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Preparation method of germane gas

A technology of gas and germane, which is applied in the field of germane gas preparation, can solve the problems of low conversion rate and easy generation of yellow precipitates, etc., and achieve the effect of increasing the conversion rate of germane and reducing the generation of yellow precipitates

Active Publication Date: 2011-11-23
中锗科技有限公司
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  • Summary
  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

However, yellow precipitates are easily produced during the reaction process of this method, resulting in a low conversion rate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Weigh 151.3g (4mol) sodium borohydride, add it to 3L 1mol / L sodium hydroxide solution, add 15mL polypropylene glycol PPG600, stir to dissolve, transfer to the reactor; take 46.5mL (0.4mol) germanium tetrachloride Dissolve in 280mL tetrahydrofuran and transfer to the dropping funnel. Put the dropping funnel into the germane generating system and check the airtightness of the device. Use a vacuum pump to evacuate the system. After the vacuum degree drops below 10Pa, control the dropping funnel to add liquid dropwise to the reactor at a rate of 30mL / min, and react under stirring. The reaction time is 1.5h. The generated gas is passed into the calcium chloride drying pipe, and collected by a gas collector after removing moisture. A small amount of yellow precipitate appeared during the reaction, and the conversion rate of germane was 86.4%.

Embodiment 2

[0015] Change the addition amount of polypropylene glycol PPG600 in Example 1 to 150 mL, and other conditions are the same. No yellow precipitate occurred during the reaction, and the conversion rate of germane was 87.6%.

Embodiment 3

[0017] Change the addition amount of polypropylene glycol PPG600 in Example 1 to 60 mL, and other conditions are the same. No yellow precipitate appeared during the reaction, and the conversion rate of germane was 87.3%.

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PUM

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Abstract

The invention provides a preparation method of germane gas. According to the method, a sodium hydroxide solution of sodium borohydride is prepared; polyether with a volume of 0.5% to 5% of that of the solution is added to the solution; and a tetrahydrofuran solution of germanium tetrachloride is added to the solution for preparing germane gas. Compared to previously disclosed methods, according to the present method, polyether is added to the reaction solution, such that a substantial effect is brought in, generation of yellow precipitate is greatly reduced, and a conversion rate of germane is improved by approximately 7%.

Description

technical field [0001] The invention relates to a method for preparing germane gas, in particular to a method for preparing germane by adding polyether to a reaction solution to increase the conversion rate. Background technique [0002] High-purity germane is an important raw material gas for the semiconductor industry. It has been gradually applied to metal organic compound vapor phase epitaxy (MOVPE) to prepare germanium-containing semiconductor materials or devices, such as germanium-silicon thin-film solar cells. [0003] There are many ways to prepare germane. The early method is to use LiAlH in ether medium 4 Reduced GeCl ４ to prepare germane; the classical method for preparing germane is Mg ２ Ge is hydrolyzed in dilute acid (such as hydrochloric acid) solution; Ge(IV) in aqueous solution is reduced to germane by reducing agent or electrolysis; germane can also be produced by reducing Ge(IV) in acidic solution with sodium borohydride ; A better way to prepare germa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/06
Inventor 柯尊斌黄兴灯吴志湘
Owner 中锗科技有限公司
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