CN103754838B - A kind of method and apparatus preparing cadmium antimonide powder fast - Google Patents
A kind of method and apparatus preparing cadmium antimonide powder fast Download PDFInfo
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- CN103754838B CN103754838B CN201410045809.6A CN201410045809A CN103754838B CN 103754838 B CN103754838 B CN 103754838B CN 201410045809 A CN201410045809 A CN 201410045809A CN 103754838 B CN103754838 B CN 103754838B
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Abstract
The invention provides a kind of method and apparatus preparing cadmium antimonide powder fast, described equipment comprises furnace chamber, the first dividing plate and second partition is provided with in the horizontal direction in described furnace chamber, vertically be provided with the 3rd dividing plate and the 4th dividing plate, furnace chamber is divided into melting evaporating area, combining zone, solidification zone and finished product collecting region by described four dividing plates; First dividing plate and second partition are provided with ventilating pit or dividing plate can reciprocate in the horizontal direction; Formation return flow line, space is provided with between the 3rd dividing plate and the 4th dividing plate; Melting evaporating area, combining zone, solidification zone and finished product collecting region are respectively equipped with heating system, and gas can circulate in four districts; When preparing cadmium antimonide powder only need in melting evaporating area throwing raw materials, vacuumize after passing into rare gas element in furnace chamber, then control the temperature of four not same districts.Present device is easy, simple to operate, and cost is low, and reaction time is short, production efficiency is high, realizes continuous prodution, prepares that cadmium antimonide powder is thin, prevented from caking and free from foreign meter.
Description
Technology is led
The present invention relates to a kind of preparation method and equipment of cadmium telluride, particularly a kind of method and apparatus preparing cadmium antimonide powder fast.
Background technology
Cadmium telluride is a kind of semiconductor compound synthesized by cadmium and tellurium, and its energy gap is generally 1.45eV, is desirable photoelectric conversion material.At present, cadmium telluride is widely used in infrared optical window material, electrooptic modulator and solar cell neck, has very high economic worth.
Low for its cost of production cadmium telluride diaphragm solar battery, consider other costs such as wage, management, electric power and equipment amortization, the cost of cadmium telluride diaphragm solar battery is about 60% of the present price of crystal silicon solar energy battery.The simultaneously efficiency of conversion about 9% of its software-component of cadmium telluride diaphragm solar battery, the most high conversion efficiency of assembly reaches 11%, is the good solar cell of application prospect.And polycrystalline cadmium telluride alloy powder is the key core material preparing cadmium telluride diaphragm solar battery, therefore how prepares highly purified cadmium antimonide powder fast and realize the task of top priority that suitability for industrialized production is raising cadmium telluride diaphragm solar battery.
Current, domestic main pressed powder or particle high-temperature high-pressure synthesis cadmium telluride, as Chinese patent 200910312590.0 discloses a kind of preparation method of high-purity cadmium telluride, reaction process occurs in the airtight silica tube after the painting carbon process of more than tellurium and cadmium fusing point, wherein the mass ratio of 5N cadmium material and 5N tellurium material is 1:1.1 ~ 1.15, load weighted tellurium material is divided into N part according to material times N, load weighted cadmium material is divided into N-1 part, every part of tellurium material and every part of cadmium material are alternately added silica tube and add tellurium material at first, finally add tellurium material, deoxidation also carries out sintering tube sealing with envelope bubble, slowly carry out the building-up reactions of High Temperature High Pressure.Namely silica tube is put into vacuum system deoxidation, when the vacuum tightness of vacuum system reaches 5 × 10 after charging
-4pa-10 × 10
-4by silica tube tube sealing after Pa, after tube sealing, stop deoxidation.Again the silica tube unloaded from vacuum system is put into synthetic furnace, at 600 DEG C-800 DEG C isothermal reaction 1.5-2.5h, then slow cooling to 900 DEG C-1050 DEG C again after 1100 DEG C-1200 DEG C isothermal reaction 2.5-3.5h, breaks silica tube and removes cadmium telluride product.Can not produce larger vapour pressure in whole process, cadmium also can not react with silica tube, realizes the sealing of high temperature high vacuum simultaneously.But need in its building-up process to feed intake in silica tube, deoxidation, tube sealing, and broken silica tube feeding, wherein tube sealing achieves high temperature high vacuum tube sealing, therefore processing unit and complicated operation; Can not realize continuous prodution, production efficiency religion is low and reaction time is longer; The standby cadmium telluride of this legal system easily lumps, and needs attrition process powdered, and this process easily introduces that impurity pollutes etc. thus product purity is not high; In addition, the production unit cost intensive of this method is adopted.
