CN113526955A - Preparation method of cadmium zinc telluride target - Google Patents
Preparation method of cadmium zinc telluride target Download PDFInfo
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- CN113526955A CN113526955A CN202110874417.0A CN202110874417A CN113526955A CN 113526955 A CN113526955 A CN 113526955A CN 202110874417 A CN202110874417 A CN 202110874417A CN 113526955 A CN113526955 A CN 113526955A
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- QWUZMTJBRUASOW-UHFFFAOYSA-N cadmium tellanylidenezinc Chemical compound [Zn].[Cd].[Te] QWUZMTJBRUASOW-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 37
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000007731 hot pressing Methods 0.000 claims abstract description 25
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000013077 target material Substances 0.000 claims abstract description 18
- 239000011812 mixed powder Substances 0.000 claims abstract description 17
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 11
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052714 tellurium Inorganic materials 0.000 abstract description 7
- 239000000843 powder Substances 0.000 abstract description 6
- SKJCKYVIQGBWTN-UHFFFAOYSA-N (4-hydroxyphenyl) methanesulfonate Chemical compound CS(=O)(=O)OC1=CC=C(O)C=C1 SKJCKYVIQGBWTN-UHFFFAOYSA-N 0.000 abstract description 3
- 238000011112 process operation Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/547—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on sulfides or selenides or tellurides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/40—Metallic constituents or additives not added as binding phase
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
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Abstract
The invention provides a preparation method of a cadmium zinc telluride target, which comprises the following steps: mixing tellurium powder, zinc powder and cadmium powder to obtain mixed powder; and carrying out vacuum hot-pressing sintering on the mixed powder to obtain the tellurium-zinc-cadmium target material. The preparation method of the cadmium zinc telluride target material provided by the invention has the advantages that the relative density of the prepared cadmium zinc telluride target material is more than 99%, the free cadmium and the free tellurium are less than 200ppm, the process is simple, the cadmium zinc telluride target material is directly synthesized by adopting three kinds of powder, cadmium telluride and zinc telluride do not need to be synthesized, the process operation is reduced, and the cost is saved.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a preparation method of a cadmium zinc telluride target.
Background
The chemical formula of cadmium telluride is CdTe, the molecular weight is 240.00, and the cadmium telluride is an important II-VI compound semiconductor material and is mainly used for thin film solar energy; a small amount of Zn is doped into cadmium telluride to form cadmium zinc telluride, so that the carrier concentration of the cadmium telluride thin film can be improved, and the photoelectric conversion efficiency can be improved. However, the prior art for preparing cadmium zinc telluride has complex process.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing a cadmium zinc telluride target, which has a simple process, and the prepared cadmium zinc telluride target has a high relative density and low free cadmium and free tellurium contents.
The invention provides a preparation method of a cadmium zinc telluride target, which comprises the following steps:
mixing tellurium powder, zinc powder and cadmium powder to obtain mixed powder;
and carrying out vacuum hot-pressing sintering on the mixed powder to obtain the tellurium-zinc-cadmium target material.
Preferably, the molar ratio of the tellurium powder, the cadmium powder and the zinc powder is 1:1: (0.03-0.06).
Preferably, the tellurium powder has a particle size of less than 200 microns.
Preferably, the particle size of the zinc powder is less than 200 microns.
Preferably, the cadmium powder has a particle size of less than 200 microns.
Preferably, the vacuum hot-pressing sintering further comprises:
and putting the mixed powder into a mould and then carrying out vacuum hot-pressing sintering.
Preferably, the vacuum hot-pressing sintering method comprises the following steps:
raising the temperature to a first temperature at a first speed under a vacuum environment, preserving the heat for a first time, and then raising the temperature to a second temperature at a second speed, preserving the heat for a second time;
the first speed is 1-3 ℃/min; the first temperature is 350-450 ℃; the first time is 1-3 hours;
the second speed is 5-10 ℃/min; the second temperature is 650-750 ℃; the second time is 1.5-2 hours.
Preferably, the vacuum degree of the vacuum environment is less than 10 Pa.
Preferably, the pressurizing method in the vacuum hot-pressing sintering process comprises the following steps:
when the temperature reaches the second temperature and the temperature is kept for the third time, pressurizing and maintaining the pressure;
the third time is 15-20 min.
Preferably, the pressurizing pressure is 35-55 MPa;
and the pressure maintaining time is 30-60 min.
