草酸沉淀法制备大颗粒氧化钇及前驱体的遗传性研究

Genetic study on large-particle yttrium oxide and precursors prepared by oxalic acid precipitation method

  • 摘要: 通过深入探讨草酸沉淀法制备氧化钇及前驱体的遗传性问题,旨在优化制备条件,以获得具有理想粒径分布的氧化钇材料。实验采用高纯氧化钇、盐酸和草酸作为原料,通过精确控制反应条件(氯化钇溶液酸度、草酸浓度、沉淀方式、陈化时间和反应温度等),成功制备了氧化钇及其前驱体。利用激光粒度仪和X射线多晶衍射仪对产物的粒度、形貌和物相进行分析。结果表明,氯化钇浓度0.2 mol/L、酸度2 mol/L、草酸浓度1.5 mol/L、正向沉淀2 h、反应温度80 ℃、陈化6 h是制备大颗粒氧化钇的较优条件。此外,前驱体草酸钇在陈化过程中发生了关键的物相转变,从Y2(C2O43·6H2O变为YH(C2O4)·2H2O,这一变化对煅烧后氧化钇的粒径产生了显著影响。通过优化陈化条件,不仅提高了草酸钇的遗传性,还有效控制了煅烧后氧化钇的粒径,避免其过度减小。从而为制备高性能氧化钇材料提供了有效途径。

     

    Abstract: In this study, the heredity of yttrium oxide precursors prepared by the oxalic acid precipitation method was deeply discussed, aiming at optimizing its preparation process to obtain yttrium oxide materials with ideal particle size distribution. In the experiment, with high-purity yttrium oxide, hydrochloric acid and oxalic acid used as raw materials, yttrium oxide and its precursors were successfully prepared by accurately controlling the reaction conditions (acidity of yttrium chloride solution, oxalic acid concentration, precipitation direction, time and temperature, etc.). The products’ particle size, morphology and phase were analyzed by a laser particle size analyzer and X-ray polycrystalline diffractometer. The results showed that the best conditions for preparing large-particle yttrium oxide were 0.2 mol/L yttrium chloride concentration, 2 mol/L acidity, 1.5 mol/L oxalic acid concentration, forward precipitation for 2 hours, reaction temperature at 80 ℃, and aging for 6 hours. In addition, a key phase transition occurred in the aging process of yttrium oxalate, from Y2 (C2O4) 3 6H2O to YH (C2O4) 2H2O, which had a significant impact on the particle size of yttrium oxide after calcination. By optimizing the aging conditions, the heredity of yttrium oxalate improved, but also the particle size of calcined yttrium oxide was effectively controlled to avoid excessive reduction, which provides an effective way to prepare high-performance yttrium oxide materials.

     

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