Summary of the invention
The invention provides a kind of method and apparatus preparing cadmium antimonide powder fast, solve in prior art processing unit when preparing cadmium antimonide powder and complicated operation, can not realize continuous prodution, production efficiency is lower and reaction time is longer; The cadmium telluride product of preparation easily lumps, and the technical problem of equipment cost costliness.
For solving the problems of the technologies described above, the equipment preparing cadmium antimonide powder fast provided by the invention is a kind of vapourizing furnace, comprises furnace chamber, is provided with the first dividing plate and second partition in the horizontal direction in described furnace chamber; Vertically be provided with the 3rd dividing plate and the 4th dividing plate; Furnace chamber is divided into melting evaporating area, combining zone, solidification zone and finished product collecting region by four dividing plates be provided with in described furnace chamber; The vertical lower of the first dividing plate is melting evaporating area, and the vertical direction of the first dividing plate is combining zone; The vertical direction of second partition is solidification zone, and the vertical lower of second partition is finished product collecting region; First dividing plate and second partition are provided with ventilating pit or dividing plate can reciprocate in the horizontal direction; Be connected with bottom vapourizing furnace bottom 4th dividing plate, space is left at the 3rd dividing plate and vapourizing furnace top, is provided with formation return flow line, space between the 3rd dividing plate and the 4th dividing plate; Melting evaporating area, combining zone, solidification zone and finished product collecting region are respectively equipped with heating system, and gas can circulate in melting evaporating area, combining zone, solidification zone and four, finished product collecting region district; Described vapourizing furnace is provided with intake valve and air outlet valve, and the furnace wall of the finished product collecting region of described vapourizing furnace is provided with discharge port, and the solidification zone of described vapourizing furnace or the furnace wall of finished product collecting region are provided with vacuum valve.
Another preferred version of the present invention is: the heating system of described melting evaporating area, solidification zone and finished product collecting region is electromagnetic induction heating system and/or electric-heating-wire-heating system, and the heating system of described combining zone is electric-heating-wire-heating system.
Another preferred version of the present invention is: described melting evaporating area is provided with one or two raw material tank.
Meanwhile, the invention provides a kind of method preparing cadmium antimonide powder fast fast using described vapourizing furnace, it comprises the following steps:
1) proportioning of getting tellurium and cadmium 1:1 in molar ratio mixes, and is loaded in vapourizing furnace melting evaporating area after mixing by tellurium cadmium compound;
2) in vapourizing furnace, pass into rare gas element makes rare gas element be full of whole vapourizing furnace furnace chamber;
3) in the solidification zone of vapourizing furnace or finished product collecting region, vapourizing furnace furnace chamber is vacuumized, and by the tellurium cadmium mixed material heating in vapourizing furnace melting evaporating area to 200-300 DEG C, constant temperature 3-4 hour;
4) again by the tellurium cadmium mixed material heating in vapourizing furnace melting evaporating area to 450-550 DEG C, the combining zone of vapourizing furnace is heated to 900-1100 DEG C, and the solidification zone of vapourizing furnace is heated to 600-800 DEG C, and finished product collecting region is heated to 450-550 DEG C respectively;
5) after having reacted, stop heating and vacuumize, after stove to be evaporated cools, in vapourizing furnace finished product collecting region, opening discharge port take out cadmium antimonide powder.
Another preferred version of the present invention is: the purity of tellurium and cadmium is 4-5N.
Another preferred version of the present invention is: described rare gas element is nitrogen, helium or argon gas.
Another preferred version of the present invention is: the type of cooling is air cooling, water-cooled or use one or more of cooling fin mode.
