CN104860272A - New method for quick preparation of high-purity cadmium telluride powder - Google Patents
New method for quick preparation of high-purity cadmium telluride powder Download PDFInfo
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Abstract
The invention discloses a new method for quick preparation of high-purity cadmium telluride powder. The method comprises the steps of: firstly, mixing cadmium powder and tellurium powder at a mole ratio of 1: 1 and then uniformly grinding and mixing; cold-pressing the uniformly mixed powder into a block-shaped blank body; triggering a self-propagating high temperature synthesis reaction on the obtained block-shaped blank body; at the end of the reaction, naturally cooling and grinding to be the single-phase high-purity cadmium telluride powder. The new method provided by the invention is quick in reaction speed, simple in process, low in cost, low in equipment dependency, efficiency and energy-efficient; the whole preparation process can be finished within 10 min, synthesis efficiency of the cadmium telluride powder can be greatly improved and batch production is easily realized.
Description
Technical field
The invention belongs to new forms of energy technical field of photoelectric material preparation, be specifically related to a kind of novel method preparing high-purity cadmium telluride powder fast.
Background technology
Cadmium telluride is a kind of binary compound synthesized by tellurium element and cadmium element, and belong to typical wide bandgap compound semiconductor, its energy gap is generally 1.45eV, is a kind of desirable photoelectric conversion material.Current cadmium telluride is mainly used in infrared optical window material, electrooptic modulator and solar film battery.
The key core material of sun power cadmium telluride thin-film battery is the cadmium antimonide powder of polycrystalline.The method of current synthesis cadmium antimonide powder mainly contains chemical method and the large class of Physical two.Wherein Physical mainly synthesizes cadmium telluride with the simple substance block of tellurium and cadmium or powder by pyroreaction.As Chinese patent 200710049890.5 discloses a kind of preparation method of high-purity cadmium telluride, it is characterized by and the tellurium of 5N and cadmium are mixed according to CdTe stoichiometric ratio, then pulverize or grind to form pellet to load subsequently in silica tube, vacuum-sealing under 1-1.2Pa, again the silica tube after good seal is put into high―temperature nuclei stove and carry out Reactive Synthesis cadmium-telluride block, finally grinding obtains cadmium antimonide powder.Chinese patent 201210401061.X discloses a kind of high-temperature liquid-phase synthetic method relying on specific installation to synthesize cadmium antimonide powder, it is characterized in that by cadmium block and tellurium block in molar ratio 1:1 be transferred to the two ends of " Y " shape silica tube respectively, then silica tube level is put into suitable " Y " shape burner hearths of foldings of three sections of heating; Silica tube vacuumizes and is heated to 350 ~ 400 DEG C respectively to its three sections, 480 ~ 600 DEG C, 600 ~ 1100 DEG C again, insulation is to having tested, then by follow-up a series of valve switch manipulation, the tellurium of fusing is contacted with the form of atomizing droplet with cadmium, finally synthesizes cadmium antimonide powder.Also there is chemical method to prepare the Patents of cadmium antimonide powder at present, as Chinese patent 201310015697.5 discloses a kind of method that liquid-phase reduction and hydrogen process prepare cadmium antimonide powder, it is characterized in that according to Cd
2+the proportioning being 0.9 ~ 1.1 with the mol ratio of Te (IV) dissolves the oxide compound of cadmium and tellurium, oxyhydroxide or salt in acid, is mixed with Cd
2+, Te concentration be the solution of 0.2 ~ 1mol/L; Then this solution is placed in thermostat water bath, thermostat temperature is 20 ~ 90 DEG C; Then add reductive agent and constantly stir, the solution after finally reaction being terminated filters, and vacuum-drying, is placed in hydrogen atmosphere tube furnace and reacts 0.5 ~ 4h at 150 ~ 450 DEG C, obtain cadmium antimonide powder after cooling by the much filtrate obtained.All there is the weak points such as high to device dependence, synthesis cycle length, complicated operation, preparation cost are high several preparation in the method for cadmium antimonide powder above, these factors all seriously can govern mass preparation and the commercial applications of cadmium telluride.
Therefore, finding the low synthetic method of simple and fast, less energy consumption, preparation cost further for preparing cadmium antimonide powder, seeming very important.
