Receiveddate:2011-05-09 收稿日期:2011-05-09 Foundationitem:FundamentalResearchFundsforCentralUniversities(2010MS006);SpecializedResearchFundfortheDoctoralProgramofHigherEducation(20100142120091) 基金项目:中央高校基本科研业务基金资助项目(2010MS006);高等学校博士学科点专项科研基金资助项目(20100142120091) Biography:WANGYunqi(1985-),male,borininHeilongjiangProvince.Mastercandidate.Hisresearchareascoversthepiezoelectricceram-icsanddevices.Correspondentauthor:FANGuifen(1974-),female,borninHubeiProvince,PH.D,associateprofessor.Herre-sarchareascoverstheferroelectricandpiezoelectricceramicsanddevices. 作者简介:王允祺(1985-),男,黑龙江哈尔滨人,硕士生,主要从事压电材料与器件的研究。通信作者:范桂芬(1974-),女,湖北蕲春人,副教授,博士,主要从事铁电、压电陶瓷材料与器件的研究。 文章编号:1004-2474(2011)04-0597-05
EffectsofZnOAdditionontheSinteringTemperatureandPiezoelectric
PropertiesofPSN-PZTCeramic
WANGYunqi1,2,FANGuifen1,2,LVWenzhong1,2
(1.Dept.ofElectronicScienceandTechnology,HuazhongUniversityofScienceandTechnology,Wuhan430074,China;2.KeyLab.ofFunctionalMaterialsForElectronicInformation,MOE,HuazhongUniversityofScienceandTechnology,Wuhan430074,China) Abstract:TheeffectsofZnOadditiononthesinteringtemperatureandpiezoelectricpropertiesofPSN-PZTce-
ramicmodifiedbyBaandFewereinvestigatedinthiswork,inordertodecreasethesinteringtemperatureofPZTpiezoelectricceramic.TherelationshipbetweenthemicrostructureandpropertieswasanalyzedbymeansofXRDandSEM.TheXRDpatternsshowedthatalltheceramicsexhibitedthetetragonalperovskitestructure.Thepiezoe-lectricpropertiesarepromotedwhenZnOcontentislowerthan0.1wt.%.Meanwhile,thespecimenswith0.1wt.%ofZnOadditionalsoexhibitedexcellentpiezoelectricproperties.TheseresultsdemonstratedthatproperZnOadditivecoulddecreasethesinteringtemperatureandenhancethepiezoelectricproperties.Keywords:piezoelectricceramic;lowtemperaturesintering;ZnOaddition
ZnO掺杂对PSN-PZT陶瓷烧结温度及压电性能的影响
王允祺1,2,范桂芬1,2,吕文中1,2
(1.华中科技大学电子科学与技术系,湖北武汉430074;2.华中科技大学电子信息功能材料教育部重点实验室(B类),湖北武汉430074) 摘 要:为了降低PZT压电陶瓷的烧结温度,研究了ZnO掺杂对Ba、Fe改性的PSN-PZT陶瓷的烧结温度和
压电特性的影响。通过XRD和SEM测试手段,分析了微观结构和材料性能的关系。XRD结果显示所有样品均呈现四方钙钛矿结构。在w(ZnO)<0.1%时陶瓷压电性能随ZnO的增加而提高;当w(ZnO)=0.1%时,陶瓷样品同样展现出了优良的压电性能。这些结果证明了适量的ZnO掺杂可以降低陶瓷的烧结温度并提高压电性能。关键词:压电陶瓷;低温烧结;ZnO掺杂中图分类号:TM282 文献标识码:A
0 Introduction
ThePZTceramicsarewidelyusedinvarious
electronicdevicesfortheirexcellentpiezoelectric
anddielectricproperties.Withthedevelopmentofmicro-electronics,themultilayerceramicdevices
havereceivedconsiderableattentionbecauseofthe
widerangeoftheirapplications[1].Thesinteringtemperatureofceramicsisneededtobelowerto
enabletheuseofcheaperelectrodes.Consequent-
ly,extensiveresearchworkshavebeencarriedouttodecreasethesinteringtemperatureofthemater-i
alsuchasusingadvancedsinteringtechnologyand
chemicaldoping.Theadvancedtechnologiessuchashotpressingrequireexpensiveequipmentsand
theproductionvolumeislimited.Bycontrast,the第33卷第4期压 电 与 声 光Vol.33No.42011年8月PIEZOELECTRICS&ACOUSTOOPTICSAug.2011chemicaldopingismuchcheaper.Hence,manyre-searchershavereportedPZT-basedpiezoelectricce-
ramicswithlowsinteringtemperaturebyusing
