BCl3の亜鉛還元により生成したボロンの純度および結晶性について

伊藤 尚, 柳ケ瀬 勉, 東 敬

doi:10.2473/shigentosozai1953.78.891_667

By reducing gaseous BCl₃ with zinc, boron was prepared with the yield of 75-87%, but uhe resulted boron always contains substantial amount of zinc together with a little silicon. The zinc in boron could be vaporized and removed by treating the crude boron at high temperature in vacuum.As the effective removal of silicon could not be expected in this vacuum heating, it is necessary to prevent silicon from coming into boron throughout a whole operation. Silicon may be formed according to the following reaction. 2SiO₂+4BCl₃→2B₂O₃+3SiCl₄ SiCl₄+2Zn→Si+2ZnCl₂ The former reaction suggests that BCl₃ may attack quartz tube used as a part of apperatus.Since the rate of the attack is considered to decrease at lower temperature, the silicon contamination in boron could be reduced by preparing at the temperature lower than 800°C. The boron obtained by reducing gaseous BCl₃ with zinc at 750°C and then subjecting to vacuum heat treatment at 1100°C for 2 hours showed the purity, of 99.2%. X-ray diffraction studies indicate that the boron obtained in vapor phase is amorphous, but the crystalization seems to occur when it is heated in vacuum at 1000°-1250°C.

BCl<SUB>3</SUB>の亜鉛還元により生成したボロンの純度および結晶性について

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