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无机材料学报

无机材料学报

• 研究论文 • 上一篇    下一篇

络合作用对Sol-gel法制备Er3+掺杂TiO2粉末光致发光特性影响

白凌云1,2, 苏显云1, 雷明凯2   

  1. 1. 大连理工大学化工学院化学系, 大连 116024; 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

  • 收稿日期:2005-11-04 修回日期:2006-02-27 出版日期:2006-09-20 网络出版日期:2006-09-20

Effect of Chelation on PL Properties of Er3+-doped TiO2 Powders Prepared by Sol-gel Method

BAI Ling-Yun 1,2, SU Xian-Yun1, LEI Ming-Kai2   

  1. 1. Department of Chemistry, School of Chemical Engineering, Dalian University of Technology, Dalian 116024, China; 2. Surface Engineering Laboratory, School of Materials Science and Engineering, Dalian University of Technology, Dalian 116024, China

  • Received:2005-11-04 Revised:2006-02-27 Published:2006-09-20 Online:2006-09-20

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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°C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% Er 3+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°C络合改性前驱体制备的粉末均升高40°C. X射线衍射(XRD)分析表明, 700°C烧结, 室温络合所得掺0.1~3.0mol% Er 3+:TiO2粉末为单一锐钛矿结构, 70°C络合所得粉末为锐钛矿和少量金红石的混合相结构. 400~800°C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°C烧结的粉末PL强度最强. 70°C络合较室温络合的粉末PL强度可提高3倍.

关键词: Sol-gel法, TiO2, 光致发光, 络合改性

Abstract:

0.1-3.0mol% 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°C, 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 70C, both phase transformation temperatures of 1mol% Er3+-doped TiO2 xerogels from amorphous to anatase and anatase to rutile were decreased about 40C. XRD analysis showed that, sintered at 700C 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°C is the mixture of anatase and rutile in small amount. The photoluminescence (PL) spectra centered at about 1.53nm with the form of multi-peak were obtained forthe powders by chelating at the two temperature sintered in the temperature range of 400°C. For 1mol% Er 3+ -doped TiO2 powders sintered at 700°C, the PL peak intensity at 1.53μm increased by a factor of 3 with increasing the chelating reaction temperature to 70°C.

Key words: sol-gel method, TiO2, photoluminescence, chelating reaction

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