CN117209277A - Preparation method of cuprous telluride powder and target material - Google Patents
Preparation method of cuprous telluride powder and target material Download PDFInfo
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- CN117209277A CN117209277A CN202311192560.7A CN202311192560A CN117209277A CN 117209277 A CN117209277 A CN 117209277A CN 202311192560 A CN202311192560 A CN 202311192560A CN 117209277 A CN117209277 A CN 117209277A
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- cuprous telluride
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- cuprous
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- MZEWONGNQNXVKA-UHFFFAOYSA-N [Cu].[Cu].[Te] Chemical compound [Cu].[Cu].[Te] MZEWONGNQNXVKA-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000000843 powder Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000013077 target material Substances 0.000 title abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 56
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 18
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004321 preservation Methods 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 11
- 239000010949 copper Substances 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 7
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000007731 hot pressing Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 238000005245 sintering Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 238000007599 discharging Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910052714 tellurium Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910004613 CdTe Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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Abstract
The application belongs to the field of material preparation, and discloses cuprous telluride powder and a preparation method of a target material. The preparation method of the cuprous telluride powder comprises the following steps: mixing tellurium powder and copper powder, and carrying out heating reaction under the conditions of hydrogen atmosphere and temperature of 350-400 ℃ to obtain cuprous telluride powder. Carrying out a heating reaction by taking cuprous telluride powder as a raw material to obtain a cuprous telluride target; the heating mode of the heating reaction is as follows: heating to 600-650 ℃ under vacuum condition, and preserving heat for 90-120 min; and after the temperature is raised to the highest temperature, pressurizing to 60-70 mpa, and maintaining the pressure until the heat preservation time is finished. The method for preparing the cuprous telluride powder by adopting the tubular furnace low-temperature powder synthesis method can realize mass production, has low requirements on equipment, adopts vacuum hot-pressing sintering to prepare the cuprous telluride target, has short process flow and simple and convenient operation, and the obtained cuprous telluride target has low oxygen content and high relative density.
Description
Technical Field
The application belongs to the field of material preparation, and relates to cuprous telluride powder and a preparation method of a target material.
Background
Cuprous telluride (Cu) 2 Te) is an important semiconductor material with an octahedral crystal structure belonging to the group of metal chalcogenides. Cuprous telluride has unique ionic conductivity and thermoelectric property and is widely applied to the fields of solar cells, thermoelectric materials and the like. In CdS/CdTIn e solar cell, cu 2 Te is used as an intermediate layer to balance the work function of the external electrode and the valence state of the CdTe material, so that a back surface electric field is formed to reduce the load probability of carriers, and the efficiency of the solar cell is greatly improved.
There are many Cu in the literature 2 Study of Te preparation. For example, patent document with publication number CN106241752B discloses a preparation method of cuprous telluride, comprising the following steps: mixing simple substance copper and simple substance tellurium, and heating to react under the vacuum condition to obtain cuprous telluride. The heating mode of the heating reaction is as follows: a) Heating to 400-550 ℃, and preserving heat for 1-2 hours, wherein the heating rate of heating is 5-10 ℃/min; b) Heating to 850-950 ℃, and preserving heat for 1-3 hours, wherein the heating rate of heating is 3-6 ℃/min; c) Heating to 1100-1180 ℃, and preserving heat for 2-4 hours, wherein the heating rate is 3-6 ℃ per minute. The preparation method is complex, the heating process is three-stage sintering, the steps are complex, the equipment requirements are high in the preparation process, and the temperature regulation and control conditions are severe.
Disclosure of Invention
The application aims to provide a preparation method of cuprous telluride powder, which has a simple and easily controlled process.
The second purpose of the application is to provide a preparation method of the cuprous telluride target.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows:
a method for preparing cuprous telluride powder, comprising the following steps:
mixing tellurium powder and copper powder, and carrying out heating reaction under the conditions of hydrogen atmosphere and temperature of 350-400 ℃ to obtain cuprous telluride powder.
Considering that the vapor pressure of copper powder is large, the copper powder is difficult to remove, and the tellurium powder is excessive, so that copper can fully react, free tellurium is removed well in the follow-up process, and further, the molar ratio of the tellurium powder to the copper powder is 1.1-1.2: 2, uniformly mixing.
Further, tellurium powder of-100 mesh was used, and copper powder of-100 mesh was used. The smaller the particles of the powder, the better the activity, the more complete the reaction and the lower the reaction temperature.
Considering the low temperature reaction of the powder, the reaction is carried out at the temperature, the speed is too high, the reaction is incomplete, too low tellurium can volatilize much, and further, in the heating reaction process: heating to 350-400 ℃ at a heating rate of 5-10 ℃/min, and reacting for 90-120 min.
