CN102849693B - High-temperature liquid-phase synthesis method of cadmium telluride powder - Google Patents
High-temperature liquid-phase synthesis method of cadmium telluride powder Download PDFInfo
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Abstract
The invention discloses a high-temperature liquid-phase synthesis method of cadmium telluride powder, which comprises the following steps: respectively containing cadmium blocks and tellurium blocks in the end A and the end B of a Y-shaped tube according to a mol ratio of 1:1; horizontally placing the Y-shaped quartz tube in an open/close type Y-shaped furnace chamber performing three-section heating; then vacuumizing the quartz tube to 1*10<-3>-1*10<-4> Pa; respectively heating the section A, the section B and the section C of the Y-shaped quartz tube to 350-400 DEG C, 480-600 DEG C and 600-1100 DEG C, and keeping the temperature until the test is finished; when the tellurium and the cadmium are molten into liquids, vertically arranging the open/close type furnace performing three-section heating through a bracket 8; then closing vacuum valves 1 and 2, opening breather valves 3 and 4 and a bleed valve 5, and introducing Ar gas of 0.01-1 MPa, so that the tellurium and cadmium liquids are respectively sprayed out from nozzles 6 and 7 and atomized, the high-purity cadmium telluride powder can be synthesized through the contact of the atomized tellurium and cadmium liquid drops, and the cadmium telluride powder scatters on the bottom of the end C of the Y-shaped quartz tube; and after the atomization process is finished, stopping heating, cooling to room temperature, opening an end cover 9 at the end C, and collecting the high-purity cadmium telluride powder.
Description
Technical field
The present invention relates to a kind of preparation method of cadmium antimonide powder, particularly a kind of high-temperature liquid-phase atomization production.
Background technology
Cadmium telluride is a kind of compound semiconductor, its energy gap is generally 1.45eV, be desirable photoelectric conversion material, mainly for the production of cadmium telluride solar battery thin film, and polycrystalline cadmium telluride alloy powder is the key core material of preparing solar cell Cadimium telluride thin film.At present domestic mainly with pressed powder or the synthetic cadmium telluride of particle high-temperature, as Chinese patent 200710049890.5 discloses a kind of preparation method of high-purity cadmium telluride, be characterized in by 5N tellurium and 5N cadmium in molar ratio the proportioning of 1:1 mix, pellet is pulverized or ground to form to compound, particle diameter is 8～13um, and 500～600 weight parts, pack silica tube into, be evacuated to 1～1.2Pa sealing, then the silica tube after good seal put into cadmium telluride synthetic furnace and react.Chinese patent 200910312590.0 discloses a kind of preparation method of high-purity cadmium telluride, reaction process occurs in the airtight silica tube after tellurium and painting carbon more than cadmium fusing point processing, 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 to silica tube and finally add at first tellurium material, after charging, deoxidation is also carried out sintering tube sealing with envelope bubble, slowly carries out the building-up reactions of High Temperature High Pressure.Its advantage of above patent 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 and produce, and output is not high and reaction time is longer; The cadmium telluride of preparation easily lumps in addition, needs attrition process powdered, and this process is easily introduced again impurity etc., causes product purity not high.
Summary of the invention
The object of the invention is to: a kind of preparation method that can continuous production cadmium antimonide powder is provided.
Technical scheme of the present invention is: by cadmium piece material and tellurium piece material, according to mol ratio 1:1, be respectively charged into the A of " Y " shape pipe (as shown in Figure 1), and B two ends, and " Y " shape silica tube level is put into open-close type " Y " the shape burner hearth of three sections of heating; Then silica tube is evacuated to 1 * 10
-3pa～1 * 10
-4pa, and the A to " Y " shape silica tube, B, tri-sections of C are heated to respectively 350 ℃～400 ℃, 480-600 ℃ and 600-1100 ℃, insulation is to having tested.When tellurium and cadmium are fused into after liquid, by support 8, the open-close type stove of three sections of heating is vertically placed, then close vacuum valve 1 and 2, open breather valve 3,4 and purging valve 5, and pass into 0.01-1Mpa Ar gas, make tellurium and cadmium liquid respectively from 5 and 6 spout ejection atomizations, the atomizing droplet of tellurium and cadmium contacts high-purity cadmium telluride powder that can be synthetic, and becomes scattered about the C bottom portion of " Y " shape silica tube.After atomization completes, stop heating, be cooled to room temperature, open C end end socket 9, can collect high-purity cadmium telluride powder.
