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Production method and production device with regulation of electromotive force to control preparation of germane

A production method and electromotive force technology, applied in chemical instruments and methods, metal hydrides, inorganic chemistry, etc., can solve the problems of lack of control methods, difficulty in application, poor repeatability, etc., achieve simplified reaction condition measurement and control technology, and improve effective performance and accuracy, low by-product hydrogen

Inactive Publication Date: 2017-03-01
贺孝鸣
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the actual application parameters of this method are complex, there is no control method for the formation of foam and by-product hydrogen, the repeatability is poor and optimization is difficult, and it is very difficult to maintain effective high-yield production
[0007] In short, the existing methods for preparing germane lack effective control ability, the practical application is difficult and the cost is high

Method used

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  • Production method and production device with regulation of electromotive force to control preparation of germane
  • Production method and production device with regulation of electromotive force to control preparation of germane
  • Production method and production device with regulation of electromotive force to control preparation of germane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Embodiment 1, with reference to figure 1

[0047] The germane preparation equipment includes reactor 3, and the germane preparation equipment is also provided with:

[0048] Feeder for acidic aqueous solution 1, MBH 4 and GeO 2 Alkaline aqueous solution feeder 2, alkaline feed sampler 7, acidic feed sampler 6, discharge sampler 8 and electrical function test controller 9;

[0049] The feed line of feeder 1 for acidic aqueous solution has a first valve 10, MBH 4 and GeO 2 The feed pipeline of the alkaline aqueous solution feeder 2 has a second valve 11;

[0050] The feeder 1 of the acidic aqueous solution is connected to the reactor 3 through a pipeline and is provided with a third valve 12; MBH 4 and GeO 2 The alkaline aqueous solution feeder 2 and the reactor 3 are connected by a pipeline and are provided with a fourth valve 13;

[0051] The discharge pipe of the reactor has a fifth valve 14;

[0052] The acid feed sampler 6 has a sampling point between the fi...

Embodiment 2

[0063] The invention adopts the method and device for manipulating the preparation of germane by adjusting the electromotive force, which is characterized in that the controlled reaction conditions are within the range of spontaneous electromotive force and satisfy E A >0, optimize the conditions of temperature, starting material and product concentration within the spontaneous reaction range. GeO 2 (8.1 g) and NaBH 4 (17.69 grams) is successively dissolved in the KOH solution of 520 milliliters, and the pH value after sampling 10-fold dilution is 13.45; Prepare sulfuric acid solution respectively, the pH value after sampling 10-fold dilution is 0.82; Mix the acidic solution and alkaline solution prepared To meet the discharge requirement of PH value of 1.18, the reaction temperature is controlled at 25°C; the product collected in the gas phase is roughly separated and separated to remove moisture to obtain 5.80 grams of crude germane, and then remove impurities such as carbo...

Embodiment 3

[0065] The present invention adopts the method and device for manipulating the preparation of germane by adjusting the electromotive force, opens the second valve, and the raw material MBH 4 (17.52 g) and GeO 2 (8.08 grams) of KOH alkaline aqueous solution (515 milliliters) is fed through alkaline feeder 2 and the 4th valve of opening after alkaline sampler 7 sampling and electric function test 9 analysis approvals (10 times dilution pH value is 13.45) To reactor 3, be acidified by the sulfuric acid from acidic feeder 1 then, this sulfuric acid passes through the first valve that opens before entering reactor and acid sampler 6 sampling and electrical function test controller 9 test approvals (10 times diluted PH value is 0.52) enters reactor 3 through the 3rd valve 12 of opening again; The discharged material after the reaction is sent to electrical function test controller 9 by sampling through the 5th valve of opening and sampler 8, after test approval ( The pH value is 1....

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Abstract

The invention provides a production method and a production device with regulation of electromotive force to control preparation of germane. An acidic water solution is used for performing acidity regulation in a MBH4 and GeO2 alkaline water solution until the spontaneous reaction electromotive force of generation of the germane. In the subsequent germane preparation process, the electromotive force or parameters related to the electromotive force of the reaction liquid are monitored and controlled so as to control preparation of the germane, thereby reducing consumption of raw materials and generation of a byproduct, hydrogen. When the electromotive force or the parameters related to the electromotive force of the reaction liquid are abnormal, the electromotive force or the parameters related to the electromotive force of the reaction liquid are regulated in some manner to a normal range. The method implements effective reaction condition control to the reaction system quantitatively, thereby achieving high germane yield, low raw material consumption and low byproduct hydrogen. Meanwhile, in the aspect of improving security control of production, the method lays the foundation for automatic production and simplifies reaction condition measurement and control technologies of preparation of the germane, and also increases the effectiveness and accuracy of the control on the reaction conditions.

Description

technical field [0001] The invention belongs to the field of gas production, and relates to the process of reducing germanium compounds with hydrides and producing high-yield germane (GeH) through electromotive force manipulation. 4 Germane for short), Digermane (Ge 2 h 6 ) and other methods are especially suitable for the production of germane. [0002] technical background [0003] Germane is a promising precursor of germanium films and germanium-silicon alloys, and is one of the attractive special gases in the semiconductor industry. However, the existing germane preparation method is mainly due to the difficulty of control, the consumption of many raw materials, and the expensive equipment, which lead to high production costs and serious waste of germanium resources. [0004] The Chinese patent document with application number 200910095214.0 discloses a method for preparing germane by reacting magnesium germanium with ammonium chloride in a liquid ammonia medium. Beca...

Claims

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Application Information

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IPC IPC(8): C01B6/06
Inventor 贺孝鸣
Owner 贺孝鸣
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