACS.,PACS.PACSSiH,18,16.SiH18.,PACSF,SiH(2).2PACSCPACSFTable2PropertiesandcuringbehaviorsofPACS-CandPACS-FbersPACSCPACSFCuringtemperature/200200Curingtimeat200(min)360360Greenbers(ASiH/ASiCH3)0.690.67Aftercuring(ASiH/ASiCH3)0.0970.24SiHreactiondegree(%)86.064.2Massgains(%)1

13、0.749.141300N2,SiAlCO;SiAlCO1800,SiC(Al).3PACSF3PACSCPACSFTable3PropertiesofceramicbersderivedfromPACSCandPACSFbersPACSCPACSFTensileStrength/GPa13001.92.1Diameter/µm130014.213.7TensileStrength/GPa18001.01.1Diameter/µm180011.610.9225PACSFPACSC1800XRDFig.5XRDpatternsofberssinteredat1800de-ri

14、vedfromPACSFandPACSCPACSC.XRDSiC(5),236.560.171.9(111),(220)(311);234.241.475.7SiC.,PACSSiC(Al).6,PACSSiC(Al),PACS.2.3SiC(Al)PSCSAl(AcAc)3PACS,PSCS(Kumada),PSCSAl(AcAc)314.,PACSSiSi(2)SiC(1),(1).15,Kumada,SiCH2·,.SiCH2·,.PSCS,.,.6:SiC(Al)6276PACSF9(a),(c)PACSC(b),(d)SiC(Al)Fig.6SEMphotogra

15、phofSiC(Al)bersobtainedfromPACSF(a),(c)andPACSC(b),(d),.PSCS.SiC1+xOy(s)SiC(s)+SiO(g)+CO(g)+C(s)11,19,PSCS,.PSCSPSCS,.2,.,PACSFSiC(Al),PACSF.,.3,SiSiSiCSi.(PACS),SiSiSiC46%,PACSF1008Si.,2436,PACSFPACSF(3),(PACSC,SiSi(1).N2,400,N24004).),120065%69%.(PACS-F,SiPACS,SiPACSFSiAlCOSiCSi.PACSF.SiSiPACSC,Si

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