Further, described by cadmium piece and tellurium piece, raw materials size is 1～6mm, and purity is not less than 5N level.
Further, the A of described " Y " shape silica tube, B two ends angle is 5-160 °.
Further, the spout aperture of described " Y " shape silica tube is 0.1-2mm.
The present invention has following beneficial effect:
1, the present invention is bonded into cadmium antimonide powder by the atomization direct of liquid phase tellurium and liquid phase cadmium, is a kind of safe, efficient processing method.
2, the cadmium antimonide powder that prepared by the present invention, due to after atomization is synthetic through the flat-temperature zone of 600-1100 ℃, tellurium or cadmium excessive in powder evaporate into gaseous state and remove under high-temperature, thereby have guaranteed to become scattered about the purity of the C bottom portion cadmium antimonide powder of " Y " shape silica tube; By controlling the large I of spout, realize the control of the granularity of cadmium antimonide powder simultaneously.
3, the cadmium antimonide powder method that prepared by the present invention, technical process is short, and equipment is simple, can realize serialization preparation, and be easy to industrialization.
Accompanying drawing explanation
Fig. 1 is the high-temperature liquid-phase synthetic method schematic diagram of cadmium antimonide powder, wherein 1,2: vacuum valve; 3,4: breather valve; 5: purging valve; 6,7: spout; 8: support; 9: end socket.
Fig. 2 is the cadmium antimonide powder X-ray diffractogram of embodiment 2 preparations.
Embodiment
Below by embodiment, the present invention is specifically described, the present embodiment is only used to further illustrate the present invention, and can not be interpreted as limiting the scope of the invention.
Embodiment 1
By approximately 1～6mm cadmium piece and tellurium piece, purity 5N level, 1:1 is respectively charged into the A of " Y " shape pipe in molar ratio, B two ends, and A, the angle at B two ends is 5 °, and " Y " shape silica tube level is put into open-close type " Y " the shape burner hearth of three sections of heating; Then silica tube is evacuated to 1.0 * 10
-3pa, and the A to " Y " shape silica tube, B, tri-sections of C are heated to respectively 360 ℃, and 480 ℃ and 800 ℃, insulation is to having tested.When tellurium and cadmium are fused into after liquid, by support 8, the open-close type stove of three sections of heating is vertically placed, then close vacuum valve 1 and 2, open breather valve 3,4 and purging valve 5, and pass into the Ar gas of 0.01Mpa, and make tellurium and cadmium liquid respectively from 5 and 6 spouts ejection atomizations, dispersive nozzle aperture is 2.0mm, the atomizing droplet of tellurium and cadmium contacts and has synthesized high-purity cadmium antimonide powder, and becomes scattered about the C bottom portion of " Y " shape silica tube.After atomization completes, stop heating, be cooled to room temperature, open C end end socket 9, can collect high-purity cadmium telluride powder.
