低压化学气相渗透法制备25维SiCfSiC复合材料

第36卷第2期 2008年2月 硅酸盐学报 JOURNAL0FTHECHINESECERAMICSOCIETY V01．36，No．2 Febma拶，2008 低压化学气相渗透法制备2．5维SiC／SiC复合材料 于新民，周万城，罗发 (西北工业大学，凝固技术国家重点实验室，西安710072) 摘要：采用低压化学气相渗透法制各了具有和不具有熟解炭界面层的2．5维连续sic纤维增强的sic复合材料(sicf，sic)。sic纤维的体积分数为30％ 和41％。所制备复合材料的气孔率为20％左右。当纤维为30％时，沉积有0．1¨m热解炭界面层的复合材料的弯曲强度由未加热解炭界面层的232MPa 增加到328MPa，而且材料由灾难性断裂转变为非灾难性断裂。在同一制备条件下，纤维体积分数为41％的siC，sic比30％的Sic，SiC具有更高的气 孔率。纤维为41％时，热解炭界面层厚度为0．1岫的sic—sic的弯曲强度只有244MPa，但是它具有更高的韧性和更长的纤维拔出长度。 关键词：碳化硅纤维磁化硅；低压化学气相渗透法；界面层；力学性能 中图分类号：TB332文献标识码：A 文章编号：045扯5648(2008)02_0150_04 2．5-DIMENSIoNSiC洚iCCoMPoSITESFf姬RICATEDBYLoWPRESSURE CHEMICAL、厂APoR矾FⅡ用RATIoN lUX{nm锄，zHOU晌nche昭，LUoFa (NationalKeyLabo咖ofSolidificationProcess协g，Nor吐1west锄P01ytechnicalUniVers峨Xi’an710072，Ch协a) Abstract：2．5．mmensioncominuoussiliconcarbidefiberreinforcedsiliconc抽idccomposites(SiC—SiC)0nt11einteI_f如ewithand wi出outapyrocarbonlayerwerefabricatedbylowpressurech锄icalvaporin6l廿ation．Thevolume丘actionsofSiCfiberwere30％ and4l％．Theporosityofthefabricatedcompositeswasabout20％。Theflex啪ls虹它ngthoftheSiC／SiCcompositewith30％fiber aIldhavingaIlinterf沁epymcarbonlayerabout0．1岬thickincreased舶m232Mpato328MPaand廿le妇turebehaviorchaIlged 丘omcatas仃ophicfailllretonon—catas仃ophicfailurecomparedwitht11ecompositewinlouttIlep”ocarbonlayer．Theporosi够ofme compositesligtltIyitlcre嬲edwiththei11creaseoffibervolumefhctionf而m30％to4l％When也ef．ab矗cationprocessconditions weres狮e．Thenexuml蚰．e119mofSiC—SiCwi廿141％fiberandanimerfacelayerabout0．1umt11ickwasonly244MPa，butthe 丘acturetougllIlesswasgreaterandmelengthoffiberpull—outwas10nger． Keywords：siliconcarbidefiber／siliconcarbide；lowpressurechemicalvapori11filtration；interfkelayer；mecharIicalproperties Continuousfiberreinf．orcedce“unicm撕xcompos— itesfCFCCs)showsup鲥orpe晌珊anceateleVated temperaturesandhighertoughnesswhencomparedwith mon01ithiccemmics．【1J Formesereasons．CFCCshaVe tllemostpotentialtobeusedinadvancedaem—engines， space，andfusio畦powerreactors．AmongtheseCFCCs， continuoussiliconcarbideflberreinf．orcedsiliconcarbide composite(SiC／SiC)isapromisingm砷erialthathas receivedconsiderableattention．Manyinvestigationshave beenconductedonone—dimension(1D)，铆o．dimension仨D) andthree．dimension(3D)wovenSiC／SiCcomposite m劬erials．【¨J2．5DwovenSiC—SiCcompositeshave 收稿日期：2007_07h09。 第一作者：于新民(1980一)， 通讯作者：周万城(1953一)， 修改稿收到日期：2007-09—10。 男，博士研究生。 男，教授。 weakae010m)pismcom口aredwinllDaIld2Dwoven compositesandalowweavecostcomparedwith3D woVencomposites． Sof札fblWkindsofnlethodshavebeendevelopedfor f-abricatingSiC／SiCcompositematerials：hot-pressing， reactivemeltillfil仃ation，polymerin6ltrationa11dp)，roly- sis(PInalldch锄icalvaporinfil仃ation(CⅥ)．