上海大学学报(自然科学版) ›› 2017, Vol. 23 ›› Issue (3): 422-431.doi: 10.12066/j.issn.1007-2861.1857

• 研究论文 • 上一篇    下一篇

水解氧化法制备氧化钇荧光粉及样品荧光性能

王晓旭1, 冯盼盼1, 李倩1, 李瑛2, 胡业旻2   

  1. 1. 上海市质量监督检验技术研究院, 上海 201114; 2. 上海大学材料科学与工程学院, 上海 200444
  • 收稿日期:2016-11-04 出版日期:2017-06-30 发布日期:2017-06-30
  • 通讯作者: 胡业旻(1979—), 男, 副研究员, 博士, 研究方向为纳米材料. E-mail: huyemin@shu.edu.cn
  • 作者简介:胡业旻(1979—), 男, 副研究员, 博士, 研究方向为纳米材料. E-mail: huyemin@shu.edu.cn
  • 基金资助:

    国家质量基础共性技术研究与应用重点专项资助项目(2016YFF0204506)

Synthesis of Y2O3 phosphor power by hydrolysis and oxidation and its fluorescence performance

WANG Xiaoxu1, FENG Panpan1, LI Qian1, LI Ying2, HU Yemin2   

  1. 1. Shanghai Institute of Quality Inspection and Technical Research, Shanghai 201114, China;
    2. School of Materials Science and Engineering, Shanghai University, Shanghai 200444, China
  • Received:2016-11-04 Online:2017-06-30 Published:2017-06-30

摘要:

采用水解氧化法制备Y2O3 稀土材料, 其工艺特点是先将稀土钇与石墨在真空感应炉中熔炼得到碳化钇合金, 再经水解、热处理后即可得到Y2O3 粉末. 采用X射线衍射(X-ray diffration, XRD) 等测试手段对所制备的Y2O3 粉末的组成、微观结构和荧光性能等进行了研究, 得到以下结果: 将碳化钇合金研碎成1 mm 左右的颗粒, 并与去离子水按质量浓度比为1∶20 配置, 将PEG-400 与去离子水按体积比为8∶100 比例配置, 放置于磁力恒温搅拌器上, 在25°C 下搅拌24 h 后抽滤、洗涤, 在80°C 烘箱中烘干后得到Y(OH)3 粉末, 最后经过400~1 000°C热处理后得到Y2O3 粉末. 碳化钇合金水解后得到的Y(OH)3 粉末经过400°C热处理后得到PDF卡片编号为No. 65-3178 的立方晶型Y2O3, 但需要继续加热到800°C 后才具有荧光性能. 由此工艺制得的Y2O3 荧光粉在激发波长为355 nm的氙光照射下, 在430~600 nm 波长范围内分别在468 和578 nm 处有明显的荧光峰出现, 且所发的光为蓝白光. 样品的发光机理是由于C 元素在Y2O3 晶格中形成COOY 和C—OY 这两种结构断裂后, 所引起的光电子耦合所致.

关键词: 水解氧化, 荧光粉, Y2O3

Abstract:

A novel and convenient hydrolysis and oxidation method is used in preparing Y2O3 powders. In this work, yttrium carbide was obtained from yttrium and the graphite by melting in a vacuum melting furnace. Y2O3 powders were prepared with a hydrolysis and oxidation method. The composition, crystal structure, photoluminescence properties, morphology and microstructure of Y2O3 powders were investigated with X-ray diffration(XRD), etc. The following results had been obtained. The triturated alloys sized about 1 mm were introduced into deionized water with 1∶20 mass ratios and PEG-400 and deionized
water with 8∶100 volume ratio under agitation for 24 h at 25°C. After filtering, washing and deionized water drying in a cabinet at 80 °C, and 400~1 000°C heat treatment, Y2O3 powders were obtained. Crystallization peaks appeared around 400°C. These XRD data were entirely consistent with the PDF card No. 65-3178, showing that the samples were cubic Y2O3. When the annealing temperature was raised to 800°C, the sample exhibited fluorescence. The obtained powders showed good bluish-white PL emissions, ranging from 430 to 600 nm, with peaks at 468 and 578 nm, under xenon light excitation. The luminescent mechanism was ascribed to the breakage of C—OY and COOY structures, giving rise to photoluminescence through a strong electron-photon coupling.

Key words: hydrolysis and oxidation, phosphor, Y2O3