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Method for preparing high-purity germanium tetrafluoride through thermal decomposition of barium fluorogermanate

A technology of high-purity germanium tetrafluoride and barium fluorogermanate, which is applied in the direction of germanium halide, etc., can solve the problems of introducing too many impurities into germanium tetrafluoride and difficulty in obtaining fluorine gas, etc., achieving less impurities, wide application fields, and high yield high rate effect

Inactive Publication Date: 2021-10-22
YUNNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

my country's standard GB / T 26251-2010 for fluorine gas has a maximum purity of 99.0%. Due to the lively nature of fluorine gas, it is filled with a mixture of fluorine and nitrogen. Therefore, it is difficult to obtain high-purity tetrafluoroethylene on the market. Fluorine gas for germanium
[0009] Although method (b) can be produced quantitatively, its by-products will introduce too many impurities into germanium tetrafluoride

Method used

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  • Method for preparing high-purity germanium tetrafluoride through thermal decomposition of barium fluorogermanate
  • Method for preparing high-purity germanium tetrafluoride through thermal decomposition of barium fluorogermanate

Examples

Experimental program
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Effect test

Embodiment 1

[0046] At 25°C, 100g of soluble germanium dioxide was put into 250mL of 25mol / L HF hydrofluoric acid solution, and stirred for 10min. It can be seen that the obtained mixed solution of fluorogermanic acid and hydrofluoric acid was clear and transparent. Add 205g BaCl 2 Powder, stir for 10 minutes to make it fully precipitated, and white granular precipitates can be seen in the solution. After filtration, the crystals were washed once with pure water and three times with absolute ethanol. Press it into a block of 10*10*10mm, put it into an oven, set the drying temperature to 70°C, and dry it for 10 hours to obtain 311.7g of the product. The reaction between germanium dioxide and hydrofluoric acid is complete. The molar ratio of hydrofluoric acid solution to soluble germanium dioxide is 6.53:1, which is greater than 6-6.25:1. After the reaction of germanium dioxide is complete, a large amount of hydrogen fluoride remains in the solution, and barium salt is added. Afterwards, b...

Embodiment 2

[0048] Put 100g of soluble germanium dioxide into 235mL of 25mol / L HF hydrofluoric acid solution at 25°C and stir for 10min. It can be seen that the obtained mixed solution of fluorogermanic acid and hydrofluoric acid is clear and transparent. Add 205g BaCl 2 Powder, stir for 10 minutes to make it fully precipitated. It can be seen that white granular precipitates appear in the solution. After filtration, the crystals were washed once with pure water and three times with absolute ethanol. Press it into a block of 10*10*10mm, put it into an oven, set the drying temperature at 70°C, and dry it for 10 hours to obtain 307.9g of the product. The content of barium fluorogermanate is 99.6%, and the content of germanium is 99.6%. The comprehensive recovery rate was 99.0%.

[0049] Dry nitrogen gas 4 was introduced into the quartz tube to replace the system, and 100.0 g of block barium fluorogermanate was taken and put into the quartz tube 3, and the pressure inside the quartz tube ...

Embodiment 3

[0052] At 25°C, put 500g of soluble germanium dioxide into 1.15L of 25mol / L HF hydrofluoric acid solution, and stir for 20min. It can be seen that the obtained mixed solution of fluorogermanic acid and hydrofluoric acid is clear and transparent. Add 990.0g BaCl 2 Powder, stir for 30 minutes to make it fully precipitated. It can be seen that white granular precipitates appear in the solution. After filtration, the crystals were washed once with pure water and three times with absolute ethanol. Press it into a block of 10*10*10mm, put it into an oven, set the drying temperature at 70°C, and dry it for 10 hours to obtain 1546.7g of the product. The content of barium fluorogermanate is 99.7%, and the content of germanium is The comprehensive recovery rate was 99.6%.

[0053] Dry nitrogen gas 4 was introduced into the quartz tube to replace the system, and 1000.0 g of block barium fluorogermanate was taken and put into the quartz tube 3, and the pressure inside the quartz tube w...

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Abstract

The invention belongs to the technical field of germanium tetrafluoride preparation, and particularly discloses a method for preparing high-purity germanium tetrafluoride through thermal decomposition of barium fluorogermanate. The method comprises the following steps: dissolving soluble germanium dioxide in a hydrofluoric acid solution to prepare a fluorogermanic acid solution, wherein the concentration of hydrofluoric acid is 25mol / L, and the molar ratio of the hydrofluoric acid solution to the soluble germanium dioxide is (6-6.25): 1; adding barium salt into the fluorogermanic acid solution to generate barium fluorogermanate precipitate; and making the generated barium fluorogermanate precipitate washed with absolute ethyl alcohol to remove hydrogen fluoride residues, placing the precipitate into a mold to be pressed into blocks and performing drying. Barium fluorogermanate can be rapidly decomposed at the temperature of 600-700 DEG C to generate germanium tetrafluoride, the germanium yield is high, and the solid by-product barium fluoride has very wide application field and scientific application research value. The reaction does not need fluorine gas participation, the requirement for a reaction device is low, configuration is simple, control is easy, and germanium tetrafluoride produced through thermal decomposition is high in purity and few in impurity.

Description

technical field [0001] The invention belongs to the technical field of germanium tetrafluoride preparation, and in particular relates to a method for preparing high-purity germanium tetrafluoride by thermally decomposing barium fluorogermanate. Background technique [0002] High-purity germanium tetrafluoride is mainly used as an intermediate for germanium isotope separation in the nuclear industry, and can be used as a dopant and ion implantation agent in the semiconductor industry. There are several preparation methods: [0003] (a) Elemental metal germanium reacts with fluorine gas: [0004] Ge+2F 2 → GeF 4 [0005] (b) Reaction of germanium dioxide with bromine trifluoride: [0006] 3GeO 2 +4BrF 3 →3GeF 4 +3O 2 +2Br 2 [0007] Method (a) The manufacturing method of application number 200980138501.3 titled germanium tetrafluoride discloses a manufacturing method of germanium tetrafluoride, which uses diluted fluorine gas to react with a germanium block heated to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G17/04
CPCC01G17/04C01P2006/80
Inventor 柴皓茗普世坤张红萧熊浩邵雨萌尹国文罗中旭王东
Owner YUNNAN UNIV
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