电子陶瓷材料钛酸钡的制备研究

湘潭大学硕士学位论文电子陶瓷材料钛酸钡的制备研究姓名：宋方平申请学位级别：硕士专业：应用化学指导教师：朱启安20060501I2µm1µmBaTiO3BaTiO3Ba(OH)2·8H2O16nmBaTiO3(TEM)X1.0/TritionX-10//BaTiO3ωoX20nm~80nmICP1.0/OPEmulsifier-10//ωoTEM40nm300nm6µmICP1.0:W/OIIAbstractFerroelectricparticlesBaTiO3,akindofelectronicceramicswithhighdielectricconstantatroomtemperature,havebeenusedasrawmaterialsforthemanufactureofmultilayerceramiccapacitors,positivetemperaturecoefficientresistivity(PTCR)thermistorsandotherelectro-opticcomponents.Thepropertiesandmicrostructureofbariumtitanateceramicsarehighlydependentontheratioofbariumtotitanium.Preparationoffineceramicpowdershasbecomeanimportantpartofmodernceramicresearch.Thereisastrongtrendtowardtheapplicationofchemicalmethodforpowdersynthesisinelectronicceramics.Recently,withtheminiaturizationofelectronicdevices,thethicknessofdielectriclayersinMLCChasbeenreducedto2µm,anditcanbeexpectedthatthisthicknesswillbecomelessthan1µminthefuture.Consequently,withthereductionofthicknessofthedielectriclayersinMLCC,BaTiO3particleswithsizesfromafewhundrednmtoafewtensofnmarerequired.Besides,Thesuper-fineBaTiO3ceramicpowderslowersinteringtemperature,achievefineceramicgrainsizeuniformlyandsaveenergy.Tobeginwith,BaTiO3nanoparticlesweresynthesizedwiththediameterabout16nmusingBa(OH)2·8H2Oandtetrabutyltitanateastherawmaterialsbyhydrothermalmethodinthispaper.Theeffectofthesynthesistemperatureandconcentrationofreactantsontheparticlessize,theeffectofthemolarratioofbariumhydroxidetotetrabutyltitanateontheratioofbariumtotitanateinproducts,andtheeffectofdifferentannealtemperatureonthecrystallatticeparameterwerestudied.TheproductswerecharacterizedbyFT-IR,TEMandXRD.Theresultsshowthattheproductsaresinglecubicsystemnanoparticles,themolarratioofbariumtotitaniumofproductsis1.0fromchemicalanalysis.furthermore,NanisizedBaTiO3particlesweresynthesizedinreversemicroemulsionconsistingofwater,Trition-10,n-hexanolandcyclohexane.Thereactionconditionswereoptimizedonthebasisofthestudyoftheinfluenceofthemolarratioofwatertosurfactant,theconcentrationofreactantsandageingtimeontheshapeandsizeofBaTiO3particles.ThepreparedBaTiO3sampleswerecharacterizedbyXRDandTEM.TheresultsshowthatthesphericalBaTiO3nanoparticleswithanaveragesizeof2080nmbelongtosingletetragonalsystem,Themolarratioofbariumtotitaniumofproductsis1.0fromICPanalysis.Finally,BaTiO3nanorodsweresynthesizedbyadopingwater/OPE-10/n-hexanol/cyclohexanereversemicroemulsionsysteminthispaper.ThereactionIIIconditionswereoptimizedonthebasisofthestudyoftheinfluenceofthedifferentωoandtheconcentrationofreactantsontheproducts.TheresultsofcharacterizationofsamplesbyTEMshowthatthediametersofthepreparedBaTiO3nanorodsareapproximately40nm,andthelengthsrangefrom300nmto6µm.Themolarratioofbariumtotitaniumofproductsis1.0fromICPanalysis.Keyword:hydrothermalsynthesis;W/Omicromulsion;bariumtitanate;sphecalparticle;nanoparticle;nanorod11.11.1.1nanomaterial0.1~100nm1.1.21.1.31.1.4100nm1.1.51.121.11.1.61.2BCC20037630.62008287BCC2003398200875173%1.3PTC(MLCC)[1,2](DRAM)BaTiO3(MLCC)2µm1µmBaCO3TiO21000~1200[1]BaTiO3[3~11]ZhuWeidong[9]BaTiO3TakeuchiTomonari[10]BaTiO395%HuaruiXu[12]ZhuWeidongBaTiO370nmBaTiO3500nmBaTiO3BaTiO31.4BaTiO31.4.1-[1315]BaTiO34BaTiO3BaCO3+TiO2BaTiO3+CO2(1.1)1200~13001.21.2Na2CO3+K2CO3,600~1200BaCO3TiO2BaTiO3700~800BaTiO3120.2µm10µm3(1350)1.4.21(Complexprecursors)[16]1BaCO3,TiO2BaCl251Oxalatecoprecipitationmethod[17]BTOBTO85BTOBTOBaCl2+TiOCl2+2H2C2O4+4H2OBaTiO(C2O4)2·4H2O+4HCl(1.2)BaTiO(C2O4)2·4H2O800BaTiO3+4H2O+2CO2+2CO2(1.3)1.31.3BTOX-DTATGAGCIRBTO(BaCO3+TiO2)BaTiO5BaTiO3(CO)BaTiO3(CO)2Ba2TiO2CO31225BTOBTOTiCl4H2OBaCl2TiCl4H2OH2C2O4BaCl26BTO2[18]BaTiO3BaTiBaTiO3BaTiO3BaTiO3PechiniBaO·TiO2·3C6H7O8·3H2O6506MulderpH2.61.06003CN1061776ADE-24332791JP49-69399TiO2+Ba2+NH3·H2OH2O2pH8.70±0.20600BaTi1.001H2TiO4+H2O2+2NH3(NH4)2TiO4·H2O2(1.4)(NH4)2TiO4·Ba(NO3)2BaTiO4+2NH4NO3+H2O(1.5)2BaTiO42BaTiO3+O2(1.6)1.41.4H2O2TiO2+Ba2+NH3·H2OH2OpH8.700.2060072-Sol-Gel[1926]-60--pHBa(OC3H7)+Ti(OC5H11)4+4H2OBaTiO3·H2O+2C3H7OH+4C5H11OH(1.7)BaTiO3·H2OBaTiO3+H2O(1.8)1.51.5-Weilingluan[26]pHpH7pH813nm-PTCPTCBaTiO3PTC()-BaTiO3PTC3[8,2738]1:181004000.1MPBaTiO3123Hertl[39]TiO2BaTiO3BaTiO3TiO2TiO2Ovramenko[40]-TiO2Ti(OH)x4-xBa2+BaOH+BaTiO3TiO2BaTiO3TiO2TiO2TiO2James[29]BaTiO3-Walton[41]BaTiO3TiO2BaTiO3TiO2-BaTi()BaTi1.04.[42]9Ba/Ti=1.0pHH2TiO3350BaOTiO2950BaTiO3CO25.[4345]Wada[43]10nmBaTiO3TiCl410Ba(OH)2·8H2OBa(OH)2KOHpH13pH110nm1BaTiO32BaTiO3N2BaCO3BaTiO3[43]6.[46,47]JohnWangBa(NO3)2TiCl459550BeckTNP-35-BaTiO3101.4.3BaTiO3[48][48][49,50][51][5254][55][1,56][57,58]1.5BaTiO3NbTaBiSbYLaBaTiO3MnFeCuCr)PTCRPTCRBaTiO3BaTiO3BaTiO31.5.1BaTiO3TiCl4ZrOCl2BaZrxTi1-xO3x=0.1TiCl4ZrOCl2LaCl3ClBa(OH)2Bal-5yLayZrxTi1-xO330000[59]0.4atm%(P2O50.14%)11501350XRDSEMTMABaO-TiO2-P2O51112002h96%1150120061005500[60]XRDSEM1.0%208030001%Ta5+BTi4+ABa2+A[61]PTCPTC-1.5.2PTCBaTiO3[62]YF3XRDSEMXRFYF3YF3NYAFOYF3PTCR12PTCRO[63]-BaTiO3TG-DTAXRDFT-IRXRFSEM[64]100Ba1-xSrxYyTi1-yO30≤x≤0.40≤y≤0.1SEMBaTiO39500BaTiO353[65]Eu2O3TiO2BaCO34.0GPa1090Ba1-xEuxTiO3(x=0.10.4)x0.5ABO3Eu2Ti2O7XEuABaEuXX(XPS)Eu3+Eu3+(4f6)Eu