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作 者:陈金清[1] 丘丽莉 张魁芳 袁祥奕 饶帅 刘志强 Chen Jinqing;Qiu Lili;Zhang Kuifang;Yuan Xiangyi;Rao Shuai;Liu Zhiqiang(Faculty of Materials Metallurgical Chemistry,Jiangxi University of Science and Technology;Institute of Resources Utilization and Rare Earth Exploitation,Guangdong Academy of Sciences)
机构地区:[1]江西理工大学材料冶金化学学部,江西赣州341000 [2]广东省科学院资源利用与稀土开发研究所,广东广州510006
出 处:《中国稀土学报》2022年第5期815-826,共12页Journal of the Chinese Society of Rare Earths
基 金:国家自然科学基金项目(52074094);广东省基础与应用基础研究基金项目(2019A1515012173,2021A1515012268);梅州市科技计划项目(2019A0102003)资助。
摘 要:探索了以YCl_(3)为原料,碳酸盐为沉淀剂,采用沉淀法制备纳米Y_(2)O_(3)粉体的工艺条件。实验研究了加料方式、Y^(3+)浓度、沉淀剂浓度、沉淀剂与YCl_(3)摩尔比、搅拌速度、反应温度、反应时间、表面活性剂和沉淀剂组成等条件对Y_(2)O_(3)粉体的影响,并且对Y_(2)O_(3)前驱体组成和分解过程进行了探索。结果表明:采用正加料方式,以体积分数10%Na_(2)CO_(3)和90%NaHCO_(3)混合为沉淀剂,在反应温度30℃,搅拌速度300 r·min^(-1),加料速度10 mL·min^(-1)等较优条件下得到D_(50)=0.0603μm,比表面积为17.2707 m^(2)·g^(-1),分散性良好的纳米Y_(2)O_(3)粉体。通过综合热分析仪、红外光谱测试仪等对前驱体进行表征分析,前驱体组成为Y(OH)CO_(3)·H_(2)O,其热分解反应过程如下:Y(OH)CO_(3)·H_(2)O→Y(OH)CO_(3)+H_(2)O,Y(OH)CO_(3)→(1/2)Y_(2)O_(3)+(1/2)H_(2)O+CO_(2)。The nanometer yttrium oxide powder was prepared by precipitation method with yttrium chloride as raw material and carbonate as precipitator.The effects of feeding mode,Y^(3+)concentration,precipitator concentration,molar ratio of precipitator to yttrium chloride,stirring speed,reaction temperature,reaction time,composition of surfactant and precipitator on the precursor of yttrium oxide were studied.The results show that:The nanometer Y_(2)O_(3) with D_(50)=0.0603μm,specific surface area of 17.2707 m^(2)·g^(-1) and good dispersion was obtained by positive feeding method with 10%sodium carbonate and 90%sodium bicarbonate mixed as precipitator under the optimal conditions of reaction temperature of 30℃,stirring speed of 300 r·min^(-1) and feeding rate of 10 mL·min^(-1).The precursor was characterized and analyzed by comprehensive thermal analyzer and infrared spectrometer,etc.The composition of the precursor was Y(OH)CO_(3)·H_(2)O,and the thermal decomposition reaction process was as follows:Y(OH)CO_(3)·H_(2)O→Y(OH)CO_(3)+H_(2)O,Y(OH)CO_(3)→1/2Y_(2)O_(3)+1/2H_(2)O+CO_(2).
关 键 词:沉淀法 碳酸盐 纳米Y_(2)O_(3)
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