Raw material purifying method and device for removing H2O through reactive gas

A technology of reactive gas and purification method, applied in post-processing devices, chemical instruments and methods, crystal growth, etc., can solve the problem of high O impurity content, achieve the effect of improving photoelectric performance and reducing wetting effect

Active Publication Date: 2020-06-19
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem that the present invention solves is: in order to solve the H that still exists in the existing high-purity raw material 2 For...

Method used

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  • Raw material purifying method and device for removing H2O through reactive gas

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Experimental program
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Effect test

Embodiment 1

[0040] The first step is to take 40g of Cd metal with 4N purity and place it in the upper crucible structure of the purification device, transfer and fix the crucible to the gas circuit, and put it vertically into the heating furnace body.

[0041] The second step is to vacuumize the crucible, raw materials and pipelines to below 50Pa, and flow a protective atmosphere at a flow rate of preferably 0.3L / min to wash and maintain it. At this time, the pressure in the pipeline is kept within the range of 50Pa.

[0042] The third step is preferably to raise the temperature of the furnace body to 340°C at a heating rate of 10°C / min, and keep the temperature for 60 minutes.

[0043] The fourth step, preferably access to reactive gas SiCl 4 , the flow rate is 5ml / min, it is brought into the melt part through a protective atmosphere, fully reacted for 90min, and the exhaust gas is discharged to the atmosphere after passing through the exhaust gas purification device that comes with the ...

Embodiment 2

[0047] The first step is to take 35g of Cd metal with 4N purity and place it in the upper crucible structure of the purification device, transfer and fix the crucible to the gas circuit, and place it in the heating furnace body.

[0048] The second step is to vacuumize the crucible, raw materials and pipelines to below 50Pa, and flow a protective atmosphere at a flow rate of preferably 0.3L / min to wash and maintain it. At this time, the pressure in the pipeline is kept within the range of 500Pa.

[0049] The third step is preferably to raise the temperature of the furnace body to 340°C at a heating rate of 10°C / min, and keep the temperature for 60 minutes.

[0050] The fourth step, preferably access to reactive gas SiCl 4 , the flow rate is 2ml / min, it is brought into the melt part through the protective atmosphere, fully reacted for 120min, and the exhaust gas is discharged to the atmosphere after passing through the exhaust gas purification device that comes with the vacuum ...

Embodiment 3

[0057] In the first step, take 120g of sodium iodide with a purity of 5N and place it in the upper crucible structure of the purification device, transfer and fix the crucible to the gas circuit, and place it in the heating furnace body.

[0058] The second step is to vacuumize the crucible, raw materials and pipelines to below 50Pa, and flow a protective atmosphere at a flow rate of preferably 0.3 L / min to wash and maintain it. At this time, the pressure in the pipeline is kept within the range of 250 Pa.

[0059] The third step is preferably to raise the temperature of the furnace body to 800°C at a heating rate of 10°C / min and keep the temperature for 90 minutes.

[0060] The fourth step, preferably access to reactive gas SiBr 4 , with a flow rate of 4 ml / min, which is brought into the melt through a protective atmosphere, fully reacted for 180 min, and the exhaust gas is discharged to the atmosphere after passing through the exhaust gas purification device attached to the ...

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Abstract

The invention discloses a universal raw material dewatering and purifying method and device, which are used for solving the problem of water pollution ubiquitous in high-purity raw materials in the existing crystal industry. The method comprises the following steps: taking a high-purity 4N-6N metal or halogen compound as a to-be-purified raw material, and putting the to-be-purified raw material atthe upper part of a crucible structure connected by a capillary tube provided by the invention; transferring and fixing the crucible structure into a gas circuit and a furnace body; introducing a protective atmosphere, and heating the furnace body to melt the to-be-treated raw material; introducing halogen or silane compound reactive gas into the melt to make H2O in the melt fully react with thereactive gas to generate inert substances and tail gas, and enabling the inert substances and the tail gas to be discharged along with the protective atmosphere; and after the reaction is finished, adjusting the flow rate of the gas to extrude the melt into a lower crucible and sealing the tube. As H2O in the to-be-treated raw material fully reacts with the reactive gas in a high-temperature meltstate, the content of H2O in the raw material is reduced by 1-2 orders of magnitudes, the wetting effect of a crucible and a crystal can be effectively reduced, and the photoelectric property of a corresponding crystal is remarkably improved.

Description

technical field [0001] The invention belongs to the field of purification of crystal raw materials, in particular to the removal of H by reactive gases 2 O raw material purification method and device. Background technique [0002] Since the appearance of the pulling method and the vertical Bridgman method in the 1920s, the rapid progress of crystal growth technology has made inorganic single crystal materials, such as single crystal silicon germanium, III-V and II-VI compounds, metal halides Compounds, etc., account for an increasing proportion in national life, defense industry and high-tech fields. This also puts forward new requirements for the raw materials required for crystal growth. For example, the purity requirements for metal raw materials generally need to reach 4N (99.99%) or even 6N (99.9999%). Removing impurities in raw materials can significantly improve the growth of crystals. Physical and chemical, electrical, optical and other properties. [0003] At pre...

Claims

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Application Information

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IPC IPC(8): C30B35/00C30B29/12C30B29/02C22B9/05C22B17/02C22B17/06C01D3/12C01D3/14
CPCC01D3/12C01D3/14C22B9/05C22B17/02C22B17/06C30B29/02C30B29/12C30B35/007
Inventor 殷子昂张香港杨帆孙茂钧王涛
Owner NORTHWESTERN POLYTECHNICAL UNIV
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