Owing to have employed described equipment and technical scheme, beneficial effect of the present invention is as follows:
1, the vapourizing furnace preparing cadmium antimonide powder is easy and simple to operate, and equipment cost cost is low;
The invention provides a kind of equipment preparing cadmium antimonide powder fast and be vapourizing furnace, the furnace chamber of this vapourizing furnace is divided into four districts: evaporating area, combining zone, solidification zone and finished product collecting region, gas can circulate in these four districts, because each district respectively establishes heating system, the temperature that can control these four districts in furnace chamber is different, and be provided with vacuum valve in solidification zone or finished product collecting region, the gas being gathered in furnace chamber top can be made toward solidification zone and the flowing of finished product district, thus make the material in furnace chamber can realize conversion between solid-gas and circulation in predetermined district, cadmium telluride disposable Fast back-projection algorithm in vapourizing furnace is made to become possibility.
2, realize continuous prodution, reaction time is short, and production efficiency is high;
When the present invention prepares cadmium antimonide powder, tellurium cadmium compound is heated to 450-550 DEG C of melting in melting evaporating area, because combining zone is heated to 900-1100 DEG C, therefore the tellurium of melting and cadmium flash to tellurium steam and cadmium vapor and be gathered in combining zone after being provided with baffle plate of breather or the dividing plate that can reciprocate in the horizontal direction by being heated, and then combination reaction occurs generate cadmium telluride steam.Because whole system is in the state of vacuumizing always, be namely in negative pressure state in vapourizing furnace furnace chamber, and pressure is followed successively by from high to low: melting evaporating area, combining zone, solidification zone and finished product collecting region always.Therefore, cadmium telluride steam is gathered in solidification zone under the effect of pressure, and the temperature of solidification zone is set in 600-800 DEG C, is starkly lower than the fusing point of cadmium telluride, therefore cadmium telluride steam will be caught a cold and is frozen into cadmium antimonide powder, and cadmium antimonide powder is gathered in finished product collecting region under gravity.Temperatures involved by combining zone is flashed to steam by return flow line continuation generation combination reaction by the tellurium and the cadmium that remain in finished product collecting region on a small quantity simultaneously, circulate with this thus realize the continuous seepage of the feeding intake of tellurium and cadmium raw material, melting, reaction, taking-up cadmium antimonide powder, shorten reaction time simultaneously, improve production efficiency.
3, thin, the prevented from caking of the cadmium antimonide powder of preparation and free from foreign meter.
The cadmium telluride steam generated in reaction process is gathered in solidification zone, and because solidification zone temperature only has 600-800 DEG C, and the fusing point of cadmium telluride is 1092 DEG C, and therefore cadmium telluride steam can fall to being gathered in finished product collecting region by instantaneous coagulation powdered.Therefore the thin and prevented from caking of the above-mentioned cadmium antimonide powder be obtained by reacting.Meanwhile, be automatically produce continuously in whole reaction process, not by the interference of extraneous factor, therefore free from foreign meter.
Accompanying drawing explanation
Fig. 1 shows the structural representation of vapourizing furnace.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated, but the scope of protection of present invention is not limited to the scope that embodiment is expressed.
