Preparation method of high purity zinc phosphide

A zinc phosphide, high-purity technology, applied in the direction of phosphide, can solve the problems of low synthesis rate, incomplete reaction, high investment cost, etc., and achieve the effect of improving synthesis rate, avoiding tube explosion, and ensuring yield

Inactive Publication Date: 2017-03-08
衡阳恒荣高纯半导体材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are two technical schemes in the prior art: one is the combustion method, and the other is the ZnP2 vacuum thermal decomposition method. The main disadvantages of the two schemes are: 1. Higher requirements on the form of raw materials
2. Incomplete reaction, low synthesis rate
3. The equipment is relatively complicated and the investment cost is high
4. The product does not meet the high-purity requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method of high-purity zinc phosphide, comprising the steps of:

[0021] a. Use pyrolysis reaction to deposit carbon film in the clean quartz tube. The specific operation of the carbon film treatment of the quartz tube is: heating the furnace to 800-1100°C, fixing the vent pipe, and feeding it into the high temperature at a rate of 0.5-1 liter / min. Pure argon bubbles to transport acetone vapor into the quartz tube, and at the same time, move the heating furnace with the quartz tube at a speed of 10-20cm / 10 seconds;

[0022] b. Pick red phosphorus with a purity of 6N and zinc of 6N and put them into the quartz tube. Put the zinc and phosphorus with a molar ratio of 4:3 into the quartz tube after step a. The maximum amount of material in the quartz tube is 500g when batching. ;

[0023] c. After heating the deoxidation furnace to 250°C, put the quartz tube into the vacuum system for deoxidation. When the vacuum degree of the vacuum system reaches 5×10-4pa~10...

Embodiment 2

[0028] A preparation method of high-purity zinc phosphide, comprising the steps of:

[0029] a. Use pyrolysis reaction to deposit carbon film in the clean quartz tube. The specific operation of the carbon film treatment of the quartz tube is: heating the furnace to 900°C, fixing the vent tube, and feeding high-purity argon drum at a rate of 1 liter / min. Bubble transport acetone vapor into the quartz tube, at the same time, move the heating furnace with the quartz tube at a speed of 15cm / 10 seconds;

[0030] b. Pick red phosphorus with a purity of 6N and zinc of 6N and put them into the quartz tube. Put the zinc and phosphorus with a molar ratio of 4:3 into the quartz tube after step a. The maximum amount of material in the quartz tube is 500g when batching. ;

[0031] c. After heating the deoxidation furnace to 260°C, put the quartz tube into the vacuum system for deoxidation. When the vacuum degree of the vacuum system reaches 5×10-4pa~10×10-4pa, seal the quartz tube, and st...

Embodiment 3

[0036] A preparation method of high-purity zinc phosphide, comprising the steps of:

[0037] a. Use pyrolysis reaction to deposit carbon film in the clean quartz tube. The specific operation of the carbon film treatment of the quartz tube is: heating the furnace to 900°C, fixing the vent tube, and feeding high-purity argon drum at a rate of 1 liter / min. Bubble transport acetone vapor into the quartz tube, at the same time, move the heating furnace with the quartz tube at a speed of 15cm / 10 seconds;

[0038] b. Pick red phosphorus with a purity of 6N and zinc of 6N and put them into the quartz tube. Put the zinc and phosphorus with a molar ratio of 4:3 into the quartz tube after step a. The maximum amount of material in the quartz tube is 500g when batching. ;

[0039] c. After heating the deoxidation furnace to 270°C, put the quartz tube into the vacuum system for deoxidation. When the vacuum degree of the vacuum system reaches 5×10-4pa~10×10-4pa, seal the quartz tube and sto...

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PUM

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Abstract

The invention discloses a preparation method of high purity zinc phosphide. The preparation method comprises a, preparing a clean quartz tube, b, adding zinc and phosphorus in a molar ratio of 4: 3 into a quartz tube and fully mixing the materials, c, heating a deoxidizing furnace to 200-280 DEG C, putting the quartz tube into a vacuum system, carrying out deoxidation, sealing the quartz tube in the vacuum system, and then stopping deoxidation, d, putting the quartz tube into a synthesis furnace, slowly heating the quartz tube to 600-800 DEG C at a heating rate of 100-200 DEG C / h, keeping the temperature for 1.5 to 2.5 hours, slowly heating the quartz tube to 1100-1200 DEG C at a heating rate of 100-200 DEG C / h, keeping the temperature for 2.5-3.5h, slowly cooling the quartz tube to 900-1050 DEG C at a cooling rate of 100-200 DEG / h and stopping the furnace, and e, opening the quartz tube, taking out a zinc phosphide product, putting the zinc phosphide product into a dry container and carrying out sealed storage. The preparation method prevents pipe explosion caused by overlarge pressure of high-purity phosphorus vapor, utilizes slow heating to ensure a complete reaction and produces the product meeting the stoichiometric ratio requirements.

Description

technical field [0001] The invention relates to a preparation method of high-purity zinc phosphide. Background technique [0002] High-purity zinc phosphide is a II-V semiconductor material with a band gap of 1.5ev. In recent years, zinc phosphide materials have been highly concerned by people, and compound semiconductors such as gallium arsenide and indium phosphide are indispensable semiconductor materials in the field of modern wireless communication and optical communication. In device technology such as indium phosphide, high-purity zinc phosphide is often used as a diffusion source. Zinc phosphide is one of the semiconductor materials that countries are currently actively investing in applied research, including applied research on solar cells and single-dimensional nanodevices. Therefore, with the continuous expansion of its application fields, the demand for zinc phosphide materials will also increase. There will be a large increase, and the development prospect is...

Claims

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Application Information

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IPC IPC(8): C01B25/08
CPCC01B25/08C01P2006/80
Inventor 聂玉周晴陈建国
Owner 衡阳恒荣高纯半导体材料有限公司
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