单质硅溶解法制备大粒径硅溶胶

31420108()JournalofQingdaoUniversityofScienceandTechnology(NaturalScienceEdition)Vol.31No.4Aug.2010:16726987(2010)04035506,*,,,赟(,266042):考察常压状态和加压状态下单质硅溶解法制备硅溶胶的工艺条件,探索加压状态下的大粒径硅溶胶的制备结果表明:常压状态下,硅溶胶制备的较佳工艺为反应温度80,反应时间8h,200mL蒸馏水中加入10g硅粉和03g氢氧化钠,所得硅溶胶粒径在30nm左右;加压状态下,硅溶胶制备的较佳反应条件:压力2MPa,温度150,反应时间8h,200mL蒸馏水中加入10g硅粉和03g氢氧化钠,可制得粒径在100nm以上,单分散状态良好的大粒径硅溶胶:单质硅;溶解法;大粒径硅溶胶:TQ127.2:APreparationofSilicaSolofLargeParticleSizebySiliconDissolvingMethodHUANGCaixia,LIZhenqiu,ZHANGYuanjing,LIJinghua,CAOChengyun(CollegeofChemicalEngineering,QingdaoUniversityofScienceandTechnology,Qingdao266042,China)Abstract:Silicasolwaspreparedbysilicondissolutionmethodusingsiliconpowderandwaterasrawmaterialsunderatmosphericstateandpressurestate.Theresultsshowedthat,underatmosphericstate,theoptimumreactionconditionsweresiliconpowder10g,sodiumhydroxide03g,water200mL,reactiontime8hat80.Underaboveconditions,theparticlesizeofobtainedsilicasolwasabout30nm.Whileundertheconditionsofreactionpressure2MPaandtemperature150,theparticlesizeofobtainedsilicasolwaslargerthan100nmwithgoodmonodispersity.Keywords:siliconpowder;dissolution;silicasoloflargeparticlesize:20091024:(1983),,.*.1958,,,,[12],130~170,,[3]:,,,,SiO2,100nm50%[4][5],zeta,120nm()3111.1,,,,,:Si+2OH-+H2OSiO32-+2H2!SiO32-+H2OSiO2+2OH-1mSi+(2m+n)H2OmSiO2∀nH2O+2mH2![6]:,SiO2H+OH-,SiO2,:,SiO2pH,pH,,,SiO2pH=2,pH2,OH-,:HOSiOHOHOH+HOSiOHOHO-HOSiOHOHOSiOHOHOH+OH-,,,,SiO2,,1.2,,;,,,NDJ5S,;,JEM100CX#,;,ZEN3690,1.31.3.1,,,,,,,,,1.3.2,,,,,,,,,,1.4,,,22.12.1.1,200mL10g,NaOH03g,8h,11,80,,80,,1(a)(b),65~80,,pH,(85~10);80802.1.280,200mL10g,NaOH03g,22,,8h,,53mPa∀s15∃B,pH86,8h3564:1Fig.1Effectofreactiontemperatureonpropertiesofsilicasol2Fig.2Effectofreactiontimeonpropertiesofsilicasol2.1.3200mL,03g,80,8h,33Fig.3Effectofsiliconpowderdosageonpropertiesofsilicasol3,,pH10g,,pH10g2.1.4,,Na+,200mL10g,8h,80,,44,,,,;,Na+,,,03g357()314Fig.4Effectofcatalystdosageonpropertiesofsilicasol2.1.5TEM200mL10g03g,808h,53mPa∀s,15∃B,pH9,55,,,,30nm5TEMFig.5TEMimageofthepreparedsilicasol2.22.2.1SiO2[3],1002MPa,10MPa,,200mL10g03g,80,8h,,,,66(a),,,2MPa6MPa,,120nm111nm,24MPa8MPa,,6(b),22,21,2MPa6MPa,6(b)2,1,,2,,2MPa,2,6Fig.6Particlesizedistributionsofsilicasolpreparedunderdifferentpressures3584:,:,,,8077Fig.7Particlesizedistributionsofsilicasolpreparedunderlowpressure7(a),,2MPa,957%50nm2MPa,881%50~100nm7(b),,;2MPa2MPa2.2.22MPa,2.2.1,80,100,120,150,180,,88Fig.8Particlesizedistributionsofsilicasolpreparedunderdifferenttemperatures8(a),,,150,4(8(b))8(a)150,90%100~200nm,8(b)82%,,,TEM99:,,,:200mL10g03g,2MPa,150,8h359()319TEM(50000%)Fig.9TEMimageofthepreparedlargeparticlesizesilicasol(50000%)31):200mL10g03g,80,8h30nm2):200mL10g03g,2MPa,150,8h100nm,[1]Rule,Hundred,Del.Aqueoussilicadispersionsandtheirproduction:US,3012972[P].1962.