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钌的精炼过程分为钌盐的精制和高纯钌的制取两个步骤。本文以氧化还原标准电极电位作为选择性氧化分离锇、钌的判据,从理论上分析了采用二段分步氧化蒸馏分离锇、钌的必要性和可行性。研究了氧化-真空蒸馏方法从一次钌盐酸吸收液中,一段氧化加入H_2O_2选择性氧化-真空蒸馏分离锇,使钌盐酸溶液中的锇被选择氧化而以OsO_4气体单独蒸馏出来并被NaOH溶液吸收,而未氧化的钌则留在蒸馏余液中;之后在分离锇后的一次钌盐酸蒸馏余液中,二段氧化加入H_2SO_4+NaClO_3进行氧化-真空蒸馏分离钌和残留的锇。氧化蒸馏出的RuO_4经HCl吸收并还原得到精制的二次钌盐酸溶液,进一步经硫化钠结晶沉淀提纯制得高纯硫化钌盐,并对沉钌过程做了初步的理论分析。所得精制硫化钌沉淀物在氢气氛围下煅烧还原制得高纯海绵钌,海绵钌经王水与氢氟酸混合酸煮洗后水洗,在氢气氛围下干燥后制得的钌粉经辉光放电质谱法(GDMS)分析,纯度达到4N5(99.995%)以上,可直接用于溅射靶材。本研究为靶材用5N(99.999%)高纯钌粉的制备及其工业化生产提供了理论和实验依据。
The ruthenium refining process is divided into ruthenium salt purification and high purity ruthenium preparation two steps. In this paper, the potential of redox standard electrode was used as the criterion for selective oxidation of osmium and ruthenium, and the necessity and feasibility of separation of osmium and ruthenium by two-stage fractional oxidation distillation was theoretically analyzed. The oxidation-vacuum distillation method was used to separate osmium from the ruthenium hydrochloric acid absorption solution by adding H 2 O 2 selective oxidation-vacuum distillation to ruthenium hydrochloride solution. The osmium in the ruthenium hydrochloride solution was selectively oxidized and was separated by the OsO 4 gas and absorbed by the NaOH solution , While the unoxidized ruthenium remains in the distillate; after that, the ruthenium and hydrochloric acid remain after the separation of osmium is oxidized and vacuum distilled to separate ruthenium and residual osmium by the second stage oxidation by adding H 2 SO 4 + NaClO 3. RuO_4 oxidized and distilled off was recovered by HCl and reduced to obtain a purified solution of ruthenium dihydrochloride. The purified ruthenium salt was further purified by sodium sulphide crystallization and precipitation, and a preliminary theoretical analysis of the ruthenium deposition process was made. The resulting purified ruthenium sulfide precipitate calcined in a hydrogen atmosphere to obtain high purity sponge ruthenium, sponge ruthenium by aqua regia and hydrofluoric acid mixed acid boiled water washed, dried in a hydrogen atmosphere after the resulting ruthenium powder glow discharge Mass spectrometry (GDMS) analysis, the purity of 4N5 (99.995%) above, can be directly used for sputtering target. This study provides a theoretical and experimental basis for the preparation of target 5N (99.999%) high purity ruthenium powder and its industrial production.