Summary of the invention
The object of this invention is to provide a kind of novel method preparing high-purity cadmium telluride powder fast, the method has the advantages such as speed of response is fast, technique is simple, reproducible, energy-efficient, and the cadmium antimonide powder purity of preparation is high, is applicable to applying.
For achieving the above object, the technical solution used in the present invention is, a kind of novel method preparing high-purity cadmium telluride powder fast, comprises following processing step:
1) cadmium powder and tellurium powder are mixed by the mol ratio of 1:1, then carry out ground and mixed evenly, obtain mixing raw material;
2) by step 1) gained mixing raw material carries out colding pressing and makes block base substrate;
3) by step 2) block base substrate initiation self-propagating high-temperature building-up reactions (SHS) of gained, react rear naturally cooling, then gained reaction product has been ground, obtain single-phase high-purity cadmium telluride powder.
In such scheme, described step 1) in cadmium powder, tellurium powder quality purity all >=99.99%.
In such scheme, described step 2) in cold-press process be: pressurize 2 ~ 8min under 2 ~ 6MPa.
In such scheme, described step 3) in self-propagating high-temperature building-up reactions adopt the some end of type of heating to block base substrate to heat, detonate initiation self-propagating reaction in local.
In such scheme, described step 3) in use air atmosphere, inert atmosphere or vacuum condition in self-propagating reaction.
In such scheme, the gas that inert atmosphere selects argon gas etc. not react with cadmium powder, tellurium powder; Vacuum condition is≤10Pa.
According to such scheme, single-phase high-purity cadmium telluride powder can be obtained in 10min.
The present invention needs to provide necessary energy to bring out thermal chemical reaction to raw material, and form combustion wave, reaction after this just proceeds under the support of reacting institute's release of heat before, and self-propagating high-temperature combustion reactions terminates the cadmium telluride needed for rear formation.
Beneficial effect of the present invention is:
1) the present invention's high-purity cadmium telluride powder body material that adopted SHS technology to prepare first, has that speed of response is fast, equipment is simple, an advantage such as reproducible, energy-efficient and temperature rate is fast.
2) the present invention can prepare high-purity cadmium telluride powder body material in 10min, and what relate to is simple to operate, avoids numerous and diverse technical process, and the product purity of acquisition is high, and significantly improves production efficiency, is very applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram (XRD) of cadmium antimonide powder prepared by the embodiment of the present invention 1.
Fig. 2 is that magnification is from left to right respectively 1.00k times and 10.00k through the field emission scanning electron microscope figure without the primary product ground that self-propagating high-temperature building-up reactions obtains in the embodiment of the present invention 1.
Embodiment
For a better understanding of the present invention, illustrate content of the present invention further below in conjunction with drawings and Examples, but content of the present invention is not only confined to the following examples.
In following examples, the quality purity of Cd powder, Te powder all >=99.99%.
Embodiment 1
Prepare a novel method for high-purity cadmium telluride powder fast, comprise the following steps:
1) 4N cadmium powder and 4N tellurium powder are mixed by the mol ratio of 1:1, raw material total mass is 5g, then that raw material powder ground and mixed is even, obtains mixing raw material;
2) by step 1) the mixing raw material jin of gained carries out colding pressing and makes the cylindrical block base substrate that diameter is 10mm, and wherein pressing process is at 3MPa pressurize 5min;
3) by step 2) the block base substrate of gained carries out one end sparking mode and causes self-propagating high-temperature building-up reactions, reacted rear naturally cooling, can obtain high-purity cadmium antimonide powder after grinding.
Fig. 1 is the X-ray diffractogram (XRD) of the cadmium antimonide powder that the present embodiment obtains, show in figure: the powder product X-ray characteristic diffraction peak obtained after self-propagating high-temperature building-up reactions mates very well with (JCPDS#03-065-0440) characteristic peak of CdTe standard JC-PDF card, show to obtain single-phase cadmium antimonide powder in 10min by present method, for theoretical basis has been established in the preparation of its mass.
Fig. 2 is after self-propagating high-temperature building-up reactions, without the field emission scanning electron microscope figure (FESEM) of the primary product of grinding.Show the product obtained through self-propagating high-temperature building-up reactions in figure and there is no obvious orientation, and there is stair-stepping shape characteristic.
