含钌废料直接制备溅射靶材用高纯钌粉的研究
发布时间：2018-10-18 18:13
【摘要】：目前我国靶材用钌粉依赖进口,成本高,含钌废料直接制备靶材用高纯钌粉具有十分重要的现实意义。论文针对含钌废料的特点,提出了采用碱熔-水浸-氧化蒸馏-离子交换除杂-沉淀-煅烧还原工艺直接制备溅射靶材用高纯钌粉的研究。本论文取得结论如下:(1)钌废料碱熔-水浸研究表明,在Na_2O_2+NaOH为熔剂、碱熔温度750°C、Na_2O_2、NaOH及钌废料质量比为4:3:1、碱熔时间3h、水浸温度95℃、水浸时间4h的条件下,钌的浸出率达到97%,获得含钌溶液。(2)含钌溶液氧化蒸馏研究表明,采用硫酸为介质体系,以氯酸钠为氧化剂进行氧化蒸馏,钌被氧化为四氧化钌挥发,并用盐酸吸收液吸收,达到初步除杂的目的,获得氯钌酸溶液。在蒸馏温度95℃、蒸馏负压0.08MPa的条件下,钌的直收率达到94.4%。(3)离子交换除杂研究表明,实验中选择D001与001×7为交换树脂,溶液酸度为0.5mol/L(以H~+浓度计),溶液流速为2m L/min,交换级数为11级,净化后氯钌酸溶液中杂质含量均低于0.0005g/L。(4)氯化铵沉淀研究表明,加入氧化剂将钌全部转化为氯钌(IV)酸铵,达到进一步除杂的目的;同时通过严格控制沉淀条件,制备出颗粒均匀、尺寸合适及分散性良好的颗粒。最佳工艺条件为:钌酸盐的浓度为30g/L,沉淀过程中持续滴加氧化剂,氯化铵的加入方式为饱和溶液,温度为90℃,反应过程中持续搅拌。(5)煅烧-还原、混酸煮洗的研究表明,煅烧过程通入氮气煅烧,氢气还原的方式可将氯钌酸铵颗粒还原为形貌规整、尺寸均一的钌粉;用酸煮的方式进一步深度除杂,钌粉纯度可达99.995%。最佳工艺条件为:煅烧温度500℃、煅烧时间2小时、还原温度700℃、还原时间2小时。通过研究,确立了含钌废料直接制备高纯钌粉的工艺流程和参数,该工艺原料适应性强,钌的回收率较高,制备出的钌粉粒度均一、形貌规整、纯度较高。
[Abstract]:At present, ruthenium powder used for target in our country depends on import and its cost is high. It is very important to produce high purity ruthenium powder with ruthenium waste material. According to the characteristics of ruthenium waste material, the preparation of high purity ruthenium powder for sputtering target by alkali melting, water immersion, oxidation distillation, ion exchange removal, precipitation and calcination reduction process was studied in this paper. The conclusions obtained in this paper are as follows: (1) the results of alkaline melting and water leaching of ruthenium waste show that under the conditions of Na_2O_2 NaOH as flux, alkali melting temperature 750 掳C ~ (2 +) Na _ 2O _ 2 NaOH and the mass ratio of ruthenium waste 4: 3: 1, alkali melting time 3 h, leaching temperature 95 鈩，
本文编号：2279963
[Abstract]:At present, ruthenium powder used for target in our country depends on import and its cost is high. It is very important to produce high purity ruthenium powder with ruthenium waste material. According to the characteristics of ruthenium waste material, the preparation of high purity ruthenium powder for sputtering target by alkali melting, water immersion, oxidation distillation, ion exchange removal, precipitation and calcination reduction process was studied in this paper. The conclusions obtained in this paper are as follows: (1) the results of alkaline melting and water leaching of ruthenium waste show that under the conditions of Na_2O_2 NaOH as flux, alkali melting temperature 750 掳C ~ (2 +) Na _ 2O _ 2 NaOH and the mass ratio of ruthenium waste 4: 3: 1, alkali melting time 3 h, leaching temperature 95 鈩，
本文编号：2279963
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