络合作用对Sol-gel法制备Er^(3+)掺杂TiO_2粉末光致发光特性影响  

Effect of Chelation on PL Properties of Er^(3+)-doped TiO_2 Powders Prepared by Sol-gel Method

作　　者：白凌云[1,2] 苏显云[1] 雷明凯[2] 

机构地区：[1]大连理工大学化工学院化学系 [2]大连理工大学材料科学与工程学院表面工程研究室,大连116024

出　　处：《无机材料学报》2006年第5期1085-1091,共7页Journal of Inorganic Materials

基　　金：教育部科学研究重点项目(01052)

摘　　要：以钛酸正丁酯为前驱体,乙酰丙酮为络合剂,分别在室温和70℃进行对前驱体改性的络合反应,获得改性前驱体Ti(O-Bu)4-x(AcAc)x．以异丙醇为溶剂,采用溶胶-凝胶(sol-gel)法制备0．1-3．0mol％Er3+掺杂TiO2粉末．差热-热重(TG-DTA)分析结果表明,由室温络合改性前驱体制备的粉末,无定型到锐钛矿和锐钛矿到金红石的相变温度,较由70℃络合改性前驱体制备的粉末均升高40℃．X射线衍射(XRD)分析表明,700℃烧结,室温络合所得掺0．1-3．0mol％Er3+:TiO2粉末为单一锐钛矿结构,70℃络合所得粉末为锐钛矿和少量金红石的混合相结构．400-800℃烧结,两种络合所得粉末均获得中心波长为1．53μm的多峰结构光致发光(PL)谱．其中,700℃烧结的粉末PL强度最强．70℃络合较室温络合的粉末PL强度可提高3倍．0.1-3.0mo1% Er^3＋-doped TiO2 powders were prepared by the sol-gel method using the modified titanium （Ⅳ） n-butoxide [Ti（O-Bu）4-x（AcAc）x] as the precursor which is prepared by chelating reaction between Ti（O-Bu）4 and acetylacetone （AcAc） at room temperature and 70℃, respectively. The preparation was performed by using iso-propyl （i-PrOH） as solvent with the addition of hydrated erbium nitrated [Er（NO3）3·5H2O]. When the temperature of the chelating reaction increased from room temperature to 70℃, both phase transformation temperatures of 1mol% Er^3＋-doped TiO2 xerogels from amorphous to anatase and anatase to futile were decreased about 40℃. XRD analysis showed that, sintered at 700℃ the phase structure for the TiO2 powders prepared by using Ti（O-Bu）4-x（AcAc）x chelated at room temperature is anatase, while that for the TiO2 powders chelated at 70℃ is the mixture of anatase and futile in small amount. The photoluminescence （PL） spectra centered at about 1.53μm with the form of multi-peak were obtained for the powders by chelating at the two temperature sintered in the temperature range of 400-800℃. For 1mol% Er^3＋-doped TiO2 powders sintered at 700℃, the PL peak intensity at 1.53μm increased by a factor of 3 with increasing the chelating reaction temperature to 70℃.

关 键 词：SOL-GEL法 TIO2 光致发光 络合改性 

分 类 号：O648[理学—物理化学] TQ133[理学—化学]