Embodiment 2
Prepare a novel method for high-purity cadmium telluride powdered material fast, it comprises the following steps:
1) 5N cadmium powder and 5N tellurium powder are mixed by the mol ratio of 1:1, raw material total mass is 10g, then by even for raw material powder ground and mixed;
2) by step 1) powder mixed that obtains is pressed into the cylindrical block base substrate that diameter is 12mm, and wherein pressing process is 4MPa pressurize 8min;
3) by step 2) the block base substrate of gained carries out one end sparking mode and causes self-propagating high-temperature building-up reactions, reacted rear naturally cooling, can obtain high-purity cadmium antimonide powder after grinding.
Embodiment 3
Prepare a novel method for high-purity cadmium telluride powdered material fast, it comprises the following steps:
1) 5N cadmium powder and 5N tellurium powder are mixed by the mol ratio of 1:1, raw material total mass is 20g, then by even for raw material powder ground and mixed;
2) by step 1) powder mixed that obtains is pressed into the cylindrical block base substrate that diameter is 15mm, and wherein pressing process is 5MPa pressurize 2min;
3) by step 2) the block base substrate of gained carries out one end sparking mode and causes self-propagating high-temperature building-up reactions, reacted rear naturally cooling, can obtain high-purity cadmium antimonide powder after grinding.
Embodiment 4
Prepare a novel method for high-purity cadmium telluride powdered material fast, it comprises the following steps:
1) 4N cadmium powder and 4N tellurium powder are mixed by the mol ratio of 1:1, raw material total mass is 20g, then by even for raw material powder ground and mixed;
2) by step 1) powder mixed that obtains is pressed into the cylindrical block base substrate that diameter is 20mm, and wherein pressing process is 5MPa pressurize 4min;
3) by step 2) the block base substrate of gained carries out one end sparking mode and causes self-propagating high-temperature building-up reactions, reacted rear naturally cooling, can obtain high-purity cadmium antimonide powder after grinding.
The foregoing is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, without departing from the concept of the premise of the invention, make some improvement and conversion, these all belong to protection scope of the present invention.
Claims (5)
1. prepare a novel method for high-purity cadmium telluride powder fast, it is characterized in that, comprise following processing step:
1) cadmium powder and tellurium powder are pressed the mixed in molar ratio of 1:1, then ground and mixed is even, obtains mixing raw material;
2) by step 1) gained mixing raw material carries out colding pressing and makes block base substrate;
3) by step 2) gained block base substrate initiation self-propagating high-temperature building-up reactions, react rear naturally cooling, then gained reaction product has been ground, obtain single-phase high-purity cadmium telluride powder.
2. the novel method preparing high-purity cadmium telluride powder fast according to claim 1, is characterized in that, described step 1) in cadmium powder, tellurium powder quality purity all >=99.99%.
3. the novel method preparing high-purity cadmium telluride powder fast according to claim 1, is characterized in that, described step 2) in cold-press process be: pressurize 2 ~ 8min under 2 ~ 6MPa.
4. the novel method preparing high-purity cadmium telluride powder fast according to claim 1, it is characterized in that, described step 3) in self-propagating high-temperature building-up reactions adopt the some end of type of heating to block base substrate to heat, detonate initiation self-propagating reaction in local.
5. the novel method preparing high-purity cadmium telluride powder fast according to claim 1, is characterized in that, can obtain single-phase high-purity cadmium telluride powder in 10min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110282975A (en) * | 2019-07-08 | 2019-09-27 | 先导薄膜材料（广东）有限公司 | A kind of Germanium selenide target and preparation method thereof |
| US11207731B2 (en) * | 2016-04-07 | 2021-12-28 | First Solar, Inc. | Devices and methods for making polycrystalline alloys |
-
2015
- 2015-05-12 CN CN201510238809.2A patent/CN104860272A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11207731B2 (en) * | 2016-04-07 | 2021-12-28 | First Solar, Inc. | Devices and methods for making polycrystalline alloys |
| CN110282975A (en) * | 2019-07-08 | 2019-09-27 | 先导薄膜材料（广东）有限公司 | A kind of Germanium selenide target and preparation method thereof |
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