CN103496678B - Cadmium telluride synthesizing device and method - Google Patents

Cadmium telluride synthesizing device and method Download PDF

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CN103496678B
CN103496678B CN201310497858.9A CN201310497858A CN103496678B CN 103496678 B CN103496678 B CN 103496678B CN 201310497858 A CN201310497858 A CN 201310497858A CN 103496678 B CN103496678 B CN 103496678B
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cadmium
tellurium
reative cell
raw material
addition vessel
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CN103496678A (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 synthesis cadmium telluride.
Background technology
The crystalline compounds that cadmium telluride is made up of tellurium element and cadmium element, its energy gap is generally 1.45eV, is desirable photoelectric conversion material, may be used for spectrum analysis, CO 2the Q modulation of laser instrument, also may be used for making solar cell, infrared modulator, Hg xcd 1-xte substrate, infrared window electroluminescent device, photocell, infrared acquisition, X-ray detector, nuclear activity detector, luminescent device etc. close to visible region.Polycrystalline cadmium telluride alloy powder is the key core material preparing solar cell Cadimium telluride thin film.
Current domestic main pressed powder or particle high-temperature synthesis cadmium telluride, first every part of tellurium material and cadmium material alternately will be added quartz ampoule, deoxidation after charging also carries out sintering tube sealing with envelope bubble, slowly carries out the synthetic reaction of HTHP.Its advantage is: the vapour pressure that process produces and heat are not very large, and experimental facilities is simpler with operation.Weak point is: building-up process needs tube sealing of feeding, broken pipe feeding, and can not realize continuous prodution, output is not high and reaction time is long; The cadmium telluride prepared in addition easily lumps, and needs attrition process powdered, and this process easily introduces impurity etc. again, causes product purity not high.
Feasible mode is that cadmium telluride reaction unit is arranged to a Y shape, and looking can the problem of continuous prodution, but, this structure, owing to being difficult to control reaction time, not only reaction efficiency is low, and the end 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 improving cadmium telluride end product quality.
For achieving the above object, the technical scheme that the present invention takes is: provide a kind of cadmium telluride synthesizer, it is characterized in that, comprises and adds thermal reaction chamber for what realize reaction raw materials to react under spray pattern; Described reative cell top stove and the cadmium stove that feeds in raw material that feeds in raw material with tellurium is respectively connected; The discharging opening of described reative cell bottom is connected with collector; The arranged outside of described reative cell has heater; The described tellurium stove that feeds in raw material is provided with tellurium addition vessel; The pipeline that described tellurium addition vessel is connected with reative cell is provided with tellurium atomizer; The arranged outside of described tellurium addition vessel has heater; The described cadmium stove that feeds in raw material is provided with cadmium addition vessel; The pipeline that described cadmium addition vessel is connected with reative cell is provided with cadmium atomizer; The arranged outside of described cadmium addition vessel has heater.
The lower end of described tellurium addition vessel is provided with flow valve.The lower end of described cadmium addition vessel is provided with flow valve.The pipeline that described tellurium addition vessel is connected with reative cell and the pipeline that cadmium addition vessel is connected with reative cell are respectively arranged with gas access; The pipeline that described tellurium addition vessel is connected with reative cell and the pipeline arranged outside that cadmium addition vessel is connected with reative cell have heater.
The pipeline that the discharging opening of described reative cell bottom is connected with collector is provided with filter; The pipeline arranged outside that the discharging opening of described reative cell bottom is connected with collector has heater.
A kind of preferred embodiment of reative cell is: described reative cell cross section is taper; In described reative cell, center is provided with rotating shaft.Described reative cell bottom discharging opening is also provided with the elevating lever for controlling cadmium telluride load.Described elevating lever is provided with gas passage.Described reative cell top is also provided with gas access.
The another kind of preferred embodiment of reative cell is: described reative cell is helix; Along helix tube axis shaft to being provided with heater strip outside reative cell.
A kind of cadmium telluride synthetic method, is characterized in that, comprise the following steps:
Step a, Raw material processing, heat raw material tellurium and cadmium, melt respectively, obtain liquid tellurium and cadmium;
Step b, raw material reaction, liquid tellurium and cadmium enter the reative cell after vacuumizing and are obtained by reacting cadmium antimonide powder after atomization; And in reative cell, lead to argon gas simultaneously;
Step c, collect cadmium antimonide powder, the cadmium antimonide powder obtained from reative cell lower end discharging opening is collected by collector.
Cadmium telluride synthetic technology scheme provided by the invention has following beneficial effect:
1, by making the tellurium after atomization and cadmium do circumnutation, while the prolongation reaction time, tellurium can be made fully to mix with cadmium, react, obtain high-purity cadmium telluride alloy powder;
2, the elevating lever that reative cell discharging opening is arranged can control reaction efficiency and the reaction time of raw material tellurium and cadmium;
3, the gas passed into, can increase the touch opportunity of tellurium and cadmium, improves reaction efficiency.
