CN103496678A - Cadmium telluride synthesizing device and method - Google Patents

Cadmium telluride synthesizing device and method Download PDF

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CN103496678A
CN103496678A CN201310497858.9A CN201310497858A CN103496678A CN 103496678 A CN103496678 A CN 103496678A CN 201310497858 A CN201310497858 A CN 201310497858A CN 103496678 A CN103496678 A CN 103496678A
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cadmium
reaction chamber
tellurium
adds
material container
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CN201310497858.9A
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CN103496678B (en
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谈逊
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Huaxia Semiconductor Shenzhen Co ltd
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Abstract

The invention discloses a cadmium telluride synthesizing device. The cadmium telluride synthesizing device comprises a heating reaction chamber which is used for achieving reaction of reaction raw materials in the atomization state, wherein the upper portion of the reaction chamber is connected with a tellurium feeding furnace and a cadmium feeding furnace, a discharge outlet in the lower portion of the reaction chamber is connected with a collector, a heating device is arranged on the outer side of the reaction chamber, a tellurium feeding container is arranged on the tellurium feeding furnace, a tellurium atomizer is arranged on a pipeline which enables the tellurium feeding container to be connected with the reaction chamber, a heating device is arranged on the outer side of the tellurium feeding container, a cadmium feeding container is arranged on the cadmium feeding furnace, a cadmium atomizer is arranged on a pipeline which enables the cadmium feeding container to be connected with the reaction chamber, and a heating device is arranged on the outer side of the cadmium feeding container. The invention further discloses a cadmium telluride synthesizing method. According to the cadmium telluride synthesizing device and method, tellurium and cadmium which are atomized are made to rotate round and round, the reaction time is prolonged, the tellurium and cadmium can be mixed and reacted fully, and high-purity cadmium telluride alloy powder is obtained.