Embodiment 1: Fig. 1 shows vapourizing furnace 1.Described vapourizing furnace 1 comprises furnace chamber, is provided with the first dividing plate 10 and second partition 11 in described furnace chamber in the horizontal direction; Vertically be provided with the 3rd dividing plate 12 and the 4th dividing plate 13; Furnace chamber is divided into melting evaporating area 2, combining zone 3, solidification zone 4 and finished product collecting region 5 by four dividing plates be provided with in described furnace chamber; The vertical lower of the first dividing plate 10 is the vertical direction of melting evaporating area 2, first dividing plate 10 is combining zone 3; The vertical direction of second partition 11 is solidification zone 4, and the vertical lower of second partition 11 is finished product collecting region 5; First dividing plate 10 and second partition 11 are provided with ventilating pit (not shown) or dividing plate can reciprocate in the horizontal direction; Be connected with bottom vapourizing furnace 1 bottom 4th dividing plate 13,3rd dividing plate 12 leaves space with vapourizing furnace 1 top, be provided with formation return flow line, space 9 between the 3rd dividing plate 12 and the 4th dividing plate 13, be convenient to the collection and confinement of gases in solidification zone 4 and finished product collecting region 5 to be back to melting evaporating area 2 and combining zone 3; Melting evaporating area 2 is provided with a raw material tank.Melting evaporating area 2, combining zone 3, solidification zone 4 and finished product collecting region 5 are respectively equipped with heating system, and gas can circulate in melting evaporating area 2, combining zone 3, solidification zone 4 and 5 four, finished product collecting region district; Described vapourizing furnace melting evaporating area 2 is provided with intake valve 6, and finished product collecting region 5 is provided with air outlet valve 7, and in vapourizing furnace 1, the time argon gas of logical argon gas enters from intake valve 6, is discharged by air from air outlet valve 7.Furnace wall when vacuumizing vapourizing furnace 1, vaccum-pumping equipment being connected vapourizing furnace 1 solidification zone 4 is provided with vacuum valve 8.Adopt the melting evaporating area 2 of electromagnetic induction heating vapourizing furnace, solidification zone 4 and finished product collecting region 5 simultaneously, adopt the combining zone 3 of electric-heating-wire-heating vapourizing furnace.Finally, material can be provided with the taking-up of discharge port (not shown) from the furnace wall of the finished product collecting region 5 of vapourizing furnace 1.
Embodiment 2: described vapourizing furnace comprises furnace chamber, is provided with the first dividing plate and second partition in described furnace chamber in the horizontal direction; Vertically be provided with the 3rd dividing plate and the 4th dividing plate; Furnace chamber is divided into melting evaporating area, combining zone, solidification zone and finished product collecting region by four dividing plates be provided with in described furnace chamber; The vertical lower of the first dividing plate is melting evaporating area, and the vertical direction of the first dividing plate is combining zone; The vertical direction of second partition is solidification zone, and the vertical lower of second partition is finished product collecting region; The dividing plate of the first dividing plate and second partition can reciprocate in the horizontal direction, as required two-phase septal area connected entrance size; Be connected with bottom vapourizing furnace bottom 4th dividing plate, space is left at the 3rd dividing plate and vapourizing furnace top, is provided with formation return flow line, space between the 3rd dividing plate and the 4th dividing plate; Melting evaporating area is provided with two raw material tanks, puts tellurium simple substance raw material for one, puts cadmium simple substance raw material for one.Melting evaporating area, combining zone, solidification zone and finished product collecting region are respectively equipped with heating system, and gas can circulate in melting evaporating area, combining zone, solidification zone and four, finished product collecting region district; Described vapourizing furnace melting evaporating area is provided with intake valve, and solidification zone is provided with air outlet valve, and in vapourizing furnace, the time argon gas of logical argon gas enters from intake valve, is discharged by air from air outlet valve.Furnace wall when vacuumizing vapourizing furnace, vaccum-pumping equipment being connected vapourizing furnace solidification zone is provided with vacuum valve.What adopt electric-heating-wire-heating vapourizing furnace melts evaporating area, combining zone, solidification zone and finished product collecting region simultaneously.Finally, material can be provided with the taking-up of discharge port (not shown) from the furnace wall of the finished product collecting region of vapourizing furnace.