CVIhas beendevelopedasanextensionof廿1eweU．established chemicalvapordepositionmeⅡ10dandhasalreadybeen usedincommercialproduction．Itisoneofthemost promisingtechniquesf-orthef．abricationoffiber_ren f-orcedca铆mic咖posites．Thep—mar矿advan切geofthe Receiveddate：2007_07_09．AppmVeddate：2007-09-10． Firstauthor：Yuxinrnin(1980_)，male，post鲜珂吼testudentf缸doctor degTee． E—maⅡ：min】【inl943@s劬．com Corr麟pond朗tauthor：zHouw如cheng(1953_)，male，pmfcssoL E—man：wczhau(园nwpu．edu．c11 万方数据 第36卷第2期 于新民等：低压化学气相渗透法制备2．5维siC—sic复合材料 CVImethodisthat也ebrittlece舢icfibersremainun． d锄aged姗ngt11ef矗bricationprocessandcomposites winlcomplexshapescanbefabricatedeasily． Inthepresentwork，2．5DwovenSiC／SiCcomposites werefabric咖dby10wpressurechemicalv印orinfiln．a— tion(LPCⅥ)，Apyrocarboninte血ce1ayerdepositedon theSiCfsu嘞cewasusedtosuccess如llyimproveboth thestrengthaJldtougllllessofthecomposites．Theporos． ity，s仃ength，aJld行actllrebehaviorofcompositeswere investigated．Thee虢ctsoffibervolume丘．actiononthe in矗l仃ationprocessaIldmechanicalpmpertiesofthe compositeswercstudied． 1 Experimentalprocedure neSiC助ersusedinthetestⅥrere：suppliedbythe NationalUniversit)rofDefenseTechnology，a11dhada tensiles仃en咖of2200MPaa11dadi锄etefof10阻． The助erswerewovenintoa2．5-dimensionpe仃om，as showninFig．1． ’ Fig．12．5DSiCfiberpeff．om Propvlenewithapuri田of99．9％wasusedasthe carbonsourcetof．abncateapyrocarboninterf配elayerby LPCVIat90肛l100℃．2—10kPa．TheSiCmatrixwas f-abricatedat900—1150℃．5—10kPa．Metllvltrichlorosi— lanewasusedtof．abricatetheSiCmatrixandcarriedinto thereactorbyhydl．ogenthroughbubbling．Hydrogenwas usedasthediluentgas． Theinterfaces臼rIlcturesoftheSiCf锄dSiCmatrixes werestudiedusingascanningelectl．onmicroscope(SEM， ModelJeol840)．Theporosi锣wasmeasuredusingthe Archimedesmethod．Thefle)【uralsn-engmofsamples withmedimensionsof2．0nunx5．0mmx40nlrnwas measuredbythet11ree-pointbendingnexllraltest，witha spanof30mmandaloadingvelocityof0．5nHn／nlin．The stress—s仃aincurvesweregivenatthesametime． 2 Resultsanddiscussion Figllre2giVestheimagesoftheinteIfacepyrocarbon layer．Theinterface1ayerwasunifomaIldhadasmoom surfIace．Itsthicknesswasabout0．1“m． F谤2Secondaryelec订on(SE)andbackscatteredelec仃on (BSE)imagesofinterfkepyrocarbonlayer ThepropertiesofSiCf／SiCcompositesaI℃listedin Table1．Theinterfacelayerhasanimportantinnuenceon themechanicalpropertiesofSiC／SiC．【卜7 J Thenexural sn．