Production method and device for controlling germane preparation by adjusting electromotive force

A production method and electromotive force technology, applied in the direction of sampling devices, chemical instruments and methods, metal hydrides, 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

Pending Publication Date: 2022-06-24
贺孝鸣
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  • Summary
  • 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
[0008] 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 device for controlling germane preparation by adjusting electromotive force
  • Production method and device for controlling germane preparation by adjusting electromotive force
  • Production method and device for controlling germane preparation by adjusting electromotive force

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Experimental program
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Effect test

Embodiment 1

[0049] Example 1, refer to figure 1

[0050] The germane preparation equipment includes a reactor 3, and the germane preparation equipment is further provided with:

[0051] Feeder for acidic aqueous solution 1. MBH 4 and GeO 2 The alkaline aqueous solution feeder 2, the alkaline feed sampler 7, the acid feed sampler 6, the discharge sampler 8 and the electrical function test controller 9;

[0052] The feed line of the feeder 1 of the 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;

[0053] The feeder 1 of the acidic aqueous solution and the reactor 3 are connected by pipelines and are provided with a third valve 12; MBH 4 and GeO 2 The alkaline aqueous solution feeder 2 and the reactor 3 are connected by pipelines and are provided with a fourth valve 13;

[0054] The outlet pipe of the reactor has a fifth valve 14;

[0055] The acidic feed sampler 6 has sampling points be...

Embodiment 2

[0066] The present invention adopts the method and device for manipulating germane preparation by adjusting electromotive force, and is characterized in that the control reaction conditions are within the range of spontaneous electromotive force, which satisfies E A >0 conditions, the temperature, starting material and product concentration conditions are optimized in the spontaneous reaction range. GeO 2 (8.1 g) and NaBH 4 (17.69 g) was dissolved in 520 ml of KOH solution successively, and the pH value after 10-fold dilution of sampling was 13.45; the sulphuric acid solution was prepared respectively, and the pH value after 10-fold dilution of sampling was 0.82; the prepared acidic solution and alkaline solution were mixed To achieve the discharge requirement of pH 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 the impurities suc...

Embodiment 3

[0068] The invention adopts the method and device for manipulating germane preparation by adjusting electromotive force, opening the second valve, raw material MBH 4 (17.52 g) and GeO 2 (8.08 g) of KOH alkaline aqueous solution (515 ml) was sampled by alkaline sampler 7 and analyzed and approved by electrical function test 9 (10-fold dilution pH value was 13.45) through alkaline feeder 2 and the fourth valve opened. to the reactor 3, then acidified by the sulfuric acid from the acid feeder 1, which was sampled by the first valve opened and the acid sampler 6 and the electrical function test controller 9 test and approved before entering the reactor (10 times diluted The pH value is 0.52) and then flows into the reactor 3 through the opened third valve 12; the reacted discharge is sent to the electrical function test controller 9 through the opened fifth valve and the sampler 8, and after the test is approved ( The pH value is 1.02) to keep the reaction continuing, otherwise t...

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Abstract

The invention provides a production method and equipment for controlling germane preparation by adjusting electromotive force, which comprises the following steps: adjusting the acidity in an alkaline aqueous solution of MBH4 and GeO2 by using an acidic aqueous solution until the spontaneous reaction electromotive force of germane is generated; in the subsequent germane preparation process, the electromotive force of the reaction liquid or parameters related to the electromotive force is monitored to control the preparation of germane, so that the consumption of raw materials and the generation of byproduct hydrogen are reduced, and when the electromotive force of the reaction liquid or the parameters related to the electromotive force is abnormal, the germane is prepared. And adjusting the electromotive force of the reaction liquid or parameter values related to the electromotive force to a normal range by selecting means. Effective reaction condition control is quantitatively implemented on a reaction system, the purposes of high germane yield, low raw material consumption and low byproduct hydrogen are achieved, meanwhile, a basis is provided for realizing automatic production in the aspect of improving production safety control, a reaction condition measurement and control technology for germane preparation is simplified, and the production cost is reduced. And the effectiveness and the accuracy of reaction condition control are improved.

Description

[0001] The present invention is a divisional application for a patent application with a patent application date of August 20, 2015, a patent application number of 201510512794.4, and the title of a production method and device for preparing germane by regulating electromotive force. technical field [0002] The invention belongs to the field of gas production, and relates to a process of reducing germanium compounds with hydrides and is capable of producing high-yield germane (GeH 4 Referred to as germane), digermane (Ge 2 H 6 ) and other methods, especially suitable for the production of germane. [0003] technical background [0004] Germane is a promising precursor of germanium films and germanium-silicon alloys, and is one of the attractive specialty gases in the semiconductor industry. However, the existing method for preparing germane is mainly due to high control difficulty, high consumption of raw materials, expensive equipment and other reasons, resulting in high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/06C01B6/34G01N1/10
Inventor 贺孝鸣
Owner 贺孝鸣
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