low-meltingpointmetaloxideadditivesassinteringaid,includingZnO,CuO,Li2CO3,LiBiO2,
Pb5Ge3O11,BiFeO3,etc[2-4].Ontheotherhand,low-
temperaturesinteringcanalsoberealizedbyusing
glassadditives,suchasB-B-iCdglass,Pb-T-iZr-
S-iBiglassetc[5-6].Inthevarioustypesofmultilayerpiezoelectricdevices,piezoelectricmotorshavebeenextensive
studiedfortheapplicationsinmicro-mechanicsandmicro-electronics.Inordertoimprovethedisplace-mentanddecreasetheresponsetimeofthepiezoe-lectricmotors,theceramicsshouldpossessahighelectromechanicalcouplingcoefficient,lowmechan-icalqualityfactorandlowsinteringtemperature.However,itisfoundthatthepiezoelectricceram-
icswithsuchpropertiesareseldomreported.PbSb1/2Nb1/2O3-PZT(PSN-PZT)ceramicmodifiedbyBaandFeisanexcellentsoftpiezoelectricmate-rialwhichexhibitshighelectromechanicalcouplingcoefficientandlowmechanicalqualityfactor,butitssinteringtemperatureishigherthan1200e.Inthispaper,theeffectofZnOadditiononthesinte-ringtemperatureandpiezoelectricpropertiesof
PSN-PZTceramicsmodifiedbyBaandFewasin-vestigated.
1 ExperimentalProcedure
TheceramicswithcompositionsofPb0.97Ba0.03[(Sb0.75Fe0.25)0.5Nb0.5]0.02(Zr0.51Ti0.47)O3(PBFSN-
PZT)+xwt.%ofZnOwerepreparedbyaconven-
tionalmixedoxideprocess,wherexwas0.05,
0.10,0.20,0.30.Thereagentgraderawpowders
ofPb3O4,ZrO2,TiO2,Sb2O3,Nb2O5,Fe2O3,Ba-
CO3,ZnOwereusedasstartingmaterials.These
powdersweremixedbyballmillingfor3h,using
zirconiaballanddeionizedwater.Afterballmil-l
ing,themixturewasdriedandsubsequentlyca-l
cinedat850efor2h.Thecalcinedpowderwas
thenballmilledagainfor3h.Afterdrying,pow-derswereaddedwith5wt.%ofPVAsolutionforgranulation,andthenwerepressedintoplateswithdimensionsof40mm@10mm@1mm.The
pelletsweresinteredat1150efor3h.Theelec-
trodesweremadebypaintingwithsilverpasteandfiringat550efor10min.Thesampleswerepoled
at120einsiliconoilbathbyapplyingaDCelec-
tricfieldof4kV/mmfor15min.Thepiezoelectric
propertiesweremeasuredafter24hofagingatroomtemperature.
Thepiezoelectricconstantd33wasmeasured
usingaquas-istaticd33meter(ZJ-3A,China).Theelectromechanicalcouplingcoefficiencekpandthe
electromechanicalqualityfactorQmwerecalculated
fromtheresonanceandantiresonancefrequencies
usingpreciseimpedanceanalyzer(HP4192,Ang-ilent).Thephasestructureofthesampleswasana-
lyzedbyX-raydiffractionanalysis(RigakuDmax-
rC,Japan).Thefracturedsurfaceswereexaminedbyscanningelectronmicroscopy(FEI-Sirion2000,
Philip,Netherland).Theferroelectricproperties
wereexaminedusingaferroelectrictestingsystem
(ZX-1).Thedielectricpropertiesweremeasuredbyacapacitancemeter(TH2613).Thetemperature
dependenceofthedielectricconstantwasmeasured
bythecapacitancemeterandanautomatictemper-
aturecontroller.
2 ResultsandDiscussions
Fig.1showstheXRDpatternsofPBFSN-PZT
ceramicsaddedwithvariousZnOconcentrations
andsinteredat1150efor3h.Allthespecimensappearacompletesinglephasewithtetragonal
perovskitephase,andnosecondaryphaseisdetec-
Fig.1 XRDpatternsofPBFSN-PZTceramicsaddedwithvariousZnOconcentrationssinteredat1150e 598压 电 与 声 光2011年