Accompanying drawing explanation
Accompanying drawing described herein is used to provide further understanding of the present application, forms a application's part, and the schematic description and description of the application for explaining the application, and forms the improper restriction to the application.In the accompanying drawings:
Fig. 1 schematically shows the front view of the cadmium telluride synthesizer of an embodiment according to the application;
Fig. 2 schematically shows the sectional view of Fig. 1 along A-A line;
Fig. 3 schematically shows the front view of the cadmium telluride synthesizer of another embodiment according to the application; And
Fig. 4 schematically shows the sectional view of Fig. 3 along B-B line.
In the drawings, use identical reference number to represent same or analogous part.
Detailed description of the invention
For making the object of the application, technical scheme and advantage clearly, 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. is shown that the embodiment of so description or example can comprise special characteristic, structure, characteristic, character, element or limit, but not each embodiment or example must comprise special characteristic, structure, characteristic, character, element or limit.In addition, reuse phrase " embodiment according to the application " although be likely refer to identical embodiment, and not necessarily refers to identical embodiment.
For the sake of simplicity, eliminate in below describing and well known to a person skilled in the art some technical characteristic.
The invention discloses a kind of cadmium telluride synthesizer.
Fig. 1 schematically shows the front view of the cadmium telluride synthesizer of an embodiment according to the application; Fig. 2 schematically shows the sectional view of Fig. 1 along A-A line.
According to an embodiment of the application, above-mentioned cadmium telluride synthesizer comprises and adds thermal reaction chamber 5 for what realize reaction raw materials to react under spray pattern.Reative cell 5 top stove 1 and the cadmium stove 3 that feeds in raw material that feeds in raw material with tellurium is respectively connected.The discharging opening of reative cell 5 bottom is connected with collector 8.The arranged outside of reative cell 5 has heater 51, for heating the raw material in reative cell 5.The tellurium stove 1 that feeds in raw material is provided with tellurium addition vessel 11.The pipeline that tellurium addition vessel 11 is connected with reative cell 5 is provided with tellurium atomizer 13, for obtaining the tellurium of atomization.The arranged outside of tellurium addition vessel 1 has heater, for being melted by solid-state raw material tellurium.The cadmium stove 3 that feeds in raw material is provided with cadmium addition vessel 31.The pipeline that cadmium addition vessel 31 is connected with reative cell 5 is provided with cadmium atomizer 33, for obtaining the cadmium of atomization.The arranged outside of cadmium addition vessel 31 has heater, for being melted by solid-state raw material tellurium.
According to an embodiment of the application, reative cell 5 cross section can be taper; Reative cell 5 can be conical structure, frustum cone structure, pyramidal structure or terrace with edge structure etc., mainly have one can the inclined-plane of slide downward sideling, the cadmium antimonide powder being convenient to obtain after reacting is slipped to bottom.
According to an embodiment of the application, in reative cell 5, center can be provided with rotating shaft.Rotating shaft rotates under driven by motor, thus drives tellurium, cadmium after atomization to do gyration along the inwall of reative cell 5.
According to an embodiment of the application, reative cell 5 bottom discharging opening can be provided with the elevating lever 9 for controlling cadmium telluride load further.Elevating lever 9 head is taper, can with form the passage that fall into the pipeline 6 that with collector 8 be connected of space as the cadmium antimonide powder synthesized between reative cell 5 inwall.Elevating lever 9 can be provided with gas passage 10, and for passing into gas, the gas passed into, under the drive of rotating shaft, also does circumnutation, improves the reaction efficiency of raw material tellurium and cadmium.By the lifting process of elevating lever 9, the airflow direction of the gas in reative cell 5 can be changed, be changed the motion state of the tellurium in reative cell 5 and cadmium by the motion of gas, and then affect the reaction time of tellurium and cadmium, thus realization to reactant whereabouts flow regulation and control.Such as, when elevating lever 9 rises, the gas flow in reative cell 5 upwards, drives raw material tellurium and cadmium to move upward, thus the motion state of feed change tellurium and cadmium, extend the reaction time, ensure that reaction is more abundant, reaction efficiency is provided.
According to an embodiment of the application, elevating lever 9 head can be tapered, and the space formed with reative cell 5 inwall bottom pyramidal structure is the dropping channel of cadmium telluride reactant.If gap length is h, by the lifting of elevating lever 9, just gap length h can be changed.
