碳酸盐沉淀法制备纳米Y_(2)O_(3)粉体研究

Preparation of Nanometer Y_(2)O_(3) Powder by Carbonate Precipitation Method

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).