Preparation method for zinc arsenide

A technology for diarsenic trizinc and zinc ingots, applied in chemical instruments and methods, arsenic compounds, inorganic chemistry, etc., can solve the problems of small synthesis scale, complicated process, slow reaction speed, etc., and the synthesis scale can be large or small. , The reaction conditions are easy to control, and the reaction is completely and fully effected

Active Publication Date: 2015-09-30
FIRST RARE MATERIALS CO LTD
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0003] At present, the method of preparing zinc diarsenide mainly adopts gas phase synthesis or vacuum volatilization synthesis, followed by vacuum distillation, separation and purification, which has problems such as slow reaction speed, large equipment investment, small synthesis scale and complicated process.
And because arsenic begins to sublimate at 613°C, its vapor pressure increases sharply with the increase of temperature, and there are safety hazards such as tube explosion. Therefore, many preparation methods currently use the synthesis of primary zinc diarsenide at a lower temperature. However, the reaction at low temperature is not sufficient, and there are a large amount of free arsenic, zinc and zinc arsenide in the synthetic material.

Method used

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  • Preparation method for zinc arsenide

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preparation example Construction

[0010] Firstly, the preparation method of zinc diarsenide according to the present invention is described, including steps: (1) weighing high-purity arsenic particles and high-purity zinc ingots according to the molar ratio of arsenic and zinc in zinc diarsenide, Evenly spread the weighed high-purity arsenic particles in a crucible boat, then cover the high-purity zinc ingots on the high-purity arsenic particles, and then put the crucible boat horizontally into the flat-mouthed quartz tube; A flat quartz tube with high purity arsenic pellets and high purity zinc ingots is evacuated to 10 -2 Below Pa, then use a hydrogen-oxygen flame to seal the flat-mouthed quartz tube at high temperature; (3) Put the sealed flat-mouthed quartz tube into the horizontal synthesis furnace, and raise the temperature to 470-550 °C at a heating rate of 8-15 °C / min And keep it warm for 90-150min, then raise the temperature to 780-850℃ at a heating rate of 5-7℃ / min and keep it warm for 60-120min, the...

Embodiment 1

[0024] (1) Put a 30cm-long high-purity graphite crucible boat filled with 5N high-purity zinc in the quartz tube of the grinding head and pass nitrogen protection into the quartz tube of the grinding head, then put the quartz tube of the grinding head into the horizontal heating furnace horizontally, and then The temperature of the horizontal heating furnace is raised to 455°C, and the temperature is kept constant for 60 minutes. After the high-purity zinc is completely melted, the horizontal heating furnace is turned off so that the high-purity zinc in the high-purity graphite crucible boat is cooled to room temperature with the furnace to form a high-purity zinc ingot;

[0025] (2) Open the quartz tube of the grinding head to take out the high-purity zinc ingot, soak in dilute hydrochloric acid for 2 minutes to treat the oxide film on the surface, then rinse it with deionized water and dry it in vacuum. The weight of the treated high-purity zinc ingot is 453.6 g;

[0026] (3...

Embodiment 2

[0031] (1) Put a 45cm-long high-purity zirconia crucible boat filled with 6N high-purity zinc in the quartz tube of the grinding head and pass argon gas into the quartz tube of the grinding head for protection, and then put the quartz tube of the grinding head into the horizontal heating furnace horizontally Afterwards, the temperature of the horizontal heating furnace is raised to 500 ° C, and the temperature is kept constant for 40 minutes. After the high-purity zinc is completely melted, the horizontal heating furnace is closed to cool the high-purity zinc to room temperature in the high-purity zirconia crucible boat to form a high-purity zinc ingot;

[0032] (2) Open the quartz tube of the grinding head to take out the high-purity zinc ingot, soak it in dilute hydrochloric acid for 3 minutes to treat the oxide film on the surface, then rinse it with deionized water and dry it in vacuum. The weight of the treated high-purity zinc ingot is 921.1 g;

[0033] (3) Calculate and...

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Abstract

The invention provides a preparation method for zinc arsenide. The preparation method comprises the following steps: weighing high-purity arsenic particles and high-purity zinc ingots with corresponding weights according to the molar proportion of arsenic and zinc in zinc arsenide, uniformly paving the weighed high-purity arsenic particles in a crucible boat, then covering the high-purity zinc ingots on the high-purity arsenic particles, and then horizontally placing the crucible boat in a plain-end quartz tube; vacuumizing the plain-end quartz tube filled with the high-purity arsenic particles and the high-purity zinc ingots by a vacuum unit, and then carrying out high-temperature sealing for the plain-end quartz tube by virtue of oxyhydrogen flame; placing the sealed plain-end quartz tube in a horizontal synthesis furnace, heating and insulating for a period of time, and then stopping heating and naturally cooling the horizontal synthesis furnace; after the horizontal synthesis furnace is cooled to a normal temperature, taking out the horizontal synthesis furnace and knocking open the plain-end quartz tube to obtain a high-purity zinc arsenide crystal. The preparation method provided by the invention increases the reaction speed of the synthesis process, can well control the arsenic vapour pressure during the synthesis process, and enables the reaction to be complete and adequate.

Description

technical field [0001] The invention relates to the technical field of material preparation, in particular to a preparation method of trizinc diarsenide. Background technique [0002] Trizinc diarsenide is a gray crystal, which is often used as a reagent for spectral analysis and a raw material for the preparation of electronic components. It is also a new type of semiconductor material. In the semiconductor material industry, trizinc diarsenide can also be used as the raw material or arsenic source of semiconductor materials such as gallium arsenide, indium arsenide, gallium arsenic phosphide, and indium arsenic phosphide prepared by methods such as epitaxy and vapor phase chemical deposition. Its use is becoming more and more extensive. [0003] At present, the method of preparing zinc diarsenide mainly adopts gas phase synthesis or vacuum volatilization synthesis followed by vacuum distillation separation and purification, which has problems such as slow reaction speed, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G28/00
Inventor 胡智向朱刘罗涛文崇斌
Owner FIRST RARE MATERIALS CO LTD
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