Description

A kind of cadmium telluride synthesizer and method
Technical field
This area belongs to chemical technology field, relates to a kind of method of cadmium telluride synthesizer and synthetic cadmium telluride.
Background technology
The crystalline compounds that cadmium telluride is comprised of tellurium element and cadmium element, its energy gap is generally 1.45eV, is desirable photoelectric conversion material, can be for spectroscopic analysis, CO 2the Q modulation of laser apparatus, also can be for making solar cell, infrared modulator, Hg xcd 1-xte substrate, infrared window electroluminescent device, photocell, infrared acquisition, X-ray detector, nuclear activity detector, approach the luminescent device of visible region etc.Polycrystalline cadmium telluride alloy powder is the key core material for preparing the solar cell Cadimium telluride thin film.
At present domesticly mainly with pressed powder or the synthetic cadmium telluride of particle high-temperature, will first every part of tellurium material and cadmium material alternately be added to silica tube, deoxidation steep and carry out the sintering tube sealing by envelope after charging, slowly carry out the building-up reactions of High Temperature High Pressure.Its advantage is: vapour pressure and heat that process produces are not very large, and experimental installation and operation are simpler.Weak point is: the building-up process tube sealing of need to feeding, and broken pipe feeding, can not realize serialization production, output is not high and reaction time is long; The cadmium telluride of preparation easily lumps in addition, needs the attrition process powdered, and this process is easily introduced again impurity etc., causes product purity not high.
A kind of feasible mode is that the cadmium telluride reaction unit is arranged to Y shape, looks the problem of can serialization producing, still, this structure, owing to being difficult to control reaction time, not only reaction efficiency is low, and the final product quality of cadmium telluride is not high, is difficult to use in suitability for industrialized production.
Summary of the invention
The object of the invention is to for above-mentioned deficiency of the prior art, a kind of cadmium telluride synthesizer that can be used in suitability for industrialized production is provided.
Another object of the present invention is, for above-mentioned the deficiencies in the prior art, provides a kind of cadmium telluride synthetic method that improves the cadmium telluride final product quality.
For achieving the above object, the technical scheme that the present invention takes is: a kind of cadmium telluride synthesizer is provided, it is characterized in that, comprise the reacting by heating chamber of reaction raw materials being reacted under atomizing state for realizing; Described reaction chamber top is connected with the reinforced stove of cadmium with the reinforced stove of tellurium respectively; The discharge port of described reaction chamber bottom is connected with collector; The arranged outside of described reaction chamber has heating unit; The reinforced stove of described tellurium is provided with tellurium and adds material container; Described tellurium adds on the pipeline that material container is connected with reaction chamber and is provided with the tellurium spraying gun; The arranged outside that described tellurium adds material container has heating unit; The reinforced stove of described cadmium is provided with cadmium and adds material container; Described cadmium adds on the pipeline that material container is connected with reaction chamber and is provided with the cadmium spraying gun; The arranged outside that described cadmium adds material container has heating unit.
The lower end that described tellurium adds material container is provided with flow valve.The lower end that described cadmium adds material container is provided with flow valve.Described tellurium adds pipeline that material container is connected with reaction chamber and cadmium and adds on the pipeline that material container is connected with reaction chamber and be respectively arranged with gas inlet; Described tellurium adds pipeline that material container is connected with reaction chamber and cadmium and adds the pipeline arranged outside that material container is connected with reaction chamber heating unit is arranged.
Be provided with strainer on the pipeline that the discharge port of described reaction chamber bottom is connected with collector; The pipeline arranged outside that the discharge port of described reaction chamber bottom is connected with collector has heating unit.
A kind of optimal way of reaction chamber is: described reaction chamber cross section is taper; In described reaction chamber, central position is provided with rotating shaft.Described reaction chamber bottom discharge port also is provided with for controlling the elevating lever of cadmium telluride load.Be provided with gas passage on described elevating lever.Described reaction chamber top also is provided with gas inlet.
The another kind of optimal way of reaction chamber is: described reaction chamber is helix; The reaction chamber outside is along the spiral tube axis shaft to being provided with heater strip.
A kind of cadmium telluride synthetic method, is characterized in that, comprises the following steps:
Step a, Raw material processing, heat raw material tellurium and cadmium, melt respectively, obtains liquid tellurium and cadmium;
Step b, raw material reaction, the reaction chamber reaction that liquid tellurium and cadmium enter after vacuumizing after atomization obtains cadmium antimonide powder; And lead to argon gas in reaction chamber simultaneously;
Step c, collect cadmium antimonide powder, and the cadmium antimonide powder obtained from reaction chamber lower end discharge port is collected by collector.
Cadmium telluride synthetic technology scheme provided by the invention has following beneficial effect:
1, by making tellurium and cadmium after atomization do cyclotron motion, when extending the reaction times, can make tellurium fully mix, react with cadmium, obtain high-purity cadmium telluride alloy powder;
2, the elevating lever of reaction chamber discharge port setting can be controlled reaction efficiency and the reaction times of raw material tellurium and cadmium;
3, the gas passed into, can increase the touch opportunity of tellurium and cadmium, improves reaction efficiency.
The accompanying drawing explanation
