4.6 Article

Process methodology for the small scale production of m6N5 purity zinc using a resistance heated vacuum distillation system

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MATERIALS CHEMISTRY AND PHYSICS
卷 122, 期 1, 页码 151-155

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ELSEVIER SCIENCE SA
DOI: 10.1016/j.matchemphys.2010.02.080

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Ultra high purity; Vacuum distillation; High resolution glow discharge mass spectrometry; Micro-hardness; Zinc; Purification

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Ultra high purity Zn (m6N5) was obtained through triple vacuum distillation using an m4N5 Zn as input material. High-volatile impurities were removed from the zinc matrix by vacuum evaporation, while traces having lower volatility than the matrix remained in the residual material after finishing of the entire purification process. The time required for the removal of the main high-volatile impurity (Cd) was monitored using a connected gas source mass spectrometer. During distillation the Zn vapor of the distillate was condensed on the cap of a glassy carbon crucible which was water cooled by a movable copper block. The temperatures were optimized for the removal of the volatiles and for the distillation process using vapor pressure data. High resolution glow discharge mass spectrometry was applied for the analysis and purity evaluation of the distilled and input zinc. The analysis confirmed the reduction of the metallic impurities from 43 mg kg(-1) to 0.5 mg kg(-1) (m6N5) after three consecutive vacuum distillations. An increase in the grain size and a decrease in the micro-hardness were observed for the purified Zn material. (C) 2010 Elsevier B.V. All rights reserved.

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