CN102086031A - Liquid-phase synthesis method of cadmium telluride - Google Patents
Liquid-phase synthesis method of cadmium telluride Download PDFInfo
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- CN102086031A CN102086031A CN 201010571424 CN201010571424A CN102086031A CN 102086031 A CN102086031 A CN 102086031A CN 201010571424 CN201010571424 CN 201010571424 CN 201010571424 A CN201010571424 A CN 201010571424A CN 102086031 A CN102086031 A CN 102086031A
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- temperature
- cadmium telluride
- cadmium
- phase synthesis
- silica tube
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- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000007791 liquid phase Substances 0.000 title claims abstract description 17
- 238000001308 synthesis method Methods 0.000 title abstract 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 19
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 16
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 16
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 18
- 238000003786 synthesis reaction Methods 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000000087 stabilizing effect Effects 0.000 abstract 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000011011 black crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a liquid-phase synthesis method of cadmium telluride. The liquid-phase synthesis method comprises the following steps of: taking tellurium and cadmium, uniformly mixing according to a mol ratio of 1:1, putting the mixture into a silica tube, starting a vacuum machine, evacuating and sealing the silica tube, arranging the sealed silica tube in a muffle furnace to heat in a heating mode of stepped temperature rise, finishing the reaction under a melting condition, cooling, discharging when the temperature of a furnace cavity is cooled to an approximate room temperature to obtain a product, i.e. cadmium telluride, wherein the raw materials of 5N tellurium and 5N cadmium are adopted; raising the temperature at a temperature raising speed of 80-100 DEG C/h and stabilizing the temperature at 100-700 DEG C for 5-10 h; and stabilizing the temperature at 1190-1200 DEG C for 1-3 h. The synthesis method of the cadmium telluride, which is provided by the invention, is a safe and high-efficiency process, generates no any other harmful substances in the preparation process and is simple in steps and easy to industrially popularize and apply.
Description
Technical field
The present invention relates to a kind of cadmium telluride synthesis technique, being meant a kind of especially is raw material with tellurium and cadmium, and heating fluid is combined to the method for cadmium telluride under high vacuum environment.
Background technology
Cadmium telluride density: 6.20, fusing point: 1041 ℃, the brownish black crystal powder, water insoluble and sour, in nitric acid, decompose.Cadmium telluride is used for spectroscopic analysis, also is used to make solar cell, infrared modulator, infrared window electroluminescent device, photocell, infrared acquisition, X ray detection, nuclear activity detector, near luminescent device of visible region etc.
The preparation method of common cadmium telluride mainly may further comprise the steps: tellurium and cadmium are mixed according to a certain ratio, and pellet is pulverized or ground to form to compound; Compound is packed in the silica tube into sealed after being vacuumized; Silica tube behind the good seal is put into the cadmium telluride synthetic furnace add the thermal synthesis cadmium telluride.
Summary of the invention
The problem that the present invention need solve provides a kind of liquid-phase synthesis process that adds the thermal synthesis cadmium telluride under high vacuum environment.
Designed a kind of cadmium telluride liquid-phase synthesis process according to the above-mentioned problem that needs to solve, this liquid-phase synthesis process step is as follows:
(1) get tellurium and cadmium, mixed was even in 1: 1 in molar ratio, batching 300～700g;
(2) compound in (1) is packed in the silica tube;
(3) start the vacuum machine, silica tube is vacuumized, vacuum tightness is 1 * 10
-1～1 * 10
-4Tube sealing behind the Pa;
(4) silica tube after will sealing places the retort furnace internal heating, and type of heating is a ladder-elevating temperature;
(5) cooling, discharging after the furnace chamber temperature is reduced near room temperature, products obtained therefrom is a cadmium telluride.
Wherein, the raw material that step (1) is used is 5N (being that purity is 99.999%, down together) tellurium and 5N cadmium.The heat-up rate of described step (4) is 80～100 ℃/hour, and constant temperature is 5～10 hours in 100～700 ℃ of scopes; Constant temperature is 1～3 hour in 1190～1200 ℃ scope.
Cadmium telluride synthetic method of the present invention is a kind of safe, technology efficiently, does not produce other objectionable impuritiess in the preparation process, and step is simple, is easy to industrialization promotion and uses.
Description of drawings
Accompanying drawing 1 is a cadmium telluride synthesis technique schematic flow sheet of the present invention.
Embodiment
Purport of the present invention provide a kind of with tellurium and cadmium raw material through after the suitable fragmentation, be heated to the cadmium telluride liquid-phase synthesis process that combination reaction generation cadmium telluride takes place after the molten state by metering than tellurium and cadmium being put into the vitreosil pipe.The invention will be further described below in conjunction with accompanying drawing.
