Production method for high-purity arsenic and its equipment

A production method and technology of production equipment, which are applied in the production method of ultra-high-purity α-type arsenic for semiconductor basic materials and the field of special equipment thereof, can solve the problem of impurity content not meeting quality requirements, hidden dangers of production workers and environmental safety, and distillation towers. Vibration and other problems, to achieve the effect of reducing the process of synthesizing alloys and separation, solving pollution problems and safety hazards, and saving labor costs

Inactive Publication Date: 2008-01-02
杨华民
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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.

Method used

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  • Production method for high-purity arsenic and its equipment
  • Production method for high-purity arsenic and its equipment
  • Production method for high-purity arsenic and its equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] First the raw material industry 1 #Arsenic 13 (purity is 99%) is put into a crucible 14, and crucible 14 is placed in the vacuum tank 1 again, then, connect a blocker 11 with 2 layers of stainless steel thin plates at the mouth of crucible 14, on the blocker 11 Covered with small holes of Φ2mm, the interlayer of the barrier 11 can be filled with some high-temperature-resistant, pollution-free and microporous adsorption materials 12, such as activated carbon, etc., and the upper part of the barrier 11 is connected with a conical condensation cylinder 10, and the conical condensation The cylinder 10 is made of titanium, and the surface has roughness requirements. A low-boiling collecting plate 7 of matching size is arranged at the small opening of the upper end of the conical condenser cylinder 10. The low-boiling collecting plate 7 is made of metal material, and three holes of Φ30mm are arranged on the surface . The outer ring of the mouth of the vacuum tank 1 is provid...

Embodiment 2

[0040] First the raw material industry 1 # Arsenic 13 (purity is 99%) is put into a crucible 14, and crucible 14 is placed in the vacuum tank 1 again, then, connect a blocker 11 with 2 layers of stainless steel thin plates at the mouth of crucible 14, on the blocker 11 Covered with small holes of Φ3mm, the interlayer of the barrier 11 can be filled with some high-temperature-resistant, pollution-free and microporous adsorption materials 12, such as activated carbon, etc., and the upper part of the barrier 11 is connected with a conical condensation cylinder 10, and the conical condensation The cylinder 10 is made of titanium, and the surface has roughness requirements. A low-boiling collecting plate 7 of matching size is arranged at the small opening of the upper end of the conical condensing cylinder 10. The low-boiling collecting plate 7 is made of metal material, and three holes of Φ25mm are arranged on the surface. . The outer ring of the mouth of the vacuum tank 1 is pro...

Embodiment 3

[0045] First the raw material industry 1 # Arsenic 13 (purity is 99%) is put into a crucible 14, and crucible 14 is placed in the vacuum tank 1 again, then, connect a blocker 11 with 2 layers of stainless steel thin plates at the mouth of crucible 14, on the blocker 11 Covered with small holes of Φ4mm, the interlayer of the barrier 11 can be filled with some high-temperature-resistant, pollution-free and microporous adsorption materials 12, such as activated carbon, etc., and the upper part of the barrier 11 is connected to a conical condensation cylinder 10, which is conical Condenser cylinder 10 is made of titanium, and the surface has roughness requirements. A low-boiling collecting plate 7 of matching size is arranged at the small opening of the upper end of conical condensing cylinder 10. Low-boiling collecting plate 7 is made of metal material, and three Φ20mm hole. The outer ring of the mouth of the vacuum tank 1 is provided with a cooling water jacket 4, and the cover...

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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 used in the preparation of optoelectronics and microelectronics gallium arsenide; infrared optical fiber, infrared lens As 2 Se 3 、As 2 Te 3 Etc. Infrared see-through glass; necessary material for As-Se alloy of photosensitive tympanic membrane. The civil popularization of gallium, infrared transparent glass and arsenic-containing alloys used in the electronics industry has increased the demand for high-purity arsenic at a rate of 25%-30% per year. [0003] At present, the production method of high-purity α-arsenic in the world is mainly based on the chlorination rectification method, followed by arsenic-lead alloy hydrogen atmosphere sublimation method, lead mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B30/04C22B9/02
CPCY02P10/20
Inventor 杨华民
Owner 杨华民
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