化学学报 ›› 2004, Vol. 62 ›› Issue (18): 1845-1848. 上一篇    下一篇

研究简报

湿化学法制备纳米氧化镱的研究

赵玉宝, 黄传敬, 陈陆千, 翁维正, 万惠霖   

  1. 厦门大学化学系, 物理化学研究所, 固体表面物理化学国家重点实验室, 厦门, 361005
  • 投稿日期:2004-04-14 修回日期:2002-06-17 发布日期:2014-02-17
  • 通讯作者: 赵玉宝,E-mail:yb_zhao2001@yahoo.com;万惠霖,E-mail:hlwan@xmu.edu.cn;Tel:0592-2182440 E-mail:yb_zhao2001@yahoo.com;hlwan@xmu.edu.cn
  • 基金资助:
    国家重点基础研究发展规划(No.G1999022408)和国家自然科学基金(Nos.20023001,20021002)资助项目.

Preparation of Nanoscale Ytterbia by Wet Chemical Methods

ZHAO Yu-Bao, HUANG Chuan-Jing, CHEN Lu-Qian, WENG Wei-Zheng, WAN Hui-Lin   

  1. State Key Laboratory for Physical Chemistry of Solid Surfaces, Department of Chemistry and Institute of Physical Chemistry, Xiamen University, Xiamen 361005
  • Received:2004-04-14 Revised:2002-06-17 Published:2014-02-17

采用通常的溶液沉淀、微乳液及均匀沉淀等溶液方法制备纳米氧化镱.TEM观测显示,采用H2O2的溶液沉淀法和采用CTAB的均匀沉淀法,都可得到有较好分散、尺度约为10 nm的球形粒子;XRD分析表明,经650℃焙烧后的氧化镱均为立方结构,采用H2O2的溶液沉淀法所得氧化镱的晶粒尺寸为9.4 nm,采用CTAB的均匀沉淀法所得氧化镱的晶粒尺寸为6.9 nm;基于低温N2吸附表征结果发现,微乳液法制得的Yb2O3的比表面积较低,采用H2O2的溶液沉淀法可以制得比表面积为47.7m2/g、等效粒径为13.6 nm的Yb2O3,采用CTAB的均匀沉淀法所得氧化镱比表面积为63.2m2/g,等效粒径为10.3 nm.表面活性剂与水合氧化镱沉淀物间的相互作用,可能对所得氧化镱的热稳定性有重要影响.

关键词: 氧化镱, 纳米晶, 高比表面, 湿化学法, 溶液沉淀, 均匀沉淀

Several wet chemical methods, such as conventional precipitation, microemulsion route and homogeneous precipitation, have been used to prepare nanosized ytterbium oxides. After being calcined at 650℃, well-dispersed spherical particles with size of about 10 nm characterized by TEM observations can be prepared by hydrogen peroxide- or CTAB-aided precipitation process. XRD results show that the as-prepared samples are cubic ytterbium oxides with the crystal sizes of 9.4 nm for hydrogen peroxide-aided way and 6.9 nm for CTAB-containing route. Nitrogen adsorption characterization at 77 K indicates that (i) the present microemulsion process gives a sample with the lowest specific surface area compared with other methods, (ii) ytterbium oxides with specific surface areas of 47.7 m2/g (equivalent diameter of 13.6 nm) and 63.2 m2/g (equivalent diameter of 10.3 nm) can be prepared by hydrogen peroxide-aided way and CTAB-containing homogeneous precipitation process, respectively. The interaction between the surfactants and the hydrous ytterbia may play an important role in the thermal stability of the derived Yb2O3.

Key words: ytterbia, ytterbium oxide, nanocrystal, high specific surface area, wet chemical method, conventional precipitation, homogeneous precipitation