Embodiment 3: as shown in Figure 1, the proportioning of the cadmium getting the tellurium of 5N and 5N 1:1 in molar ratio mixes, be loaded to by tellurium cadmium compound after mixing in a raw material tank (not shown) of vapourizing furnace 1 melting evaporating area 2, the cadmium of the tellurium and 5N that also directly can get 5N puts into 2 raw material tank (not shown) of vapourizing furnace 1 melting evaporating area 2 respectively.Then the intake valve 6 toward vapourizing furnace passes into helium and discharges chamber air by air outlet valve 7, helium is full of whole vapourizing furnace 1 furnace chamber.The vacuum valve 8 vacuum extractor being connected finished product collecting region 5 place of vapourizing furnace 1 vacuumizes, by the tellurium cadmium mixed material heating in vapourizing furnace 1 melting evaporating area 2 to 200-300 DEG C, and constant temperature 3-4 hour; Again by the tellurium cadmium mixed material heating in vapourizing furnace 1 melting evaporating area 2 to 450-550 DEG C, the combining zone of vapourizing furnace 1 is heated to 900-1100 DEG C, and the solidification zone of vapourizing furnace is heated to 600-800 DEG C, and finished product collecting region is heated to 450-550 DEG C respectively.Wherein tellurium cadmium compound is heated to 450-550 DEG C of melting in melting evaporating area 2, because combining zone 3 is heated to 900-1100 DEG C, therefore the tellurium of melting and cadmium will be heated and flash to tellurium steam and cadmium vapor is gathered in combining zone 3 through the first dividing plate 10, and then combination reaction occurs generate cadmium telluride steam.Because whole system is in the state of vacuumizing always, be namely in negative pressure state in vapourizing furnace 1 furnace chamber, and pressure is followed successively by from high to low: melting evaporating area 2, combining zone 3, solidification zone 4 and finished product collecting region 5 always.Therefore, cadmium telluride steam is gathered in solidification zone 4 under the effect of pressure, the temperature of solidification zone 4 is set in 600-800 DEG C, be starkly lower than the fusing point of cadmium telluride, therefore cadmium telluride steam will be caught a cold and is frozen into cadmium antimonide powder, and cadmium antimonide powder is gathered in finished product collecting region 5 through second partition 11 under gravity.The tellurium and the cadmium that remain in finished product collecting region 5 on a small quantity will be back in melting evaporating area 2 or combining zone 3 by return flow line 9 simultaneously, re-start combination reaction and generate cadmium telluride steam.After having reacted, stop heating and vacuumize, after the mode adopting water-cooled and cooling fin to combine cools vapourizing furnace 1, in vapourizing furnace 1 finished product collecting region 5, opening discharge port (not shown) take out cadmium antimonide powder.
Realize the continuous seepage of the feeding intake of tellurium and cadmium raw material, melting, reaction, taking-up cadmium antimonide powder with this circulating reaction, shorten reaction time simultaneously, improve production efficiency.
The announcement of book and instruction according to the above description, belonging to the present invention, the technician of neck can also change above-mentioned embodiment and revise.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition, although employ some specific terms in this specification sheets, these terms just for convenience of description, do not form any restriction to the present invention.
Claims (7)
1. prepare a vapourizing furnace for cadmium antimonide powder fast, it is characterized in that: comprise furnace chamber, in described furnace chamber, be provided with the first dividing plate and second partition in the horizontal direction; Vertically be provided with the 3rd dividing plate and the 4th dividing plate; Furnace chamber is divided into melting evaporating area, combining zone, solidification zone and finished product collecting region by four dividing plates be provided with in described furnace chamber; The vertical lower of the first dividing plate is melting evaporating area, and the vertical direction of the first dividing plate is combining zone; The vertical direction of second partition is solidification zone, and the vertical lower of second partition is finished product collecting region; First dividing plate and second partition are provided with ventilating pit or dividing plate can reciprocate in the horizontal direction; Be connected with bottom vapourizing furnace bottom 4th dividing plate, space is left at the 3rd dividing plate and vapourizing furnace top, is provided with formation return flow line, space between the 3rd dividing plate and the 4th dividing plate; Melting evaporating area, combining zone, solidification zone and finished product collecting region are respectively equipped with heating system, and gas can circulate in melting evaporating area, combining zone, solidification zone and four, finished product collecting region district; Described vapourizing furnace is provided with intake valve and air outlet valve, and the furnace wall of the finished product collecting region of described vapourizing furnace is provided with discharge port, and the solidification zone of described vapourizing furnace or the furnace wall of finished product collecting region are provided with vacuum valve.
2. the vapourizing furnace preparing cadmium antimonide powder fast according to claim 1, it is characterized in that described melting evaporating area, the heating system of solidification zone and finished product collecting region is electromagnetic induction heating system and/or electric-heating-wire-heating system, the heating system of described combining zone is electric-heating-wire-heating system.