Further, during the heating reaction: the flow of the hydrogen is 5-10L/min. In the reaction process, hydrogen is introduced, so that the reduction effect can be achieved. Avoid high oxygen after synthesis of cuprous telluride. Meanwhile, the powder has large specific surface area, is contacted with hydrogen gas and is easier to deoxidize.
The preparation method of the cuprous telluride target material comprises the steps of taking the cuprous telluride powder prepared by the preparation method of the cuprous telluride powder as a raw material to carry out heating reaction to obtain the cuprous telluride target material;
the heating mode of the heating reaction is as follows:
heating to 600-650 ℃ under vacuum condition, and preserving heat for 90-120 min;
and after the temperature is raised to the highest temperature, pressurizing to 60-70 mpa, and maintaining the pressure until the heat preservation time is finished.
Further, during the heating reaction: heating to 600-650 ℃ at 8-12 ℃/min, and preserving heat for 90-120 min; and after the temperature is raised to the highest temperature, pressurizing to 80-90 mpa in 20min, and maintaining the pressure until the heat preservation time is finished. At a certain temperature, the powder is fully expanded, and the pressurizing rate is controlled to achieve the densification process.
Further, the cuprous telluride powder is filled into a die, and is put into a vacuum hot-pressing furnace for heating reaction.
Further, in the reaction process, the vacuum condition is specifically that the vacuum degree is not more than 10pa.
Further, after the heat preservation is finished, the furnace also comprises cooling, and the cooling mode is cooling along with the furnace.
Compared with the prior art, the application has the beneficial effects that:
the method adopts the tubular furnace low-temperature powder synthesis method to prepare the cuprous telluride powder, can realize mass production, has low equipment requirement, and the used reaction graphite boat can be reused, and has low cost; hydrogen is directly introduced in the synthesis process, so that the aim of directly deoxidizing in the synthesis process is fulfilled.
The method adopts vacuum hot-pressed sintering to prepare the cuprous telluride target, has short process flow and simple and convenient operation, and the obtained cuprous telluride target has low oxygen content and high relative density.
Detailed Description
The present application will be described more fully hereinafter with reference to the preferred embodiments for the purpose of facilitating understanding of the present application, but the scope of protection of the present application is not limited to the specific embodiments described below.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present application.
Example 1
The method comprises the following steps:
(1) Tellurium powder with the mesh of-100 and copper powder with the mesh of-100 are mixed according to the mol ratio of 1.1:2 are filled into a tubular atmosphere furnace.
(2) Firstly, introducing nitrogen with the flow of 10L/min for 30min, then starting heating, switching the nitrogen into hydrogen, heating to 400 ℃ at the speed of 6 ℃ per min, and preserving heat for 90min.
(3) After cooling, the hydrogen is turned off, the inert gas is introduced to replace the hydrogen in the tube, and the copper telluride powder is obtained after discharging.
(4) Crushing cuprous telluride powder to minus 325 meshes, loading into a mould, putting into a vacuum hot-pressing furnace for hot pressing, heating to 630 ℃ at a speed of 12 ℃/min, and preserving heat for 100min; pressurizing to 70MPa within 20min after heating to the highest temperature, and maintaining the pressure to cool.
(5) And cooling to room temperature, demolding, and performing mechanical processing to obtain the cuprous telluride target.
Example 2
The method comprises the following steps:
(1) Tellurium powder with the mesh of-100 and copper powder with the mesh of-100 are mixed according to the mol ratio of 1.2:2 are filled into a tubular atmosphere furnace.
(2) Firstly, introducing nitrogen with the flow of 5L/min for 50min, then starting heating, switching the nitrogen into hydrogen, heating to 350 ℃ at 10 ℃ per min, and preserving heat for 100min.
(3) After cooling, the hydrogen is turned off, the inert gas is introduced to replace the hydrogen in the tube, and the copper telluride powder is obtained after discharging.
(4) Crushing cuprous telluride powder to minus 325 meshes, loading into a mould, putting into a vacuum hot pressing furnace for hot pressing, heating to 600 ℃ at 8 ℃/min, and preserving heat for 90min; pressurizing to 70MPa within 20min after heating to the highest temperature, and maintaining the pressure to cool.
(5) And cooling to room temperature, demolding, and performing mechanical processing to obtain the cuprous telluride target.
Example 3
The method comprises the following steps:
(1) Tellurium powder with the mesh of-100 and copper powder with the mesh of-100 are mixed according to the mol ratio of 1.2:2 are filled into a tubular atmosphere furnace.
(2) Firstly, introducing nitrogen with the flow of 8L/min for 40min, then starting heating, switching the nitrogen into hydrogen, heating to 380 ℃ at 5 ℃ per min, and preserving heat for 100min.