engthofmeSiC／SiCcomposite(sampleNo．1)with 30％SiCfandapyrocarbonintemcelayerabout0．1岬 thickincreased仔om232MPato328MPacomDaredwith Ⅱlatofthecomposite(s锄pleNo．0)withoutaninter|’ace 1ayeLSamplesNo．1andNo．2werefabricatedinthe sameconditions：allmeparametersexc印tthevolume 丘actionoftheSiCfiberwerecompletelythesame． However，也estfengthofs锄pleNo．2wasonly244MPa， whilematofs锄pleNo．1was328M咿a．Theporosi够of s锄pleNo．2wasali仕lehighermanthatofsanlpleNo．1． Withtheincreaseofthevolume仔actionofthefiber’tlle n11]mberofmicroporesbe铆eenfiberandfiberincreased， andthesizeofthesemicroDoreswassmaller．Forthese reaSons，medi舰sionofdepositiongaswasmoredimcult andcloggillgoccurredmoreeasilywimt11ed印os“ingof 1’ablel PropertiesofSiCI，SiCcomposites s枷plemcknessofillterface／FiberVolumeFlex哪Is仃ength／Porosi酬 No． 岫 丘actiof慨 MPa ％ 万方数据 硅酸盐学报 2008年 meSiCmatrix．Allthesefactorsresultedinmehi2血 poros曲andthelowstrcngthofs锄pleNo．2．Tlleyalso indicatematmeprocessingpar锄etersshouldbe changedwhen协efibefv01啪ef}actionisincl．eased6．om 30％t041％． Figure3givesthesn．ess—s仃aincurvesoftheSiCF，SiC composites．Thecomposite(sampleNo．0)withoutan interfacelaVerexhibitedcataS仃ophicfailurebutithada nonlinearincreasingstageaRerthecrackinitiation1inear increasingstageinitss仃esS-s仃a．incurve，asshownin F适．3，蛐dthereasonisthattherewasmuchhotcrackillg intheSiCmatrix，asshowninFig．4．Thishotcraucking providedmicro—cracksmatcouIdimprovethetoughness andmealbilit、rofdef．011nation．Thestress—s仃aincuIveof sampleNo．1waSa坶picaltoughened疗actIlre饥Irveand itcanbedividedintomreeportions：mecmckinitiation linearincreasingstage：thesubsequentnonlinearincreas． ingstage，inwhichmeSiCmatrixcracks；andthel弱t，a fallingstageinwhichfiberscrackeda11dwerepulledout． ComparingmecurvesofsamplesNo．0a芏ldNo．1shows matthedepositionofthepyrocarboninterfacelayerwas successfhlandefrectivelVimprovedthemechanical properties．Boththestrengthandtoughnessofthe SiC—SiCcompositeincreasednotablyduetotlleexis． tenceofaninterlj犯elaVer．Thecur~，eofs锄pleNo．2 0 0．2 O．4 0．6 0．8 1．0 1．2 1．4 1．6 S仃ain／％ Fig．3S仃ess_S仃aincurvesofSiC捐iCcomposites Fig．4HotcrackingintheSiCma打ix droppedmoreslowlymaIlmatofs锄pleNo．1．Thelength offibcrpull—outwaslonger，whichcallbeprovenbyme SEMphoto肿pllSofme位咖esllrface．Theseresultsindi． catetllattheincreaseofthefiberv01ume行action、】l协s favorableforimpmvingthetougllllessofthecomposites andthefiberDull—out． Figure5giVesmeSEMphotographsofme仔actIlre su墒ce．Thefhctu】陀sumceofs锄pleNo．Owasaplane wimnodebondingor肋erpull一out，asshowninFig．