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由煤矸石真空动态闪速还原-惰性气体冷凝法制备 GeAs 超细颗粒

One-Pot Synthesis of GeAs Ultrafine Particles from Coal Fly Ash by Vacuum Dynamic Flash Reduction and Inert Gas Condensation.

机构信息

School of Environmental Science and Engineering, Shanghai Jiao Tong University, 800 Dongchuan Road, Shanghai, 200240, People's Republic of China.

出版信息

Sci Rep. 2017 Jun 16;7(1):3641. doi: 10.1038/s41598-017-03398-1.

Abstract

Ge-monopnictides (GeAs) plays critical role in high-tech industry, especially in the field of advanced optical devices and infrared. As a secondary material, coal fly ash could be further recycled to retrieve germanium and prepare GeAs material with high added values. Hence, the aim of this paper is to propose a one-pot synthesis that uses vacuum flash reduction and inert-gas consolidation method to prepare GeAs ultrafine particles. Germanium in coal fly ash can be successfully recycled; simultaneously, GeAs ultrafine particles were prepared. Separation principle and feasibility of this process was discussed. Temperature, carrier gas flow rate and system pressure were the major factors on formation, morphology and distribution of particle size of GeAs ultrafine particles. A three steps synthetic mechanism was clarified, namely, thermal rupture of coal fly ash and release of GeO and AsO, the gas-solid phase reaction of GeO, AsO and coke to generate metallic Ge and As in vacuum flash reduction. Meantime, GeAs were produced in the gas phase reaction. Finally, GeAs ultrafine particles were obtained by carrier gas condensation. In short, this research developed a practical and environment-friendly one-pot synthesis to recycle germanium in coal fly ash and prepare GeAs ultrafine particles with high added values.

摘要

锗-单卤化物(GeAs)在高科技产业中起着关键作用,特别是在先进的光学器件和红外领域。作为一种二次材料,粉煤灰可以进一步回收锗,并制备具有高附加值的 GeAs 材料。因此,本文旨在提出一种使用真空闪蒸还原和惰性气体固结法制备 GeAs 超细颗粒的一锅合成法。粉煤灰中的锗可以得到成功回收,同时制备出 GeAs 超细颗粒。讨论了该工艺的分离原理和可行性。温度、载气流速和系统压力是影响 GeAs 超细颗粒形成、形貌和粒径分布的主要因素。阐明了一个三步合成机制,即在真空闪蒸还原中,粉煤灰的热破裂和 GeO 和 AsO 的释放,GeO、AsO 和焦炭的气-固相间反应生成金属 Ge 和 As,同时,在气相反应中生成 GeAs。最后,通过载气冷凝得到 GeAs 超细颗粒。总之,本研究开发了一种实用且环保的一锅合成法,用于回收粉煤灰中的锗,并制备具有高附加值的 GeAs 超细颗粒。

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