The preparation method of the cadmium zinc telluride target material provided by the invention has the advantages that the relative density of the prepared cadmium zinc telluride target material is more than 99%, the free cadmium and the free tellurium are less than 200ppm, the process is simple, the cadmium zinc telluride target material is directly synthesized by adopting three kinds of powder, cadmium telluride and zinc telluride do not need to be synthesized, the process operation is reduced, and the cost is saved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The invention provides a preparation method of a cadmium zinc telluride target, which comprises the following steps:
mixing tellurium powder, zinc powder and cadmium powder to obtain mixed powder;
and carrying out vacuum hot-pressing sintering on the mixed powder to obtain the tellurium-zinc-cadmium target material.
In the invention, the molar ratio of the tellurium powder, the cadmium powder and the zinc powder is preferably 1:1: (0.03 to 0.06), more preferably 1:1: (0.04-0.05).
In the invention, the granularity of the tellurium powder is preferably less than 200 microns.
In the present invention, the zinc powder preferably has a particle size of less than 200 μm.
In the present invention, the cadmium powder preferably has a particle size of less than 200 μm.
In the present invention, the mixing is preferably uniform.
In the present invention, before the vacuum hot pressing sintering, the vacuum hot pressing sintering preferably further comprises:
and putting the mixed powder into a mould and then carrying out vacuum hot-pressing sintering.
In the present invention, the vacuum hot press sintering is preferably performed in a vacuum hot press furnace.
In the present invention, the vacuum hot press sintering method preferably includes:
raising the temperature to a first temperature at a first speed under a vacuum environment, keeping the temperature for a first time, and then raising the temperature to a second temperature at a second speed, keeping the temperature for a second time.
In the present invention, the degree of vacuum of the vacuum environment is preferably < 10 Pa.
In the present invention, the first speed is preferably 1 to 3 ℃/min, more preferably 1.5 to 2.5 ℃/min, and most preferably 2 ℃/min.
In the invention, the first temperature is preferably 350-450 ℃, more preferably 380-420 ℃, and most preferably 400 ℃.
In the present invention, the first time is preferably 1 to 3 hours, more preferably 1.5 to 2.5 hours, and most preferably 2 hours.
In the present invention, the second speed is preferably 5 to 10 ℃/min, more preferably 6 to 9 ℃/min, and most preferably 7 to 8 ℃/min.
In the present invention, the second temperature is preferably 650 to 750 ℃, more preferably 680 to 720 ℃, and most preferably 700 ℃.
In the present invention, the second time is preferably 1.5 to 2 hours, more preferably 1.6 to 1.9 hours, and most preferably 1.7 to 1.8 hours.
In the present invention, the pressurizing method in the vacuum hot press sintering process preferably includes:
and starting pressurization and maintaining pressure after the temperature reaches the second temperature and the heat preservation is carried out for the third time.
In the present invention, the second temperature is the same as the second temperature in the above technical solution, and details are not repeated here.
In the invention, the third time is preferably 15-20 min, more preferably 16-19 min, and most preferably 17-18 min.
In the present invention, the pressure for pressurization is preferably 35 to 55MPa, more preferably 40 to 50MPa, and most preferably 45 MPa.
In the present invention, the pressure maintaining time is preferably 30 to 60min, more preferably 40 to 50min, and most preferably 45 min.
The relative density of the tellurium-zinc-cadmium target material prepared by the method provided by the invention is more than 99%, the free cadmium and the free tellurium are less than 200ppm, the process is simple, the tellurium-zinc-cadmium target material is directly synthesized by three kinds of powder without synthesizing cadmium telluride and zinc telluride, the process operation is reduced, and the cost is saved.
Example 1
Tellurium powder, cadmium powder and zinc powder are mixed uniformly according to the molar ratio of 1:1:0.03, and the particles of the three kinds of powder are smaller than 200 microns to obtain mixed powder;
putting the mixed powder into a mould, and putting the mould into a vacuum hot pressing furnace for vacuum hot pressing and sintering to obtain a tellurium-zinc-cadmium target material;
the vacuum hot-pressing sintering method comprises the following steps: the vacuum degree is less than 10Pa, the temperature is raised to 350 ℃ at the speed of 2 ℃/min, and the temperature is kept for 2 hours; then heating to 750 ℃ at a speed of 10 ℃/min, and preserving heat for 2 hours; the pressurizing method in the vacuum hot-pressing sintering process comprises the following steps: and when the temperature reaches 750 ℃, keeping the temperature for 17min, and then starting pressurizing, wherein the pressurizing pressure is 35MPa, and the pressure maintaining time is 40 min.