With reference to accompanying drawing.The step of the inventive method is:
Cadmium telluride liquid phase synthesis and production process production process is:
(1) get tellurium and cadmium, mixed was even in 1: 1 in molar ratio, batching 300～700g;
(2) compound in (1) is packed in the silica tube;
(3) start the vacuum machine, silica tube is vacuumized, vacuum tightness is 1 * 10
-1～1 * 10
-4Tube sealing behind the Pa;
(4) silica tube after will sealing places the retort furnace internal heating, and type of heating is a ladder-elevating temperature;
(5) cooling, discharging after the furnace chamber temperature is reduced near room temperature, products obtained therefrom is a cadmium telluride.
Wherein, the raw material that uses of step (1) is 5N tellurium and 5N cadmium.The heat-up rate of described step (4) is 80～100 ℃/hour, and constant temperature is 5～10 hours in 100～700 ℃ of scopes; Constant temperature is 1～3 hour in 1190～1200 ℃ scope.
According to described step, enumerating following specific embodiment is reference.
Embodiment 1
A kind of cadmium telluride liquid phase synthesis and production process, process is as follows:
(1) 5N tellurium and 5N cadmium were mixed in 1: 1 in molar ratio after batching pulverizes, get 400g;
(2) getting compound is packed in the silica tube;
(3) start the vacuum machine, it is 1 * 10 that silica tube is evacuated to vacuum tightness
-2Tube sealing behind the Pa;
(4) silica tube after will sealing places in the retort furnace, opens heating system, heats up with 90 ℃/hour speed, 650 ℃ of constant temperature 10 hours; 1200 ℃ of constant temperature 2.5 hours.
(5) cooling, discharging after the furnace chamber temperature is reduced to room temperature promptly obtains 5N cadmium telluride product.
Embodiment 2
A kind of cadmium telluride liquid phase synthesis and production process, process is as follows:
(1) 5N tellurium and 5N cadmium are mixed the pulverizing of batching back in 1: 1 in molar ratio, get 550g;
(2) compound is packed in the silica tube;
(3) start the vacuum machine, it is 1 * 10 that silica tube is evacuated to vacuum tightness
-3Tube sealing behind the Pa;
(4) silica tube after will sealing places in the retort furnace, opens heating system, heats up with 100 ℃/hour speed, 500 ℃ of constant temperature 7 hours; 1190 ℃ of constant temperature 1.5 hours.
(5) cooling, discharging after the furnace chamber temperature is reduced near room temperature promptly obtains 5N cadmium telluride product.
Embodiment 3
A kind of cadmium telluride liquid phase synthesis and production process, process is as follows:
(1) be to mix batching 300g at 1: 1 in molar ratio with 5N tellurium and 5N cadmium;
(2) compound is packed in the silica tube;
(3) start the vacuum machine, it is 1 * 10 that silica tube is evacuated to vacuum tightness
-1Tube sealing behind the Pa;
(4) silica tube after will sealing places in the retort furnace, opens heating system, heats up with 80 ℃/hour speed, 400 ℃ of constant temperature 5 hours; 1200 ℃ of constant temperature 2 hours;
(5) cooling, discharging after the furnace chamber temperature is reduced near room temperature promptly obtains 5N cadmium telluride product.
Embodiment 4
A kind of cadmium telluride liquid phase synthesis and production process, process is as follows:
(1) be to mix batching 700g at 1: 1 in molar ratio with 5N tellurium and 5N cadmium;
(2) compound is packed in the silica tube;
(3) start the vacuum machine, it is 1 * 10 that silica tube is evacuated to vacuum tightness
-4Tube sealing behind the Pa;
(4) silica tube after will sealing places in the retort furnace, opens heating system, heats up with 100 ℃/hour speed, 2 hours, 700 ℃ constant temperature of 2 hours, 500～600 ℃ constant temperature of 2 hours, 250～350 ℃ constant temperature of 100 ℃ of constant temperature 2 hours; 1190 ℃ of constant temperature 2.0 hours;
(5) cooling, discharging after the furnace chamber temperature is reduced near room temperature promptly obtains 5N cadmium telluride product.
More than disclosed embodiment only be used for explaining treatment process of the present invention, the equivalent variations of doing according to the disclosure of invention still belongs to the invention protection domain.
Claims (3)
1. cadmium telluride liquid-phase synthesis process, this liquid-phase synthesis process step is as follows:
(1) get tellurium and cadmium, mixed was even in 1: 1 in molar ratio, batching 300～700g;
(2) compound in (1) is packed in the silica tube;
(3) start the vacuum machine, silica tube is vacuumized, vacuum tightness is 1 * 10
-1～1 * 10
-4Tube sealing behind the Pa;
(4) silica tube after will sealing places the retort furnace internal heating, and type of heating is a ladder-elevating temperature;
(5) cooling, discharging after the furnace chamber temperature is reduced near room temperature, products obtained therefrom is a cadmium telluride.
2. cadmium telluride liquid-phase synthesis process according to claim 1 is characterized in that: the raw material that step (1) is used is 5N tellurium and 5N cadmium.
