CN1483665A - Process for preparing zinc selenide (zn se) powder material - Google Patents

Process for preparing zinc selenide (zn se) powder material Download PDF

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Publication number
CN1483665A
CN1483665A CNA031344305A CN03134430A CN1483665A CN 1483665 A CN1483665 A CN 1483665A CN A031344305 A CNA031344305 A CN A031344305A CN 03134430 A CN03134430 A CN 03134430A CN 1483665 A CN1483665 A CN 1483665A
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powder
zinc selenide
znse
crucible
heating
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CN1199851C (en
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吴洪才
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Xian Jiaotong University
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Xian Jiaotong University
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Abstract

A process for preparing a crude zinc selenide (ZnSe) powder includes mixing powder of element Se with powder of element Zn in a proportion of (1-1.35):1, putting the mixture in an indirect heat crucible to be placed in a vacuum room, heating the crucible up to 300-380 deg.C. Furthermore, the high purity of zinc selenide powder can be obtained through grinding and annealing the crude reactant under the conditions of vacuum with a temp. of 550-700 deg.C and 90 minutes. Zinc selenide (ZnSe) powder is an important photoelectric material used in defense industry.

Description

The preparation method of a kind of zinc selenide (ZnSe) powdered material
One, affiliated technical field
The invention belongs to field of photovoltaic materials, relate to a kind of powdered material, be particularly related to the preparation method of a kind of zinc selenide (ZnSe) powdered material, zinc selenide (ZnSe) powdered material that this method is prepared, be applicable to be preparation zinc selenide (ZnSe) film, zinc selenide (ZnSe) single crystal material provides highly purified zinc selenide raw material.
Two, background technology
Zinc selenide (ZnSe) is a kind of important photoelectric semiconductor material, in fields such as photoluminescence and electroluminescent device, solar cell, laser technology, infrared eye, thermal imagings important purposes is arranged all.At present, zinc selenide (ZnSe) technology of preparing mainly contains chemical bath deposition method, chemical Vapor deposition process, electrochemical deposition method, molecular beam epitaxy, Metalorganic Chemical Vapor Deposition, photochemical precipitation method etc.
Three, summary of the invention
The objective of the invention is to, provide a kind of physical method to prepare zinc selenide (ZnSe) powdered material, equipment required for the present invention is simple, and is simple to operate, the material purity height of preparation, and the crystalline texture form is single.
The technical solution that realizes the foregoing invention purpose is: the preparation of zinc selenide (ZnSe) powdered material is at first in (1-1.35): 1 ratio is mixed simple substance selenium powder (Se) and simple substance zinc powder (Zn), stir, put into crucible, crucible places the vacuum chamber of vacuum system, crucible is an indirect heating, when crucible is heated to 300 ℃-380 ℃, selenium and zinc generation combination reaction, form the primary reaction resultant of zinc selenide (ZnSe), the primary reaction resultant of zinc selenide (ZnSe) is ground, place the vacuum heating anneal once more, annealing temperature is controlled at 550 ℃-700 ℃, and the time is can obtain highly purified zinc selenide (ZnSe) powdered material in 90 minutes.
The present invention is the preparation method of a kind of zinc selenide (ZnSe) powdered material, carries out according to the following step:
1) (1-1.35): 1 ratio is mixed simple substance selenium powder (Se) and simple substance zinc powder (Zn), stirs.
2) mixture that stirs is put into crucible, crucible tungsten filament indirect heating, and place the vacuum chamber of vacuum system.
3) vacuum is evacuated to 10 -1To 10 -2During Pa, heating crucible.When Heating temperature reached 300 ℃-380 ℃, mixture carried out combination reaction, generated the primary reaction thing.
4) the primary reaction thing grinds and is placed in the crucible, heating anneal under vacuum condition, and annealing temperature is 550 ℃-700 ℃, through annealing in 90 minutes, can obtain the higher zinc selenide of purity (ZnSe) powdered material.
Four, embodiment
Be described in further detail according to the embodiment that technical scheme of the present invention provides below in conjunction with the contriver.
Embodiment 1:
(1) by (1-1.35): 1 mol ratio is mixed simple substance selenium powder (Se) and simple substance zinc powder (Zn), stir, the selenium and the zinc powder mixture that stir are put into crucible, crucible is made with refractory ceramics, and use the tungsten filament indirect heating, place the vacuum chamber of vacuum system.
(2) vacuum with the vacuum chamber of vacuum system is evacuated to 10 -1To 10 -2During Pa, heating crucible.When Heating temperature reached 300 ℃-380 ℃, mixture began to carry out combination reaction, generated the primary reaction resultant of zinc selenide (ZnSe).
(3) zinc selenide (ZnSe) primary reaction resultant is taken out from vacuum chamber and grinds, after grinding, be positioned in the crucible heating anneal under vacuum condition once more.
(4) the joint annealing temperature is 550 ℃-700 ℃, carries out 90 minutes heating anneals.
(5) slowly reduce annealing temperature, when reaching room temperature, reactant is taken out, can obtain the higher zinc selenide of purity (ZnSe) powdered material.
Embodiment 2:
1) by (1-1.35): 1 mol ratio is mixed simple substance selenium powder (Se) and simple substance zinc powder (Zn), stir, the selenium and the zinc powder mixture that stir are put into crucible, crucible is made with refractory ceramics, and use the tungsten filament indirect heating, place the vacuum chamber of vacuum system.
2) vacuum of the vacuum chamber of vacuum system is evacuated to 10 -1To 10 -2During Pa, heating crucible.When Heating temperature reached 300 ℃-380 ℃, mixture began to carry out combination reaction, generated the primary reaction resultant of zinc selenide (ZnSe).
3) zinc selenide (ZnSe) primary reaction resultant takes out from vacuum chamber and grinds, and after grinding, is positioned in the crucible heating anneal under vacuum condition once more.
4) the joint annealing temperature is 550 ℃-700 ℃, carries out 90 minutes heating anneals.
5) reduce annealing temperature slowly, when reaching room temperature, reactant is taken out, can obtain the higher zinc selenide of purity (ZnSe) powdered material.

