Preparation method of germane

A technology of germane and germanium tetrachloride, which is applied in the field of special gas preparation, can solve the problems of difficult separation and purification, large consumption of raw materials, long process route, etc., and achieve the effect of easy separation and purification, low cost and simple process

Inactive Publication Date: 2010-06-09
ZHEJIANG SCI-TECH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the shortcomings of the above methods, such as long process route, large consumption of raw materials, low yield, and difficult separation and purification, their application is limited.

Method used

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  • Preparation method of germane
  • Preparation method of germane
  • Preparation method of germane

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Weigh 34.1g (0.9mol) of sodium borohydride, add it to 1mol / L sodium hydroxide solution, stir to dissolve, and transfer it to a reaction vessel; dissolve 104.7mL (0.9mol) of germanium tetrachloride in 104.7mL of tetrahydrofuran , transferred to the dropping funnel. Install the dropping funnel into the germane generation system and check the airtightness of the unit. 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 7mL / min, and react under magnetic stirring. The reaction time is 3h. The generated germane gas is passed into 10mol / L sodium hydroxide solution and calcium chloride drying tube respectively, and is collected by a gas collector after rough purification to remove impurity air and moisture. The germane gas in the above collector is adsorbed and purified through 4A molecular sieve and 5A molecular sieve respectively.

Embodiment 2

[0022] Take by weighing 30.3g (0.8mol) sodium borohydride, join in the sodium hydroxide solution of 1mol / L, stir to dissolve, transfer in the reaction vessel; Take 23.3mL (0.2mol) germanium tetrachloride and dissolve in 70mL tetrahydrofuran, Transfer to a dropping funnel. Install the dropping funnel into the germane generation system and check the airtightness of the unit. 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 3mL / min, and react under magnetic stirring. The reaction time is 0.5h. The generated germane gas is passed into 5mol / L sodium hydroxide solution and calcium chloride drying tube respectively, and is collected by a gas collector after rough purification to remove impurity air and moisture. The germane gas in the above collector is adsorbed and purified through 4A molecular sieve and 5A molecular sieve respectively.

Embodiment 3

[0024] Take by weighing 151.3g (4.0mol) sodium borohydride, join in the sodium hydroxide solution of 1mol / L, stir to dissolve, transfer in the reaction vessel; Get 46.5mL (0.4mol) germanium tetrachloride is dissolved in 280mL tetrahydrofuran, Transfer to a dropping funnel. Install the dropping funnel into the germane generation system and check the airtightness of the unit. 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 magnetic stirring. The reaction time is 1.5h. The generated germane gas is passed into 1mol / L potassium hydroxide solution and calcium chloride drying tube respectively, and is collected by a gas collector after rough purification to remove impurity air and moisture. The germane gas in the above collector is adsorbed and purified through 4A molecular sieve and 5A molecular sieve respectively.

[0025] figure 2 It is t...

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Abstract

The invention discloses a preparation method of germane, comprising dripping tetrahydrofuran solution of germanium tetrachloride into sodium hydroxide solution of sodium borohydride to react, and preparing the germane; wherein the molar ratio between the germanium tetrachloride and the sodium borohydride is 1:1-10. The reaction is carried out according to the equation: GeCl4+NaBH4+3NaOH=GeH4+B(OH)3+4NaCl. The method is simple in technique and lower in cost; and the prepared germane has high yield and less impurity content, and is easy to purify.

Description

technical field [0001] The invention relates to a method for preparing a special gas, in particular to a method for preparing germane. Background technique [0002] As a raw material gas, germane has important uses in the semiconductor industry. Germane is widely used in the manufacture of semiconductor devices such as diodes, transistors and integrated circuits. In addition, germane is also one of the indispensable raw materials for the preparation of infrared optical materials and resistance thermometers. Since the polycrystalline germanium prepared by decomposing germane has less impurity content, high purity and low energy consumption, germane is an important raw material for preparing polycrystalline germanium. [0003] In recent years, with the rapid development of microelectronics industry, photovoltaic industry and aerospace industry, the demand for germane is increasing. [0004] At present, the method for preparing germane mainly contains: (1) prepare germane by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/06
Inventor 席珍强杜平凡张瑞丽问明亮赵立奎
Owner ZHEJIANG SCI-TECH UNIV
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