基于均相沉淀法制备高纯度球形钌粉

来源期刊:中南大学学报(自然科学版)2020年第2期

论文作者:董海刚 裴洪营 赵家春 吴跃东 保思敏 杨海琼

文章页码:294 - 301

关键词:三氯化钌;离子交换;均相沉淀;前驱体;高纯球形钌粉

Key words:ruthenium trichloride; ion exchange; homogeneous precipitation; precursor; high purity spherical ruthenium powder

摘    要:针对高纯度球形钌粉制备技术难题,基于均相沉淀法制备高纯球形钌粉并分析其过程机理。研究结果表明:三氯化钌溶液经5级离子交换纯化处理后,以尿素为均相沉淀剂,控制钌的质量浓度为10 g/L、尿素与钌的物质的量比为6:1、反应温度为95 ℃、反应时间为4 h,获得球形或类球形钌粉前驱体,经煅烧氢还原、混酸煮洗后,可获得纯度大于99.999%的球形或类球形钌粉。在均相沉淀过程中,尿素缓慢水解生成的OH-均匀分布在溶液中,与钌络合离子反应,生成球形钌粉前驱体,煅烧后得到球形钌粉。

Abstract: In view of the difficulty in preparing high purity spherical ruthenium powder, homogeneous precipitation method was used to prepare high purity spherical ruthenium powder and its mechanism was analyzed. The results show that when the ruthenium trichloride solution is treated by 5-level ion exchange purification, with urea being the homogeneous precipitating agent, ruthenium mass concentration of 10 g/L, molar ratio of urea to ruthenium 6:1, reaction temperature 95 ℃, and reaction time 4 h, a spherical ruthenium powder precursor is obtained. Subsequently, a spherical ruthenium powder with 99.999% purity is obtained by calcination followed by hydrogen reduction and mixed acid washing. In the homogeneous precipitation process, OH- ions generated from the slow hydrolysis of urea distribute uniformly in the solution, and react with ruthenium complex ion to form a ruthenium powder precursor. In the process of calcination, the high purity spherical ruthenium powder is obtained.

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