According to an embodiment of the application, reative cell 5 top can be provided with gas access 2 further, and for passing into gas, this gas can be argon gas, and the argon gas passed into, under the drive of rotating shaft, also does circumnutation, improves the reaction efficiency of raw material tellurium and cadmium.
According to an embodiment of the application, reative cell 5 can be arranged in reacting furnace shell 4.
According to an embodiment of the application, the lower end of tellurium addition vessel 11 can be provided with flow valve 14, for the raw material tellurium that controls to enter reative cell 5 number and speed, and then control amount and the speed of participating in reaction further; Same, the lower end of cadmium addition vessel 31 is provided with flow valve 34.
According to an embodiment of the application, the pipeline that tellurium addition vessel 11 is connected with reative cell 5 and the pipeline that cadmium addition vessel 31 is connected with reative cell 5 are respectively arranged with gas access, for adding the gas needed for tellurium or cadmium atomization, as argon gas; The pipeline that tellurium addition vessel 11 is connected with reative cell 5 and the pipeline arranged outside that cadmium addition vessel 31 is connected with reative cell 5 have heater, are in molten state for keeping tellurium and cadmium.
According to an embodiment of the application, the pipeline 6 that the discharging opening of reative cell 5 bottom is connected with collector 8 is provided with filter 7, recycles after filtering out unreacted tellurium in tail gas and cadmium; Pipeline 6 Outboard Sections that the discharging opening of reative cell 5 bottom is connected with collector 8 is provided with heater 61, for ensure tellurium and cadmium reaction complete.
According to an embodiment of the application, this cadmium telluride synthesizer can be symmetrically arranged with feed in raw material stove 1 and cadmium of at least one tellurium and to feed in raw material stove 3, and to feed in raw material stove 3 as being provided with feed in raw material stove 1 and two cadmiums of two telluriums, they are uniformly distributed along reacting furnace shell 4.This cadmium telluride synthesizer is also provided with at least one gas access 2, is evenly distributed on feed in raw material stove 1 and two cadmiums of two telluriums feeds in raw material between stove 3 as being provided with four gas accesses 2.
Fig. 3 schematically shows the front view of the cadmium telluride synthesizer of another embodiment according to the application; Fig. 4 schematically shows the sectional view of Fig. 3 along B-B line.
According to another embodiment of the application, reative cell 5 ' can also be helix; Along helix tube axis shaft to being provided with heater strip 51 ' outside reative cell 5, heat for the raw material interior to reative cell 5 '.Reative cell 5 ' is respectively arranged with feed in raw material stove entrance and cadmium of tellurium to feed in raw material stove entrance.
According to an embodiment of the application, reative cell 4 top can arrange gas access further along helix tube radial direction, for passing into gas, this gas can be argon gas, and the tellurium after the argon gas atomization passed into and cadmium are diffused into the little place of pressure along helix tube by the place that pressure is large.In the process of argon gas diffusion, be equivalent to the reaction time extending the rear tellurium of atomization and cadmium, and then improve the reaction efficiency of tellurium and cadmium.
According to an embodiment of the application, the above-mentioned heater mentioned can be by electrically heated device, as electric furnace, arranges upper heater strip by needing around the device of heating.
Present invention also provides a kind of cadmium telluride synthetic method.
Cadmium telluride synthetic method under the embodiment labor 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, obtain liquid tellurium and cadmium.
According to an embodiment of the application, can utilize tellurium stove 1 and the cadmium stove 3 that feeds in raw material that feeds in raw material that raw material tellurium and cadmium can be heated to 450 DEG C and 320 DEG C of fusings respectively, obtain liquid tellurium and cadmium.
According to an embodiment of the application, first raw material tellurium and cadmium can be processed into graininess, then the raw material tellurium after processing and cadmium are heated, melt, can fusing time be shortened like this, improve energy utilization rate, reach energy-conservation object.
Step b, raw material reaction, liquid tellurium and cadmium enter the reative cell 5 after vacuumizing and are obtained by reacting cadmium antimonide powder after atomization; And in reative cell 5, lead to argon gas simultaneously.
According to an embodiment of the application, tellurium atomizer 13 and cadmium atomizer 33 can be utilized to add argon gas by the tellurium of liquid state and cadmium atomization.The intensity of the argon gas added can be controlled at 1.5MPa.
According to an embodiment of the application, before the reaction, the vacuum in reative cell 5 can remain on 1*10 -3below Pa.
According to an embodiment of the application, in course of reaction, can ensure that the temperature of reative cell 5 is at 800 DEG C.
According to an embodiment of the application, the pressure of the argon gas entered by gas access 2 can remain on 1.5MPa.
According to an embodiment of the application, in the course of reaction after tellurium and cadmium reaction, by regulating the lifting of elevating lever 9, the reaction time of reactant can be adjusted.When raw material is less, can elevating lever be controlled motionless, when raw material is more, elevating lever rising can be controlled and extend the reaction time.
