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化学学报
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化学学报 ›› 2010, Vol. 68 ›› Issue (23): 2409-2413. 上一篇    下一篇

研究论文

化学沉淀法制备BaTiO3纳米粉体的研究

陈妍妍，张云*，王晓燕   

  1. (四川大学材料科学与工程学院 成都 610064)
  • 投稿日期:2009-09-25 修回日期:2010-04-14 发布日期:2010-08-02
  • 通讯作者: 张云 E-mail:y_zhang@scu.edu.cn

Research on Preparation of Nanosized Barium Titanate by Chemical Precipitation

CHEN Yan-Yan, ZHANG Yun, WANG Xiao-Yan   

  1. (College of Material Science and Engineering, Sichuan University, Chengdu 610064)
  • Received:2009-09-25 Revised:2010-04-14 Published:2010-08-02
  • Contact: ZHANG Yun E-mail:y_zhang@scu.edu.cn

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以正钛酸(H4TiO4)、硝酸钡[Ba(NO3)2]为原料, 以双氧水、氨水为溶剂, 采用化学沉淀法制备出晶粒尺寸约20 nm的钛酸钡粉体. 研究了原料种类、煅烧温度、加料方式、反应温度对钛酸钡粉体性能的影响, 确定了最佳的制备条件. 结果表明: 当正钛酸(g)∶双氧水(mL)∶氨水(mL)＝1∶5∶3, 且采用正钛酸的双氧水-氨水溶液缓慢滴加到硝酸钡溶液中的加料方式时, 溶解完全, 制得的BaTiO3粉体粒径小、纯度高. 用X射线衍射(XRD)和扫描电子显微镜(SEM)表征了颗粒的晶体结构、晶型转变机理以及颗粒的形貌|结果显示: 前驱体的起始晶型转变温度为500, 800 ℃煅烧获得的粒子晶型完整, 形貌呈规则的球形, 当煅烧温度升高到900 ℃时, 粉体晶体结构由立方相转变为四方相.

关键词: BaTiO3纳米粉体, 正钛酸, 煅烧温度, 化学沉淀法

Nanosized BaTiO3 powders with crystallite size about 20 nm were synthesized by chemical precipitation, in which, Titanic acid (H4TiO4) and barium nitrate [Ba(NO3)2] were used as the raw materials, and hydrogen peroxide (H2O2) and ammonia (NH3•H2O) were used as solvents. The influences of species of raw materials, calcination temperatures, feeding sequence, reaction temperatures on BaTiO3 were studied in detail. The results show that the good dissolution properties, the small particle size and high purity of BaTiO3 could be obtained at the conditions of H4TiO4 (g)∶H2O2 (mL)∶NH3•H2O (mL)＝1∶5∶3 and adding the solution of H4TiO4 dissolved in H2O2 and NH3•H2O into Ba(NO3)2 aqueous solution slowly. Moreover, the crystal structure, crystallization transfer mechanism, and crystallite size were researched by X-ray diffraction (XRD) and scanning electron microscope (SEM). The results show that the beginning crystallization temperature of barium titanate is approximately 500 ℃ and the particles obtained at 800 ℃ exhibited integral crystal structure and spherical morphology. However, the crystal structure of BaTiO3 obtained at 900 ℃ was changed from cubic into tetragonal phase.

Key words: nanosized BaTiO3 powders, titanic acid, calcination temperature, chemical precipitation