3. cadmium telluride liquid-phase synthesis process according to claim 2 is characterized in that: the heat-up rate of described step (4) is 80～100 ℃/hour, and constant temperature is 5～10 hours in 100～700 ℃ of scopes; Constant temperature is 1～3 hour in 1190～1200 ℃ scope.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010571424 CN102086031A (en) | 2010-11-25 | 2010-11-25 | Liquid-phase synthesis method of cadmium telluride |
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|---|---|---|---|
| CN 201010571424 CN102086031A (en) | 2010-11-25 | 2010-11-25 | Liquid-phase synthesis method of cadmium telluride |
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| CN102086031A true CN102086031A (en) | 2011-06-08 |
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| CN 201010571424 Pending CN102086031A (en) | 2010-11-25 | 2010-11-25 | Liquid-phase synthesis method of cadmium telluride |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849693A (en) * | 2012-10-22 | 2013-01-02 | 四川大学 | High-temperature liquid-phase synthesis method of cadmium telluride powder |
| CN103274372A (en) * | 2013-06-18 | 2013-09-04 | 广东先导稀材股份有限公司 | Cadmium tellude preparation method |
| CN103420345A (en) * | 2012-05-22 | 2013-12-04 | 广东先导稀材股份有限公司 | Graphite crucible, heating furnace and preparation method for cadmium telluride |
| CN106241752A (en) * | 2016-09-20 | 2016-12-21 | 广东先导稀材股份有限公司 | A kind of preparation method of cuprous telluride |
| CN107188135A (en) * | 2016-03-14 | 2017-09-22 | 盱眙新远光学科技有限公司 | A kind of cadmium-telluride crystal |
| CN107522172A (en) * | 2017-07-31 | 2017-12-29 | 成都中建材光电材料有限公司 | A kind of preparation technology of cadmium antimonide powder |
| CN111204718A (en) * | 2020-02-28 | 2020-05-29 | 盱眙新远光学科技有限公司 | Low-temperature liquid phase preparation method of cadmium telluride crystal |
| CN114032609A (en) * | 2021-10-27 | 2022-02-11 | 安徽光智科技有限公司 | Growth method of cadmium telluride crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125679A (en) * | 2007-08-31 | 2008-02-20 | 侯仁义 | Method for preparing highly pure cadmium telluride |
| CN101734630A (en) * | 2009-12-30 | 2010-06-16 | 峨嵋半导体材料研究所 | Method for preparing high-purity cadmium telluride |
-
2010
- 2010-11-25 CN CN 201010571424 patent/CN102086031A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125679A (en) * | 2007-08-31 | 2008-02-20 | 侯仁义 | Method for preparing highly pure cadmium telluride |
| CN101734630A (en) * | 2009-12-30 | 2010-06-16 | 峨嵋半导体材料研究所 | Method for preparing high-purity cadmium telluride |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420345A (en) * | 2012-05-22 | 2013-12-04 | 广东先导稀材股份有限公司 | Graphite crucible, heating furnace and preparation method for cadmium telluride |
| CN103420345B (en) * | 2012-05-22 | 2015-04-22 | 广东先导稀材股份有限公司 | Graphite crucible, heating furnace and preparation method for cadmium telluride |
| CN102849693A (en) * | 2012-10-22 | 2013-01-02 | 四川大学 | High-temperature liquid-phase synthesis method of cadmium telluride powder |
| CN102849693B (en) * | 2012-10-22 | 2014-04-02 | 四川大学 | A kind of high temperature liquid phase synthesis method of cadmium telluride powder |
| CN103274372A (en) * | 2013-06-18 | 2013-09-04 | 广东先导稀材股份有限公司 | Cadmium tellude preparation method |
| CN103274372B (en) * | 2013-06-18 | 2014-12-10 | 广东先导稀材股份有限公司 | Cadmium tellude preparation method |
| CN107188135A (en) * | 2016-03-14 | 2017-09-22 | 盱眙新远光学科技有限公司 | A kind of cadmium-telluride crystal |
| CN106241752A (en) * | 2016-09-20 | 2016-12-21 | 广东先导稀材股份有限公司 | A kind of preparation method of cuprous telluride |
| CN106241752B (en) * | 2016-09-20 | 2018-07-06 | 广东先导稀材股份有限公司 | A kind of preparation method of cuprous telluride |
| CN107522172A (en) * | 2017-07-31 | 2017-12-29 | 成都中建材光电材料有限公司 | A kind of preparation technology of cadmium antimonide powder |
| CN111204718A (en) * | 2020-02-28 | 2020-05-29 | 盱眙新远光学科技有限公司 | Low-temperature liquid phase preparation method of cadmium telluride crystal |
| CN114032609A (en) * | 2021-10-27 | 2022-02-11 | 安徽光智科技有限公司 | Growth method of cadmium telluride crystal |
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Application publication date: 20110608 |