According to an embodiment of the application, when elevating lever 9 is provided with gas passage 10, the pressure of the argon gas entered along gas passage 10 can control at 0.5MPa.
Step c, collect cadmium antimonide powder, the cadmium antimonide powder obtained from reative cell 5 lower end discharging opening is collected by collector 8.
According to an embodiment of the application, the temperature of the pipeline that the discharging opening of reative cell 5 bottom can be connected with collector 8 controls at 1150 DEG C, to ensure that tellurium and cadmium fully react.
According to an embodiment of the application, in technique scheme, employing argon gas realizes the atomization to tellurium and cadmium; In fact, can above-mentioned functions be realized with tellurium and the nonreactive any one gas of cadmium, can as the substitute of argon gas, special inert gas 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 is also not limited to argon gas, can be can realize adjusting tellurium in reative cell 5 and cadmium reaction time and not with any one gas of tellurium, cadmium reaction, preferably inert gas, comprises helium, neon, argon gas, Krypton, xenon.
The foregoing is only the embodiment of the application, be not limited to the application, for a person skilled in the art, the application can have various modifications and variations.Within all spirit in the application and principle, any amendment done, equivalent replacement, improvement etc., within the right that all should be included in the application.

Claims (10)

1. a cadmium telluride synthesizer, is characterized in that, comprises and adds thermal reaction chamber for what realize reaction raw materials to react under spray pattern; Described reative cell top stove and the cadmium stove that feeds in raw material that feeds in raw material with tellurium is respectively connected; The discharging opening of described reative cell bottom is connected with collector; The arranged outside of described reative cell has heater; The described tellurium stove that feeds in raw material is provided with tellurium addition vessel; The pipeline that described tellurium addition vessel is connected with reative cell is provided with tellurium atomizer; The arranged outside of described tellurium addition vessel has heater; The described cadmium stove that feeds in raw material is provided with cadmium addition vessel; The pipeline that described cadmium addition vessel is connected with reative cell is provided with cadmium atomizer; The arranged outside of described cadmium addition vessel has heater.
2. cadmium telluride synthesizer according to claim 1, is characterized in that, the lower end of described tellurium addition vessel is provided with flow valve; The lower end of described cadmium addition vessel is provided with flow valve.
3. cadmium telluride synthesizer according to claim 1 and 2, is characterized in that, the pipeline that described tellurium addition vessel is connected with reative cell and the pipeline that cadmium addition vessel is connected with reative cell are respectively arranged with gas access; The pipeline that described tellurium addition vessel is connected with reative cell and the pipeline arranged outside that cadmium addition vessel is connected with reative cell have heater.
4. cadmium telluride synthesizer according to claim 1, is characterized in that, the pipeline that the discharging opening of described reative cell bottom is connected with collector is provided with filter; The pipeline arranged outside that the discharging opening of described reative cell bottom is connected with collector has heater.
5. cadmium telluride synthesizer according to claim 1, is characterized in that, described reative cell cross section is taper; In described reative cell, center is provided with rotating shaft.
6. cadmium telluride synthesizer according to claim 1, is characterized in that, described reative cell bottom discharging opening is also provided with the elevating lever for controlling cadmium telluride load.
7. cadmium telluride synthesizer according to claim 6, is characterized in that, described elevating lever is provided with gas passage.
8. cadmium telluride synthesizer according to claim 1, is characterized in that, described reative cell top is also provided with gas access.
9. cadmium telluride synthesizer according to claim 1, is characterized in that, described reative cell is helix; Along helix tube axis shaft to being provided with heater strip outside reative cell.
10. utilize a method for claim 1-9 arbitrary described cadmium telluride synthesizer synthesis cadmium telluride, it is characterized in that, comprise the following steps:
Step a, Raw material processing, heat raw material tellurium and cadmium, melt respectively, obtain liquid tellurium and cadmium;
Utilize feed in raw material stove and cadmium of tellurium to feed in raw material stove by raw material tellurium and cadmium heat fused respectively, obtain liquid tellurium and cadmium;
Step b, raw material reaction, liquid tellurium and cadmium enter the reative cell after vacuumizing and are obtained by reacting cadmium antimonide powder after atomization; And in reative cell, lead to argon gas simultaneously;
Tellurium atomizer and cadmium atomizer the tellurium of liquid state and cadmium is utilized to add argon gas by the tellurium of liquid state and cadmium atomization; Reative cell after tellurium after atomization and cadmium enter and vacuumize is obtained by reacting cadmium antimonide powder;
Step c, collect cadmium antimonide powder, the cadmium antimonide powder obtained from reative cell lower end discharging opening 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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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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