Embodiment 2
By 3～6mm cadmium piece and tellurium piece, purity 6N level, 1:1 is respectively charged into the A of " Y " shape pipe, B two ends, A, B in molar ratio
The angle at two ends is 80 °, and " Y " shape silica tube level is put into open-close type " Y " the shape burner hearth of three sections of heating; Then silica tube is evacuated to 1.0 * 10
-3pa, and the A to " Y " shape silica tube, B, tri-sections of C are heated to respectively 370 ℃, and 540 ℃ and 900 ℃, insulation is to having tested.When tellurium and cadmium are fused into after liquid, by support 8, the open-close type stove of three sections of heating is vertically placed, then close vacuum valve 1 and 2, open breather valve 3,4 and purging valve 5, and pass into the Ar gas of 0.10Mpa, and make tellurium and cadmium liquid respectively from 5 and 6 spouts ejection atomizations, dispersive nozzle aperture is 1.0mm, the atomizing droplet of tellurium and cadmium contacts and has synthesized high-purity cadmium antimonide powder, and becomes scattered about the C bottom portion of " Y " shape silica tube.After atomization completes, stop heating, be cooled to room temperature, open C end end socket 9, collect high-purity cadmium telluride powder, X-ray diffraction result shows that the powder of preparation is single-phase cadmium telluride (see figure 2), more than the composition result (in Table 1) detecting by ICP-MS method shows that cadmium antimonide powder purity reaches 5N.
The composition test result of the cadmium antimonide powder of table 1 preparation
Embodiment 3
By 2～6mm cadmium piece and tellurium piece, purity 7N level, 1:1 is respectively charged into the A of " Y " shape pipe in molar ratio, B two ends, A, the angle at B two ends is 110 °, and " Y " shape silica tube level is put into open-close type " Y " the shape burner hearth of three sections of heating; Then silica tube is evacuated to 8.0 * 10
-4pa, and the A to " Y " shape silica tube, B, tri-sections of C are heated to respectively 350 ℃, and 540 ℃ and 600 ℃, insulation is to having tested.When tellurium and cadmium are fused into after liquid, by support 8, the open-close type stove of three sections of heating is vertically placed, then close vacuum valve 1 and 2, open breather valve 3,4 and purging valve 5, and pass into the Ar gas of 0.5Mpa, and make tellurium and cadmium liquid respectively from 5 and 6 spouts ejection atomizations, dispersive nozzle aperture is 0.5mm, the atomizing droplet of tellurium and cadmium contacts i.e. synthetic high-purity cadmium antimonide powder, and becomes scattered about the C bottom portion of " Y " shape silica tube.After atomization completes, stop heating, be cooled to room temperature, open C end end socket 9, can collect high-purity cadmium telluride powder.
Embodiment 4
By 2～6mm cadmium piece and tellurium piece, purity 6N level, 1:1 is respectively charged into the A of " Y " shape pipe in molar ratio, B two ends, A, the angle at B two ends is 60 °, and " Y " shape silica tube level is put into open-close type " Y " the shape burner hearth of three sections of heating; Then silica tube is evacuated to 1.0 * 10
-4pa, and the A to " Y " shape silica tube, B, tri-sections of C are heated to respectively 380 ℃, and 560 ℃ and 1000 ℃, insulation is to having tested.When tellurium and cadmium are fused into after liquid, by support 8, the open-close type stove of three sections of heating is vertically placed, then close vacuum valve 1 and 2, open breather valve 3,4 and purging valve 5, and pass into the Ar gas of 1.00Mpa, and make tellurium and cadmium liquid respectively from 5 and 6 spouts ejection atomizations, dispersive nozzle aperture is 0.1mm, the atomizing droplet of tellurium and cadmium contacts and can synthesize high-purity cadmium antimonide powder, and becomes scattered about the C bottom portion of " Y " shape silica tube.After atomization completes, stop heating, be cooled to room temperature, open C end end socket 9, can collect high-purity cadmium telluride powder.
Embodiment 5
By 2～6mm cadmium piece and tellurium piece, purity 8N level, 1:1 is respectively charged into the A of " Y " shape pipe in molar ratio, B two ends, A, the angle at B two ends is 160 °, and " Y " shape silica tube level is put into open-close type " Y " the shape burner hearth of three sections of heating; Then silica tube is evacuated to 4.0 * 10
-4pa, and the A to " Y " shape silica tube, B, tri-sections of C are heated to respectively 400 ℃, and 600 ℃ and 1100 ℃, insulation is to having tested.When tellurium and cadmium are fused into after liquid, by support 8, the open-close type stove of three sections of heating is vertically placed, then close vacuum valve 1 and 2, open breather valve 3,4 and purging valve 5, and pass into the Ar gas of 1.00Mpa, and make tellurium and cadmium liquid respectively from 5 and 6 spouts ejection atomizations, dispersive nozzle aperture is 0.1mm, the atomizing droplet of tellurium and cadmium contacts i.e. synthetic high-purity cadmium antimonide powder, and becomes scattered about the C bottom portion of " Y " shape silica tube.After atomization completes, stop heating, be cooled to room temperature, open C end end socket 9, can collect.
