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Preparation method of ZnS polycrystal

A technology of zinc sulfide and hydrogen sulfide, applied in polycrystalline material growth, chemical instruments and methods, single crystal growth, etc., can solve problems such as complex equipment requirements, difficult design of deposition chamber and vacuum system, poor process control, etc.

Active Publication Date: 2018-03-02
昆明先导新材料科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the production processes for preparing zinc sulfide polycrystalline mainly include: vacuum hot pressing method, chemical vapor deposition method and physical vapor deposition method, physical vapor deposition method (PVD) and chemical vapor deposition method (CVD) require complex equipment, deposition chamber The design of the vacuum and vacuum system is very difficult, and the process is very difficult to control. The fluctuation of temperature and vacuum in the process has a great impact on the zinc sulfide polycrystalline, resulting in cracking and low transmittance, and it takes a long time. up to half a month

Method used

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Examples

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preparation example Construction

[0014] The present invention provides a kind of preparation method of ZnS polycrystal, comprises the following steps:

[0015] Put zinc sulfide in a tubular heating furnace, start to feed hydrogen sulfide for 20-30 minutes, then raise the temperature, and keep warm for 2-4 hours after rising to the first temperature, the first temperature is 500-600°C; after rising to the first temperature Adjust the feed rate of hydrogen sulfide; after the heat preservation is over, cool down to 10-40°C to obtain pretreated zinc sulfide; the ratio of the quality of zinc sulfide, the initial feed rate of hydrogen sulfide and the adjusted feed rate of hydrogen sulfide is (0.0001-15 )kg:(1.5~2.3)L / min:(0.5~1)L / min;

[0016] Pretreated zinc sulfide and Al with a mass ratio of 100:0.3 to 0.8 2 S 3 mix to get a mixture;

[0017] Pre-compress the mixture to a pressure of 50-55MPa, then vacuumize it, heat it up to a second temperature after the vacuum degree reaches 4-10Pa, and keep it warm for 6-...

Embodiment 1

[0029] 1. Powder reduction: put 3kg of zinc sulfide with a D50 of 5 microns into a tubular heating furnace, feed hydrogen sulfide gas at 2L / min, keep it for 20min, then turn on the heating, raise the temperature to 600°C, and keep it for 3h; when the temperature After reaching the highest temperature, the flow rate of zinc sulfide gas was changed to 0.8L / min, and when the temperature dropped to room temperature, the material was taken out to obtain deoxidized zinc sulfide.

[0030] 2. Doping: zinc sulfide after deoxidation, adding 0.8% Al by mass 2 S 3 , mixed uniformly under the protection of an inert gas to obtain a mixture;

[0031]3. Vacuum hot pressing: the mixture is put into the mold, placed in a vacuum hot pressing furnace, and pre-pressed. The pre-pressing pressure is 53MPa, and the hot pressing furnace is vacuumed. 10°C / min, heated to 900°C, and kept for 7h. After rising to the highest temperature of 900°C for 4 hours, start to pressurize to 80MPa, and keep it unt...

Embodiment 2

[0034] 1. Powder reduction: Put 10kg of zinc sulfide with a D50 of 10 microns into a tubular heating furnace, feed hydrogen sulfide gas at 2L / min, keep it for 20min, then turn on the heating, raise the temperature to 550°C, and keep it for 4h; when the temperature After reaching the highest temperature, the flow rate of zinc sulfide gas is changed to 0.5L / min, and when the temperature drops to room temperature, the material is taken out to obtain deoxidized zinc sulfide;

[0035] 2. Doping: zinc sulfide after deoxidation, adding 0.5% Al by mass 2 S 3 , mixed uniformly under the protection of an inert gas to obtain a mixture;

[0036] 3. Vacuum hot pressing: the mixture is put into the mold, placed in a vacuum hot pressing furnace, and pre-pressed. The pre-pressing pressure is 50MPa, and the hot pressing furnace is vacuumed. 7°C / min, heat up to 1000°C, and keep warm for 6 hours; when the temperature rises to the highest temperature of 1000°C for 3 hours, start to pressurize, ...

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Abstract

The invention provides a preparation method of a ZnS polycrystal. The preparation method comprises the following steps: putting zinc sulfide into a tubular heating furnace; after introducing hydrogensulfide for 20min to 30min, raising the temperature; after raising the temperature to first temperature of 500 DEG C to 600 DEG C, keeping heat for 2h to 4h; after raising the temperature to the firsttemperature, adjusting an introducing speed; then cooling to obtain pre-treated zinc sulfide, wherein the ratio of the mass of the zinc sulfide to the introducing starting speed of the hydrogen sulfide to the adjusted introducing speed of the hydrogen sulfide is (0.0001kg to 15kg) to (1.5L / min to 2.3L / min) to (0.5L / min to 1L / min); mixing the pre-treated zinc sulfide and Al2S3 according to the mass ratio of 100 to (0.3 to 0.8) to obtain a mixture; after pre-pressing the mixture to 50MPa to 55MPa, vacuumizing; after raising the vacuum degree to 4Pa to 10Pa and raising the temperature to secondtemprature of 800 DEG C to 1000 DEG C, keeping the heat for 6h to 8h; after raising the temperature to the second temprature for 3h to 5h, pressurizing to 70MPa to 90MPa; keeping the pressure until the temperature is 10 DEG C to 40 DEG C to obtain the ZnS polycrystal.

Description

technical field [0001] The invention relates to the technical field of polycrystalline zinc sulfide, in particular to a method for preparing ZnS polycrystalline. Background technique [0002] ZnS is a widely used wide bandgap II-VI semiconductor material. Infrared zinc sulfide polycrystalline materials have excellent mechanical and optical properties, and are widely used in fairings for infrared imaging systems and multispectral precision guidance systems. [0003] At present, the production processes for preparing zinc sulfide polycrystalline mainly include: vacuum hot pressing method, chemical vapor deposition method and physical vapor deposition method, physical vapor deposition method (PVD) and chemical vapor deposition method (CVD) require complex equipment, deposition chamber The design of the vacuum and vacuum system is very difficult, and the process is very difficult to control. The fluctuation of temperature and vacuum in the process has a great impact on the zinc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/48C30B28/02
CPCC30B28/02C30B29/48
Inventor 文崇斌朱刘胡智向解磊鹏曾成亮余芳
Owner 昆明先导新材料科技有限责任公司
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