Accompanying drawing described herein is used to provide the further understanding to the application, forms the application's a part, and the application's schematic description and description is for explaining the application, and formation is to the application's improper restriction.In the accompanying drawings:
Fig. 1 schematically shows the front view according to the cadmium telluride synthesizer of the application's a embodiment;
Fig. 2 schematically shows the sectional view of Fig. 1 along the A-A line;
Fig. 3 schematically shows the front view according to the cadmium telluride synthesizer of another embodiment of the application; And
Fig. 4 schematically shows the sectional view of Fig. 3 along the B-B line.
In these accompanying drawings, with identical reference number, mean same or analogous part.
Embodiment
For the purpose, technical scheme and the advantage that make the application is clearer, below in conjunction with drawings and the specific embodiments, the application is described in further detail.
In the following description, quoting of " embodiment ", " embodiment ", " example ", " example " etc. shown to embodiment or the example so described can comprise special characteristic, structure, characteristic, character, element or limit, but be not that each embodiment or example must comprise special characteristic, structure, characteristic, character, element or limit.In addition, reuse phrase " according to the application's a embodiment " and, although be likely to refer to identical embodiment, not must refer to identical embodiment.
For the sake of simplicity, omitted in below describing and well known to a person skilled in the art some technical characterictic.
The invention discloses a kind of cadmium telluride synthesizer.
Fig. 1 schematically shows the front view according to the cadmium telluride synthesizer of the application's a embodiment; Fig. 2 schematically shows the sectional view of Fig. 1 along the A-A line.
According to the application's a embodiment, above-mentioned cadmium telluride synthesizer comprises the reacting by heating chamber 5 of reaction raw materials being reacted under atomizing state for realizing.Reaction chamber 5 tops are connected with the reinforced stove 3 of cadmium with the reinforced stove 1 of tellurium respectively.The discharge port of reaction chamber 5 bottoms is connected with collector 8.The arranged outside of reaction chamber 5 has heating unit 51, for the raw material in reaction chamber 5, is heated.The reinforced stove 1 of tellurium is provided with tellurium and adds material container 11.Tellurium adds on the pipeline that material container 11 is connected with reaction chamber 5 and is provided with tellurium spraying gun 13, for obtaining the tellurium of atomization.The arranged outside that tellurium adds material container 1 has heating unit, for the raw material tellurium by solid-state, melts.The reinforced stove 3 of cadmium is provided with cadmium and adds material container 31.Cadmium adds on the pipeline that material container 31 is connected with reaction chamber 5 and is provided with cadmium spraying gun 33, for obtaining the cadmium of atomization.The arranged outside that cadmium adds material container 31 has heating unit, for the raw material tellurium by solid-state, melts.
According to the application's a embodiment, reaction chamber 5 cross sections can be taper; Reaction chamber 5 can be conical structure, frustum cone structure, pyramidal structure or terrace with edge structure etc., is mainly that an inclined-plane of down sliding is sideling arranged, and the cadmium antimonide powder of being convenient to obtain after reaction is slipped to bottom.
According to the application's a embodiment, the interior central position of reaction chamber 5 can be provided with rotating shaft.Rotating shaft is rotated under driven by motor, thereby the tellurium, the cadmium that drive after atomization are done turning motion along the inwall of reaction chamber 5.
According to the application's a embodiment, reaction chamber 5 bottom discharge ports further can be provided with the elevating lever 9 for controlling the cadmium telluride load.Elevating lever 9 heads are taper, can with reaction chamber 5 inwalls between form the passage of the pipeline 6 that space is connected with collector 8 as falling into of synthetic cadmium antimonide powder.Can be provided with gas passage 10 on elevating lever 9, for passing into gas, the gas passed into, under the drive of rotating shaft, is also done cyclotron motion, improves the reaction efficiency of raw material tellurium and cadmium.By the lifting process of elevating lever 9, can change the air flow line of the gas in reaction chamber 5, change the tellurium and the kinestate of cadmium in reaction chamber 5 by the motion of gas, and then affect the reaction times of tellurium and cadmium, thus realization to reactant whereabouts flow regulation and control.For example, when elevating lever 9 rises, the gas flow in reaction chamber 5 upwards, drives raw material tellurium and cadmium and move upward, thereby the kinestate of feed change tellurium and cadmium has extended the reaction times, has guaranteed that reaction is more abundant, and reaction efficiency is provided.
According to the application's a embodiment, elevating lever 9 heads can be tapered, and the space that pyramidal structure bottom and reaction chamber 5 inwalls form is the whereabouts passage of cadmium telluride reactant.If gap length is h, by the lifting of elevating lever 9, just can change gap length h.
According to the application's a embodiment, reaction chamber 5 tops can further be provided with gas inlet 2, and for passing into gas, this gas can be argon gas, and the argon gas passed into, under the drive of rotating shaft, is also done cyclotron motion, improve the reaction efficiency of raw material tellurium and cadmium.
According to the application's a embodiment, reaction chamber 5 can be arranged in Reaktionsofen shell 4.
According to the application's a embodiment, the lower end that tellurium adds material container 11 can be provided with flow valve 14, for control, enter reaction chamber 5 the raw material tellurium the number and speed, and then further control amount and the speed of participating in reaction; Same, the lower end that cadmium adds material container 31 is provided with flow valve 34.