3. the vapourizing furnace preparing cadmium antimonide powder fast according to claim 1, is characterized in that described melting evaporating area is provided with one or two raw material tank.
4. use the vapourizing furnace of claim 1,2 or 3 to prepare a method for cadmium antimonide powder fast, it is characterized in that comprising the following steps:
1) proportioning of getting tellurium and cadmium 1:1 in molar ratio mixes, and is loaded in vapourizing furnace melting evaporating area after mixing by tellurium cadmium compound;
2) in vapourizing furnace, pass into rare gas element makes rare gas element be full of whole vapourizing furnace furnace chamber;
3) in the solidification zone of vapourizing furnace or finished product collecting region, vapourizing furnace furnace chamber is vacuumized, and by the tellurium cadmium mixed material heating in vapourizing furnace melting evaporating area to 200-300 DEG C, constant temperature 3-4 hour;
4) again by the tellurium cadmium mixed material heating in vapourizing furnace melting evaporating area to 450-550 DEG C, the combining zone of vapourizing furnace is heated to 900-1100 DEG C, and the solidification zone of vapourizing furnace is heated to 600-800 DEG C, and finished product collecting region is heated to 450-550 DEG C;
5) after having reacted, stop heating and vacuumize, after stove to be evaporated cools, in vapourizing furnace finished product collecting region, opening discharge port take out cadmium antimonide powder.
5. the method preparing cadmium antimonide powder fast according to claim 4, is characterized in that the purity of tellurium and cadmium is 4-5N.
6. the method preparing cadmium antimonide powder fast according to claim 4, is characterized in that described rare gas element is nitrogen, helium or argon gas.
7. the method preparing cadmium antimonide powder fast according to claim 4, is characterized in that the type of cooling is air cooling, water-cooled or use one or more of cooling fin mode.
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|---|---|---|---|
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| CN201410045809.6A CN103754838B (en) | 2014-02-08 | 2014-02-08 | A kind of method and apparatus preparing cadmium antimonide powder fast |
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| CN112680781B (en) * | 2020-12-09 | 2023-10-03 | 清远先导材料有限公司 | Cadmium telluride crystal growth device and growth method thereof |
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| GB983004A (en) * | 1961-01-13 | 1965-02-10 | Philips Electronic Associated | Improvements in and relating to methods of thermal treatment of semiconductor material |
| EP0650791A1 (en) * | 1993-11-02 | 1995-05-03 | H.C. Starck GmbH & Co. KG | Fine particles of metals, alloys and metal compounds |
| CN101118111A (en) * | 2007-08-31 | 2008-02-06 | 侯仁义 | Multiple layer synthesis furnace device |
| CN202092090U (en) * | 2011-04-01 | 2011-12-28 | 湘潭大学 | Controllable selenium steam or sulfur steam generation device for selenylation or sulfuration processing |
| CN103420346A (en) * | 2012-05-22 | 2013-12-04 | 广东先导稀材股份有限公司 | Preparation method for cadmium telluride |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08104600A (en) * | 1994-09-29 | 1996-04-23 | Nippon Ketsushiyou Kogaku Kk | Production of cadmium telluride single crystal and casting mold used therein |
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2014
- 2014-02-08 CN CN201410045809.6A patent/CN103754838B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB983004A (en) * | 1961-01-13 | 1965-02-10 | Philips Electronic Associated | Improvements in and relating to methods of thermal treatment of semiconductor material |
| EP0650791A1 (en) * | 1993-11-02 | 1995-05-03 | H.C. Starck GmbH & Co. KG | Fine particles of metals, alloys and metal compounds |
| CN101118111A (en) * | 2007-08-31 | 2008-02-06 | 侯仁义 | Multiple layer synthesis furnace device |
| CN202092090U (en) * | 2011-04-01 | 2011-12-28 | 湘潭大学 | Controllable selenium steam or sulfur steam generation device for selenylation or sulfuration processing |
| CN103420346A (en) * | 2012-05-22 | 2013-12-04 | 广东先导稀材股份有限公司 | Preparation method for cadmium telluride |
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