Production method for high-purity arsenic and its equipment

Abstract

The invention discloses a manufacturing method and specific equipment of semiconductor basic material hyperhigh-purity alpha-typed arsenic with purify at 99.99999% through once vacuum sublimation and twice hydrogen sublimations, which consists of vacuum sublimator and hydrogen sublimator, wherein the vacuum sublimator contains heater A, heater B, vacuum tank, water jacket, copple, obstruct board, conical titanium condenser, low-boiling collecting board and vacuum pump; the hydrogen sublimator includes hydrogen input device, argon input device, casing, quartz tube A, quartz tube B, quartz tube C, heater, scrubbing device and spray device.

Description

technical field [0001] The invention relates to a production method and equipment for the purification of non-metallic materials, in particular to a production method and special equipment for ultra-high-purity alpha-arsenic as a basic semiconductor material. Background technique [0002] High-purity α-arsenic is an essential material for the preparation of optoelectronic and microelectronic gallium arsenide; infrared optical fiber, infrared lens As2Se3, As2Te3 and other infrared see-through glasses; photosensitive tympanic membrane As-Se alloy. The higher the characteristic characteristics, the more the application value of the material can be brought into play. The popularization of gallium arsenide based on high-purity α-type arsenic, infrared see-through glass and arsenic-containing alloys for the electronics industry has caused the demand for high-purity arsenic to increase by 25%-30% per year. % speed increments. [0003] At present, the production method of high-puri...

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Problems solved by technology

Its disadvantages: ① Arsenic trichloride is a strong corrosive and strong oxidant, and only quartz glass can resist the corrosion of arsenic trichloride as the material for making the arsenic trichloride rectification tower. Internationally, it is an investment to build a rectification tower with an annual output of 20 tons No less than 25 million US dollars (only Germany can process such a quartz tower, Furukawa, Japan's 20-ton annual rectification tower is made in Germany, with an investment of 25 million US dollars). Due to the limitation of quartz processing level in China, all manufacturers use φ10 wall A small tower with a thickness of about 5mm has low production capacity, easy damage to the tower, high overall product cost, and unstable product quality; There are a large amount of high-component arsenic trichloride waste in the reaction kettle, and there is a large amount of hydrochloric acid vapor in the reduction tail gas. If the treatment is not good, it will easily cause destructive effects on the environment or casualties; ③ when the concentration of arsenic trichloride impurities in the reaction kettle is high, it will easily occur Jumping boils, causing the distillation tower to vibrate, causing destructive damage to the quartz tower body, and having a destructive impact on the safety of operators and the environment

Its disadvantages: the specific gravity of lead is twice that of arsenic. When the lead is melted, the arsenic quickly floats to the surface of the lead melt, and the effect on the purification of impurities in the arsenic is not obvious. The test quality in the range of 100-200g of arsenic is very good. , the impurity content of arsenic > 200g does not meet the quality requirements and cannot be used for industrial production

Its disadvantage is that arsine is a colorless, odorless and highly poisonous gas. Once a leak occurs, it will bring great safety hazards to production workers and the environment.

At present, it is only used to produce high-purity α-arsenic on a small scale in foreign countries, and has not realized industrialization.

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