Claims (4)
1. a high-temperature liquid-phase synthetic method for cadmium antimonide powder, is characterized in that:
Using " Y " shape silica tube is reaction vessel, and it has A, B, C holds, and wherein A, B end refers to respectively the left and right end of upside when " Y " shape pipe is vertically placement, and downside is C end; A, B end has respectively vacuum valve (1,2), breather valve (3,4) and spout (6,7), and C end has end socket (9) and purging valve (5);
The concrete steps of synthetic method are:
By cadmium piece and tellurium piece, 1:1 is respectively charged into the A of " Y " shape pipe in molar ratio, B two ends, and " Y " shape silica tube level is put into open-close type " Y " the shape burner hearth of three sections of heating; Then silica tube is evacuated to 1 * 10
-3pa～1 * 10
-4pa, and the A to " Y " shape silica tube, B, tri-sections of C are heated to respectively 350 ℃～400 ℃, 480-600 ℃ and 600-1100 ℃, insulation is to having tested; When tellurium and cadmium are fused into after liquid, by support (8), the open-close type stove of three sections of heating is vertically placed, then close vacuum valve (1,2), open breather valve (3,4) and purging valve (5), and pass into the Ar gas of 0.01-1MPa, make tellurium and cadmium liquid respectively from spout (6,7) ejection atomization, the atomizing droplet of tellurium and cadmium contacts synthetic high-purity cadmium telluride powder, and becomes scattered about the C bottom portion of " Y " shape silica tube; After atomization completes, stop heating, be cooled to room temperature, open C end end socket (9), collect high-purity cadmium telluride powder.
2. the high-temperature liquid-phase synthetic method of cadmium antimonide powder according to claim 1, is characterized in that described cadmium piece and tellurium piece raw materials size are 1～6mm, and purity is not less than 5N level.
3. the high-temperature liquid-phase synthetic method of a kind of cadmium antimonide powder according to claim 1, is characterized in that the A of described " Y " shape silica tube, and B two ends angle is 5-160 °.
4. the high-temperature liquid-phase synthetic method of cadmium antimonide powder according to claim 1, is characterized in that the spout aperture of described " Y " shape silica tube is 0.1-2mm.
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| CN103496678B (en) * | 2013-10-22 | 2015-04-29 | 谈逊 | Cadmium telluride synthesizing device and method |
| CN104014284B (en) * | 2014-06-04 | 2016-07-06 | 四川大学 | The free fall high-temperature nuclei method of IIB-VIA compounds of group powder and synthesizer |
| CN104016312B (en) * | 2014-06-04 | 2016-04-06 | 四川大学 | A kind of synthetic method of IIB-VIA compounds of group powder |
| CN110282975B (en) * | 2019-07-08 | 2022-07-01 | 先导薄膜材料（广东）有限公司 | Germanium selenide target material and preparation method thereof |
| CN111473649A (en) * | 2020-04-13 | 2020-07-31 | 合肥科晶材料技术有限公司 | Three-temperature-zone special-shaped tube furnace |
| CN115353080B (en) * | 2022-09-21 | 2023-09-01 | 安徽光智科技有限公司 | Cadmium telluride synthesizing method |
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| 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 |
| CN102086031A (en) * | 2010-11-25 | 2011-06-08 | 广东先导稀有材料股份有限公司 | Liquid-phase synthesis method of cadmium telluride |
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| 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 |
| CN102086031A (en) * | 2010-11-25 | 2011-06-08 | 广东先导稀有材料股份有限公司 | Liquid-phase synthesis method of cadmium telluride |
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