(3) After cooling, the hydrogen is turned off, the inert gas is introduced to replace the hydrogen in the tube, and the copper telluride powder is obtained after discharging.
(4) Crushing cuprous telluride powder to minus 325 meshes, loading into a mould, putting into a vacuum hot-pressing furnace for hot pressing, heating to 650 ℃ at a speed of 12 ℃/min, and preserving heat for 120min; after the temperature is raised to the highest temperature, the pressure is increased to 60Mpa in 20min, and the pressure is maintained until the temperature is reduced.
(5) And cooling to room temperature, demolding, and performing mechanical processing to obtain the cuprous telluride target.
Comparative example 1
Comparative example 1 is substantially identical to example 1 except that: in the steps (2) and (3) of comparative example 1, no hydrogen was introduced, and nitrogen was introduced directly. The method comprises the following steps:
(2) Introducing nitrogen with the flow of 10L/min for 30min, then starting heating, heating to 400 ℃ at the speed of 6 ℃ per min, preserving heat for 90min,
(3) After cooling, keeping nitrogen atmosphere, and discharging to obtain cuprous telluride powder.
Comparative example 2
Comparative example 2 is substantially identical to example 1, except that: the difference in the step (2) is specifically:
(2) Firstly, introducing nitrogen with the flow of 10L/min for 30min, then starting heating, switching the nitrogen into hydrogen, heating to 600 ℃ at the speed of 6 ℃ per min, and preserving heat for 90min.
This comparative example failed to synthesize cuprous telluride powder and the presence of metallic copper did not react completely.
The cuprous telluride targets obtained in examples 1 to 3 and comparative example 1/2 were tested, and the test data are shown in table 1.
Table 1 test data
The cuprous telluride target product prepared by the method has stable quality, low oxygen content and high relative density of the target.
The above is only a preferred embodiment of the present application, and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the present application.
Claims (10)
1. The preparation method of the cuprous telluride powder is characterized by comprising the following steps of:
mixing tellurium powder and copper powder, and carrying out heating reaction under the conditions of hydrogen atmosphere and temperature of 350-400 ℃ to obtain cuprous telluride powder.
2. A method for preparing cuprous telluride powder according to claim 1, wherein the molar ratio of tellurium powder to copper powder is 1.1-1.2: 2, uniformly mixing.
3. A method for preparing a copper telluride powder according to claim 1, wherein-100 mesh tellurium powder is used and-100 mesh copper powder is used.
4. A method for preparing the cuprous telluride powder as claimed in claim 1, wherein during the heating reaction: heating to 350-400 ℃ at a heating rate of 5-10 ℃/min, and reacting for 90-120 min.
5. A method for preparing the cuprous telluride powder as claimed in claim 1, wherein during the heating reaction: the flow of the hydrogen is 5-10L/min.
6. A method for preparing a cuprous telluride target, which is characterized in that cuprous telluride powder prepared by the method for preparing cuprous telluride powder according to any one of claims 1-5 is used as a raw material for heating reaction to obtain the cuprous telluride target;
the heating mode of the heating reaction is as follows:
heating to 600-650 ℃ under vacuum condition, and preserving heat for 90-120 min;
and after the temperature is raised to the highest temperature, pressurizing to 60-70 mpa, and maintaining the pressure until the heat preservation time is finished.
7. A method for preparing a cuprous telluride target as claimed in claim 6 wherein during the heating reaction: heating to 600-650 ℃ at 8-12 ℃/min, and preserving heat for 90-120 min; and after the temperature is raised to the highest temperature, pressurizing to 80-90 mpa in 20min, and maintaining the pressure until the heat preservation time is finished.
8. A method for preparing a cuprous telluride target as claimed in claim 6 wherein cuprous telluride powder is loaded into a die and placed into a vacuum autoclave for heating reaction.
9. A method for preparing a cuprous telluride target as claimed in claim 6 wherein vacuum condition during reaction is specifically vacuum degree of not more than 10pa.
10. A method for preparing a cuprous telluride target as claimed in claim 6, wherein after heat preservation, the method further comprises cooling in a furnace-like manner.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311192560.7A CN117209277A (en) | 2023-09-15 | 2023-09-15 | Preparation method of cuprous telluride powder and target material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311192560.7A CN117209277A (en) | 2023-09-15 | 2023-09-15 | Preparation method of cuprous telluride powder and target material |
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| CN117209277A true CN117209277A (en) | 2023-12-12 |
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| CN202311192560.7A Pending CN117209277A (en) | 2023-09-15 | 2023-09-15 | Preparation method of cuprous telluride powder and target material |
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- 2023-09-15 CN CN202311192560.7A patent/CN117209277A/en active Pending
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