Claims (1)

1. the preparation method of a zinc selenide (ZnSe) powder is characterized in that, may further comprise the steps:
1) get simple substance selenium powder (Se) and simple substance zinc powder (Zn) (1-1.35) in molar ratio: 1 mixed stirs;
2) will the stir mixture of simple substance selenium powder (Se) and simple substance zinc powder (Zn) places crucible, places the vacuum chamber of vacuum system and vacuumizes;
3) be evacuated to 10 when vacuum -1To 10 -2During Pa, heating crucible, when Heating temperature reached 300 ℃-380 ℃, mixture carried out combination reaction, generated the primary reaction thing;
4) grinding of primary reaction thing is placed in the crucible, heating anneal under vacuum condition, annealing temperature is 550 ℃-700 ℃, the time is 90min, can obtain the higher zinc selenide of purity (ZnSe) powdered material.
CN 03134430 2003-07-23 2003-07-23 Process for preparing zinc selenide (zn se) powder material Expired - Fee Related CN1199851C (en)

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CN 03134430 CN1199851C (en) 2003-07-23 2003-07-23 Process for preparing zinc selenide (zn se) powder material

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Application Number Priority Date Filing Date Title
CN 03134430 CN1199851C (en) 2003-07-23 2003-07-23 Process for preparing zinc selenide (zn se) powder material

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CN1199851C CN1199851C (en) 2005-05-04

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100369817C (en) * 2006-02-16 2008-02-20 西安交通大学 Process for rapid heating preparation of zinc selenide nano-crystal film by tubular gas furnace
CN101025416B (en) * 2007-01-04 2011-11-23 山东师范大学 Luminescent zinc selenide nano rod synthesizing method and its use
CN101665245B (en) * 2008-09-01 2012-02-01 西北工业大学 Preparation method of zinc selenide polycrystalline material for single crystal growth
CN102586949A (en) * 2012-02-24 2012-07-18 长春理工大学 Method for preparing zinc selenide nanobelt
CN102586950A (en) * 2012-02-24 2012-07-18 长春理工大学 Method for preparing zinc selenide (ZnSe) nanofiber
CN102602898A (en) * 2012-02-24 2012-07-25 长春理工大学 Method for preparing monodisperse zinc selenide particles
CN106365130A (en) * 2016-09-13 2017-02-01 中国科学院理化技术研究所 Method for quickly preparing ZnSe powder
CN106477536B (en) * 2016-10-17 2018-10-16 西北工业大学 A kind of preparation method of ultra-high purity cadmium selenide polycrystalline material
CN109943884A (en) * 2019-03-28 2019-06-28 北京中材人工晶体研究院有限公司 A kind of zinc selenide raw material high temperature purification method
CN110255508A (en) * 2019-06-26 2019-09-20 南京睿扬光电技术有限公司 A kind of high performance zinc selenide mixing coating materials and its preparation process
CN114000108A (en) * 2021-10-30 2022-02-01 平顶山学院 Preparation method for embedding CdSe regulation and control layer in ZnSe/Si heterojunction interface

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100369817C (en) * 2006-02-16 2008-02-20 西安交通大学 Process for rapid heating preparation of zinc selenide nano-crystal film by tubular gas furnace
CN101025416B (en) * 2007-01-04 2011-11-23 山东师范大学 Luminescent zinc selenide nano rod synthesizing method and its use
CN101665245B (en) * 2008-09-01 2012-02-01 西北工业大学 Preparation method of zinc selenide polycrystalline material for single crystal growth
CN102586950B (en) * 2012-02-24 2013-10-23 长春理工大学 Method for preparing zinc selenide (ZnSe) nanofiber
CN102586950A (en) * 2012-02-24 2012-07-18 长春理工大学 Method for preparing zinc selenide (ZnSe) nanofiber
CN102602898A (en) * 2012-02-24 2012-07-25 长春理工大学 Method for preparing monodisperse zinc selenide particles
CN102586949B (en) * 2012-02-24 2013-10-23 长春理工大学 Method for preparing zinc selenide nanobelt
CN102602898B (en) * 2012-02-24 2013-10-23 长春理工大学 Method for preparing monodisperse zinc selenide particles
CN102586949A (en) * 2012-02-24 2012-07-18 长春理工大学 Method for preparing zinc selenide nanobelt
CN106365130A (en) * 2016-09-13 2017-02-01 中国科学院理化技术研究所 Method for quickly preparing ZnSe powder
CN106477536B (en) * 2016-10-17 2018-10-16 西北工业大学 A kind of preparation method of ultra-high purity cadmium selenide polycrystalline material
CN109943884A (en) * 2019-03-28 2019-06-28 北京中材人工晶体研究院有限公司 A kind of zinc selenide raw material high temperature purification method
CN110255508A (en) * 2019-06-26 2019-09-20 南京睿扬光电技术有限公司 A kind of high performance zinc selenide mixing coating materials and its preparation process
CN110255508B (en) * 2019-06-26 2023-06-30 南京睿扬光电技术有限公司 High-performance zinc selenide mixed film material and preparation process thereof
CN114000108A (en) * 2021-10-30 2022-02-01 平顶山学院 Preparation method for embedding CdSe regulation and control layer in ZnSe/Si heterojunction interface
CN114000108B (en) * 2021-10-30 2023-10-17 平顶山学院 Preparation method for embedding CdSe regulating layer at ZnSe/Si heterojunction interface

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