According to the application's a embodiment, tellurium adds pipeline that material container 11 is connected with reaction chamber 5 and cadmium and adds on the pipeline that material container 31 is connected with reaction chamber 5 and be respectively arranged with gas inlet, for adding to tellurium or the required gas of cadmium atomization, as argon gas; Tellurium adds pipeline that material container 11 is connected with reaction chamber 5 and cadmium and adds the pipeline arranged outside that material container 31 is connected with reaction chamber 5 heating unit is arranged, for keeping tellurium and cadmium in melted state.
The embodiment according to the application, be provided with strainer 7 on the pipeline 6 that the discharge port of reaction chamber 5 bottoms is connected with collector 8, for being recycled after the unreacted tellurium that filters out tail gas and cadmium; Pipeline 6 Outboard Sections that the discharge port of reaction chamber 5 bottoms is connected with collector 8 are provided with heating unit 61, complete for guaranteeing tellurium and cadmium reaction.
According to the application's a embodiment, this cadmium telluride synthesizer can be symmetrically arranged with the reinforced stove 1 of at least one tellurium and the reinforced stove 3 of cadmium, and as be provided with the reinforced stove 1 of two telluriums and two reinforced stoves 3 of cadmium, they are uniformly distributed along Reaktionsofen shell 4.This cadmium telluride synthesizer also is provided with at least one gas inlet 2, and as be provided with, four gas inletes 2 are evenly distributed on the reinforced stove 1 of two telluriums and two cadmiums feed in raw material between stove 3.
Fig. 3 schematically shows the front view according to the cadmium telluride synthesizer of another embodiment of the application; Fig. 4 schematically shows the sectional view of Fig. 3 along the B-B line.
According to another embodiment of the application, reaction chamber 5 ' can also be helix; Reaction chamber 5 outsides along the spiral tube axis shaft to be provided with heater strip 51 ', for reaction chamber 5 ' interior raw material is heated.The reinforced stove entrance of reaction chamber 5 ' above be respectively arranged with tellurium and the reinforced stove entrance of cadmium.
The embodiment according to the application, reaction chamber 4 tops radially can further arrange gas inlet along spiral tube, for passing into gas, this gas can be argon gas, and the place that the tellurium after the argon gas atomization passed into and cadmium are large by pressure along spiral tube is diffused into the place that pressure is little.In the process of argon gas diffusion, be equivalent to extend the reaction times of tellurium and cadmium after the atomization, and then the reaction efficiency of raising tellurium and cadmium.
According to the application's a embodiment, the above-mentioned heating unit of mentioning can be by electrically heated device, as electrical heater, will upper heater strip be set around the device of needs heating.
The application also provides a kind of cadmium telluride synthetic method.
Cadmium telluride synthetic method under the embodiment detailed analysis of first device provided below in conjunction with the application specifically comprises the following steps:
Step a, Raw material processing, heat raw material tellurium and cadmium, melt respectively, obtains liquid tellurium and cadmium.
According to the application's a embodiment, can utilize the reinforced stove 1 of tellurium and the reinforced stove 3 of cadmium that raw material tellurium and cadmium can be heated to respectively to 450 ℃ and 320 ℃ of fusings, obtain liquid tellurium and cadmium.
The embodiment according to the application, can first be processed into particulate state by raw material tellurium and cadmium, then the heating of the raw material tellurium after processing and cadmium, fusing, can shorten fusing time like this, improves energy utilization rate, reaches energy-conservation purpose.
Step b, raw material reaction, reaction chamber 5 reactions that liquid tellurium and cadmium enter after vacuumizing after atomization obtain cadmium antimonide powder; And simultaneously to the interior logical argon gas of reaction chamber 5.
According to the application's a embodiment, can utilize tellurium spraying gun 13 and cadmium spraying gun 33 to add argon gas by liquid tellurium and cadmium atomization.Can control the intensity of the argon gas added at 1.5MPa.
According to the application's a embodiment, before reaction, the vacuum tightness in reaction chamber 5 can remain on 1*10 -3below Pa.
According to the application's a embodiment, in reaction process, can guarantee that the temperature of reaction chamber 5 is at 800 ℃.
According to the application's a embodiment, the pressure of the argon gas entered by gas inlet 2 can remain on 1.5MPa.
According to the application's a embodiment, can the reaction process after tellurium and cadmium reaction in, by regulating the lifting of elevating lever 9, adjust the reaction times of reactant.When raw material is less, can control elevating lever motionless, when raw material is more, can controls elevating lever and rise to extend the reaction times.
According to the application's a embodiment, when elevating lever 9 is provided with gas passage 10, the pressure of the argon gas entered along gas passage 10 can be controlled at 0.5MPa.
Step c, collect cadmium antimonide powder, and the cadmium antimonide powder obtained from reaction chamber 5 lower end discharge ports is collected by collector 8.
According to the application's a embodiment, the temperature of the pipeline that the discharge port of reaction chamber 5 bottoms can be connected with collector 8 is controlled at 1150 ℃, to guarantee that tellurium fully reacts with cadmium.
According to the application's a embodiment, in technique scheme, adopt argon gas to realize the atomization to tellurium and cadmium; In fact, with tellurium and the nonreactive any gas of cadmium, can realize above-mentioned functions, can be as the substitute of argon gas, special rare gas element helium, neon, Krypton and xenon etc., all can realize above-mentioned functions.In addition, the gas entered from the gas passage 10 of the first implement device also is not limited to argon gas, can be can realize adjusting tellurium in reaction chamber 5 and cadmium reaction time and not with any gas of tellurium, cadmium reaction, preferably rare gas element, comprise helium, neon, argon gas, Krypton, xenon.
The foregoing is only the application's embodiment, be not limited to the application, for a person skilled in the art, the application can have various modifications and variations.All within the application's spirit and principle, any modification of doing, be equal to replacement, improvement etc., within all should being included in the application's claim scope.