[2]Payne.Processforpreparingsilicasols:US,4356107[P].1982.[3],,,.[J].,2004,23(7):747750.[4],,,.[J].,2005,24(8):925929.[5],,,.SiO2[J].,2005,28(3):536538.[6],,.[J].,2006,44(11):2325.(责任编辑孙丽莉)(上接第354页)[1]XiaHailong,TangFangqiong.SurfacesynthesisofZincoxidenanoparticlesonsilicaspheres:preparationandcharacterization[J].JPhysChemB,2003,107:91759178.[2]JiangZhangjie,LiuChunyan.Seedmediatedgrowthtechniqueforpreparationforasilvernanoshellonsilicasphere[J].JPhysChemB,2003,107:1241112415.[3]YangYang,ChuYing,YangFuyong,etal.Uniformhollowconductivepolymermicrospheressynthesizedwiththesulfonatedpolystyrenetemplate[J].MaterialsChemistryandPhysics,2005,92:164171.[4]LiGuicun,ZhangZhikun.Synthesisofsubmicrometersizedhollowtitaniasphereswithcontrollableshells[J].MaterialsLetters,2004,58(2223):27682771.[5]AlexanderNKhramov,MaryanneMCollinson.Solgelpreparationofmacroporoussilicafilmsbytemplatingwithpolystyrenemicrospheres[J/OL].ChemCommun,2001:767768[20091116].=b008035g.[6]HuangZhangbing,TangFangqiong.Preparation,structure,andmagneticpropertiesofpolystyrenecoatedbyFe3O4nanoparticles[J].JournalofColloidandInterfaceScience.2004,275:142147.[7]DingTao,LiuZhanfang,SongKai,etal.Photoniccrystalsofoblatespheroidsbyblownfilmextrusionofprefabricatedcolloidalcrystals[J].Langmuir,2009,25(17):1021810222.[8]ManfredMuller,RudolfZentel,TorstenMaka,etal.Dyecontainingpolymerbeadsasphotoniccrystals[J].ChemMater,2000,12:25082512.[9]MarcEgen,RudolfZentel.Tuningthepropertiesofphotonicfilmsfrompolymerbeadsbychemistry[J].ChemMater,2002,14:21762183.[10]BerndGriesebock,MarcEgen,RudolfZentel.Largephotonicfilmsbycrystallizationonfluidsubstrates[J].ChemMater,2002,14:40234025.[11]RickCSchroden,MohammedAlDaous,AndreasStein.Selfmodificationofspontaneousemissionbyinverseopalsilicaphotoniccrystals[J].ChemMater,2001,13:29452950.[12]RickCSchroden,MohammedAlDaous,ChristopherFBlanford,etal.Opticalpropertiesofinverseopalphotoniccrystals[J].ChemMater,2002,14:33053315.[13],,.[J].,2004,62(20):20892092.[14],,,.[J].,2002,15(2):189193.[15],,,.[J].,2006,23(1):1012.[16],,,.BPOKPS[J].,2003(5):688692.[17],.PS[J].:,2006,42(2):170175.[18]ZhangJianhui,ChenZuo,WangZhenlin,etal.Preparationofmonodispersepolystyrenespher