降低高纯锑中Na、Si杂质含量工艺研究

Research on Reducing the Content of Na and Si Impurities in High Purity Antimony

工业锑经过氯化、精馏、三氯化锑氢气还原、真空蒸馏制备的7N高纯锑中Na、Si杂质元素含量不稳定,通过高纯锑拉晶提纯工艺、氢化工艺研究,控制直拉温度670℃±5℃,直拉速度12 mm/h,可进一步降低杂质Si元素含量至<0.005ppm;控制氢化温度820℃±5℃,氢化时间12 h,可进一步降低杂质Na元素含量至<0.00 5ppm。

The content of Na and Si impurities in 7N high-purity antimony produced by chlorination, rectification, hydrogen reduction of antimony trichloride and vacuum distillation are unstable.Via the study of Czochralski purification process and hydrogenation process, the content of Si can be further reduced to < 0.005 ppm by controlling the Czochralski temperature at 670 ℃±5 ℃ and the Czochralski speed at 12mm/h;the content of Na can be further reduced to < 0.005ppm by controlling the hydrogenation temperature at 820 ℃±5 ℃ and the hydrogenation time at 12h.