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柠檬酸盐溶胶-凝胶法制备Ba3(Ca1.18Nb1.82)O9-δ纳米粉末

宿新泰; 刘瑞泉; 胡云霞; 谢娅红; 王吉德   

  1. 新疆大学化学化工学院 乌鲁木齐 830046
  • 收稿日期:2002-11-11 修回日期:2002-12-16 出版日期:2004-01-20 网络出版日期:2004-01-20

Preparation of Nanocrystalline Ba3(Ca1.18Nb1.82)O9-δ Powder by UsingCitrate Sol-Gel Method

SU Xin-Tai; LIU Rui-Quan; HU Yun-Xia; XIE Ya-Hong; WANG Ji-De   

  1. College of Chemistry & Chemical Engineering; Xinjiang University; Urumqi 830046; China
  • Received:2002-11-11 Revised:2002-12-16 Published:2004-01-20 Online:2004-01-20

摘要: 用一种新型湿化学方法,从含Ba、Ca、Nb的柠檬酸络合物溶液中合成了Ba3(Ca1.18Nb1.82)O9-δ(BCN18)粉末.加热含Ba:Ca:Nb:citrtc acid=3∶1.18∶1.82∶12的溶液,得到浅绿色溶胶,继续干燥得到黄色干凝胶,随后将干凝胶进行焙烧得到粉体.对干凝胶进行了TG-DTA分析,粉体进行了XRD,TEM表征.实验结果表明,该方法制备BCN18粉体所需温度为750℃,平均粒径为50nm,成相温度为1000℃,比传统固相反应法合成温度降低600℃左右.该方法比目前报道的醇盐系湿化学方法具有更实用、更优越的性质.

关键词: Ba3(Ca1.18Nb1.82)O9-δ(BCN18), 溶胶-凝胶法, 高温质子导体, 复合钙钛矿

Abstract: Ba3(Ca1.18Nb1.82)O9-δ(BCN18) powders were synthesized by using a wet chemical method from a mixture of all
water-soluble compounds including Ba, Ca and Nb-citrate. Heating a mixed aqueous solution with the molar ratio of Ba:Ca:Nb:citric acid=3:1.18:1.82:12
produced a light green gelatinous viscous matter without any precipitation, then evaporating, drying and calcinating were conducted. The obtained gels
were characterized by TG-DTA, XRD and TEM. The experimental results show that the heating temperature is 750℃ for getting the powder and
the average particle size is about 50nm. Furthermore a pure BCN18 phase with a complex perovskite structure forms at 1000℃,it is lower about
600℃ than that reported by using the traditional solid-reaction method. The citrate sol-gel method is more practical and ascendant than the wet-chemical method used to the alcohol salt system reported in present literature.

Key words: Ba3(Ca1.18Nb1.82)O9-δ(BCN18), sol-gel method, high temperature proton conductors, complex perovskite

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