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无机材料学报

无机材料学报

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水热合成法制备锐钛矿型纳米TiO2粉体的研究

冉凡勇, 曹文斌, 李艳红, 张小宁   

  1. 北京科技大学材料科学与工程学院无机非金属材料系, 北京 100083
  • 收稿日期:2005-05-13 修回日期:2005-07-08 出版日期:2006-05-20 网络出版日期:2006-05-20

Preparation of Anatase Nano-TiO2 Powders by Hydrothermal Synthesis

RAN Fan-Yong, CAO Wen-Bin, LI Yan-Hong, ZHANG Xiao-Ning   

  1. Department of Inorganic Nonmetallic Materials, School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083, China
  • Received:2005-05-13 Revised:2005-07-08 Published:2006-05-20 Online:2006-05-20

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摘要： 以工业硫酸氧钛为原料, 尿素作沉淀剂, 固定6MPa的初始压力和300r/min的搅拌速度, 在110～150℃的反应温度、2～8h的反应时间、0.25～1.5mol/L的硫酸氧钛反应浓度的条件下, 采用水热合成法制备了锐钛矿型纳米TiO2粉体. 采用XRD、TEM、BET等测试手段对在不同条件下所制备粉体的物相组成、晶粒度、比表面积等进行了分析. 结果表明, 所制备的粉体均为锐钛矿型纳米TiO2. 粉体的比表面积分布在124～240m2/g、晶粒度分布在6.7～10.6nm. 随着反应温度的升高和反应时间的延长, 晶粒度增大, 比表面积降低. 随前驱体浓度的提高, 晶粒度也增大, 当前驱体浓度<0.5mol/L时, 比表面积随着前驱体浓度的增大而增大. 当前驱体浓度>0.5mol/L时, 比表面积随着前驱体浓度的增大而减少.

关键词: 水热法, 纳米TiO2, 锐钛矿, TiOSO4

Abstract: By using technical grade TiOSO4 as the precursor and urea as the precipitating agent, nano-crystalline anatase TiO2 powders were prepared by hydrothermal synthesis. The initial pressure of the system was 6MPa. Stirring speed was fixed at 300r/min. Reaction temperature was ranged from 110℃ to 150℃ with holding time from 2h to 8h and the concentration of the precursor was ranged from
0.25～1.5mol/L. The grain size, phase composition and specific surface area of the synthesized powders were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM) and BET methods. XRD results show that the synthesized powders are all anatase. Calculated grain size is from 6.7 to 10.6nm by Scherrer method. The specific surface area of the powders is ranged from 124 to 240m2/g. The grain size of the powders increases with the increase of the reaction temperature, holding time and precursor concentration. When the precursor concentration is more than 0.5mol/L, the specific surface area decreases with the increase of holding temperature, holding time and precursor
concentration. When the precursor concentration is less than 0.5mol/L, the
specific surface area increases with the increase of precursor concentration.

Key words: hydrothermal synthesis, nano-TiO2, anatase, TiOSO4

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