5(a) TherewaseXtensivefiberpull—outins锄plesNo．1and No．2andthelen劬ofpull．outforsampleNo．2was iongermanmatofsampIeNo．1(seeFigs．5(b)aIld5(c))； meirs仃ess～straincurvescanbeseeninFigure3． Fig．5Fractllremo印hologiesofSiC／SiCcomposites 万方数据 第36卷第2期 于新民等：低压化学气相渗透法制备2．5维SiC／SiC复合材料 · 153· 3 Conclusions 2．5一dimensionSiC／SiCcompositeswinlaporosi田of about20％werefabricatedbyLPCⅥ．111edepositionof apyrocarboninte而celayerise饪IectiVe：withthepyI．o． carboninte墒celayer，theneXlIrals仃en劬ofSiC／SiC compositewim30％fiberisgreaterthanthatofSiC／SiC with41％fiberaIlditss缸．ess—strajncurveisa t!l，pical tou曲enedfhcturecurve．Thecompositewith41％fiber hasalongerfiberpull．outlengththantllatofthecom． Dositewith30％fiber．Theincreaseoffibervol啪efhc— tion自om30％to4l％improvesmechanicalpropertiesof SiC／SiCcomposites． Refbrence： 【1】 JACQuESS，GIJE，丌EA，LANGLAISF，eta1．Preparati蚰andch小 acterizationofSic／SiCcompositeswi血cornposidon—gradcdC(B) inteIphase[J】．JEllrCeramSoc，1997，17(6)：l083一l092． [2】 INGI玎jLSE，LAMONJ．Anappmachtot11emechaIlicalbehaviorof c／SiC锄dSic／SiCce础micma血xcomposites，partl experin嘣1tal resul协【J】．JMaterSci，1991，26(20)：5403—5410． [3】 INGHELSE，L舢“oNJ．Anapp∞achtothemechaIlicalbehaviorof C／SiC粕dSiC／SiCcemnlicma出c伽叩osites，part2theoreticalap— proachm．JMaterSci，199l，26(20)：54lo_5419． 【4】YANGJM，D11MARSE，LNW．JI梳n咖ech趾icald啪bil蚵of cⅥ-pmcessed伽o-d曲ellsionallywoVen锄d thrce—di|msionally braidcdSiCfibre-re碰砷cedSiCconlpos沁s叨．JMacersci，1994， 29(20)：549l一5497． [5】 PlUⅥNAGEP，MAJIDIAP，CHouTW．D狮gecharactcrizationof 佃。一dimensionalwovenand也reedimensi舢mbmidedSiC—SiCc锄一 posites田．JMatersci，1996，3l(1)：232-241． 【6】 SHIYmg，ARAKIHiroshi，YANGW醯，eta1．Innuenceofpre—coating 0nmechanicalpr叩enies粕dint曲cials劬m聃sofSiC(o／SiCc锄一 posite【J】．JIno喀Mater(inChill船e)，2001，16(5)：883—888． 【7】YANGW'Ko王形AMAA，NODAT，eta1．hl锄cialch踊c翰乜ation ofCⅥ一SiC，siCcomposites[J]．JNuclMater’2002，307_31l：l089- 1 092． 万方数据 低压化学气相渗透法制备2.5维SiCf/SiC复合材料 作者： 于新民， 周万城， 罗发， YU Xinmin， ZHOU Wancheng， LUO Fa 作者单位： 西北工业大学,凝固技术国家重点实验室,西安,710072 刊名： 硅酸盐学报 英文刊名： JOURNAL OF THE CHINESE CERAMIC SOCIETY 年，卷(期)： 2008，36(2) 引用次数： 0次 参考文献(7条) 1.JACQUES S.GUETTE A.LANGLAIS F Preparation and characterization of SiC/SiC composites with composition-graded C(B)interphase 1997(6) 2.INGHELS E.LAMON J An approach to the mechanical behavior of C/SiC and SiC/SiC ceramic matrix composites,part 1 experimental results 1991(20) 3.INGHELS E.LAMON J An approach to the mechanical behavior of C/SiC and SiC/SiC ceramic matrix 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