Claims (10)

1. a cadmium telluride synthesizer, is characterized in that, comprises the reacting by heating chamber of reaction raw materials being reacted under atomizing state for realizing; Described reaction chamber top is connected with the reinforced stove of cadmium with the reinforced stove of tellurium respectively; The discharge port of described reaction chamber bottom is connected with collector; The arranged outside of described reaction chamber has heating unit; The reinforced stove of described tellurium is provided with tellurium and adds material container; Described tellurium adds on the pipeline that material container is connected with reaction chamber and is provided with the tellurium spraying gun; The arranged outside that described tellurium adds material container has heating unit; The reinforced stove of described cadmium is provided with cadmium and adds material container; Described cadmium adds on the pipeline that material container is connected with reaction chamber and is provided with the cadmium spraying gun; The arranged outside that described cadmium adds material container has heating unit.
2. cadmium telluride synthesizer according to claim 1, is characterized in that, the lower end that described tellurium adds material container is provided with flow valve; The lower end that described cadmium adds material container is provided with flow valve.
3. cadmium telluride synthesizer according to claim 1 and 2, is characterized in that, described tellurium adds pipeline that material container is connected with reaction chamber and cadmium and adds on the pipeline that material container is connected with reaction chamber and be respectively arranged with gas inlet; Described tellurium adds pipeline that material container is connected with reaction chamber and cadmium and adds the pipeline arranged outside that material container is connected with reaction chamber heating unit is arranged.
4. cadmium telluride synthesizer according to claim 1, is characterized in that, on the pipeline that the discharge port of described reaction chamber bottom is connected with collector, is provided with strainer; The pipeline arranged outside that the discharge port of described reaction chamber bottom is connected with collector has heating unit.
5. cadmium telluride synthesizer according to claim 1, is characterized in that, described reaction chamber cross section is taper; In described reaction chamber, central position is provided with rotating shaft.
6. cadmium telluride synthesizer according to claim 1, is characterized in that, described reaction chamber bottom discharge port also is provided with for controlling the elevating lever of cadmium telluride load.
7. cadmium telluride synthesizer according to claim 6, is characterized in that, on described elevating lever, is provided with gas passage.
8. cadmium telluride synthesizer according to claim 1, is characterized in that, described reaction chamber top also is provided with gas inlet.
9. cadmium telluride synthesizer according to claim 1 and 2, is characterized in that, described reaction chamber is helix; The reaction chamber outside is along the spiral tube axis shaft to being provided with heater strip.
10. a cadmium telluride synthetic method, is characterized in that, comprises the following steps:
Step a, Raw material processing, heat raw material tellurium and cadmium, melt respectively, obtains liquid tellurium and cadmium;
Step b, raw material reaction, the reaction chamber reaction that liquid tellurium and cadmium enter after vacuumizing after atomization obtains cadmium antimonide powder; And lead to argon gas in reaction chamber simultaneously;
Step c, collect cadmium antimonide powder, and the cadmium antimonide powder obtained from reaction chamber lower end discharge port is collected by collector.
CN201310497858.9A 2013-10-22 2013-10-22 Cadmium telluride synthesizing device and method Active CN103496678B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116555912A (en) * 2023-05-29 2023-08-08 武汉拓材科技有限公司 Preparation device of cadmium telluride polycrystal material

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CN202638015U (en) * 2012-05-15 2013-01-02 常州市先导干燥设备有限公司 High-temperature thermal decomposition spray device
CN203525719U (en) * 2013-10-22 2014-04-09 谈逊 High-temperature cadmium telluride synthesizing device
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CN116555912B (en) * 2023-05-29 2023-10-31 武汉拓材科技有限公司 Preparation device of cadmium telluride polycrystal material

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