Example 2
Tellurium powder, cadmium powder and zinc powder are mixed evenly according to the molar ratio of 1:1:0.04, and the particles of the three kinds of powder are smaller than 200 microns to obtain mixed powder;
putting the mixed powder into a mold, and putting the mold into a vacuum hot pressing furnace for vacuum hot pressing and sintering to obtain a cadmium zinc telluride target;
the vacuum hot-pressing sintering method comprises the following steps: the vacuum degree is less than 10Pa, the temperature is raised to 450 ℃ at the speed of 1 ℃/min, and the temperature is kept for 1.5 hours; then heating to 650 ℃ at the speed of 8 ℃/min, and preserving heat for 1 hour; the pressurizing method in the hot-pressing sintering process comprises the following steps: and when the temperature reaches 650 ℃, keeping the temperature for 15min, and then starting pressurizing, wherein the pressurizing pressure is 45MPa, and the pressure maintaining time is 50 min.
Example 3
Mixing tellurium powder, cadmium powder and zinc powder uniformly according to a molar ratio of 1:1:0.06, wherein the particles of the three kinds of powder are less than 200 microns to obtain mixed powder;
putting the mixed powder into a mold, and putting the mold into a vacuum hot pressing furnace for vacuum hot pressing and sintering to obtain a cadmium zinc telluride target;
the vacuum hot-pressing sintering method comprises the steps of heating to 400 ℃ at the speed of 3 ℃/min under the condition that the vacuum degree is less than 10Pa, and preserving heat for 3 hours; then raising the temperature to 700 ℃ at a speed of 58 ℃/min, and preserving the heat for 1.5 hours; the pressurizing method in the vacuum hot-pressing sintering process comprises the following steps: and when the temperature reaches 700 ℃, keeping the temperature for 15min, and then starting pressurizing, wherein the pressurizing pressure is 35MPa, and the pressure maintaining time is 40 min.
Performance detection
Detecting the relative density of the cadmium zinc telluride target material prepared by the embodiment of the invention by adopting an Archimedes drainage method;
detecting free cadmium and free tellurium in the cadmium zinc telluride target material prepared by the embodiment of the invention by adopting differential scanning calorimetry analysis;
the results are shown in Table 1.
Table 1 test results of products prepared in the examples of the present invention
| Relative density of target material | Free cadmium | Free tellurium | |
| Example 1 | 99.1％ | ＜100ppm | ＜100ppm |
| Example 2 | 99.2％ | ＜100ppm | ＜100ppm |
| Example 3 | 99.1％ | ＜100ppm | ＜100ppm |
From the above embodiments, it can be known that the relative density of the tellurium-zinc-cadmium target material prepared by the preparation method of the tellurium-zinc-cadmium target material provided by the invention is greater than 99%, the free cadmium and the free tellurium are less than 200ppm, and the process is simple.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a cadmium zinc telluride target comprises the following steps:
mixing tellurium powder, zinc powder and cadmium powder to obtain mixed powder;
and carrying out vacuum hot-pressing sintering on the mixed powder to obtain the tellurium-zinc-cadmium target material.
2. The method as claimed in claim 1, wherein the molar ratio of tellurium powder, cadmium powder and zinc powder is 1:1: (0.03-0.06).
3. The method of claim 1, wherein the tellurium powder has a particle size of less than 200 microns.
4. The method as defined in claim 1, characterized in that said zinc powder has a particle size of less than 200 μm.
5. The method of claim 1, wherein the cadmium powder has a particle size of less than 200 microns.
6. The method of claim 1, wherein the vacuum hot press sintering further comprises, prior to:
and putting the mixed powder into a mould and then carrying out vacuum hot-pressing sintering.
7. The method of claim 1, wherein the vacuum hot press sintering method comprises:
raising the temperature to a first temperature at a first speed under a vacuum environment, preserving the heat for a first time, and then raising the temperature to a second temperature at a second speed, preserving the heat for a second time;
the first speed is 1-3 ℃/min; the first temperature is 350-450 ℃; the first time is 1-3 hours;
the second speed is 5-10 ℃/min; the second temperature is 650-750 ℃; the second time is 1.5-2 hours.
8. The method of claim 7, wherein the vacuum environment has a vacuum level of < 10 Pa.
9. The method of claim 7, wherein the pressurizing method in the vacuum hot pressing sintering process comprises:
when the temperature reaches the second temperature and the temperature is kept for the third time, pressurizing and maintaining the pressure;
the third time is 15-20 min.
10. The method according to claim 9, wherein the pressurization pressure is 35 to 55 MPa;
and the pressure maintaining time is 30-60 min.
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| JPH03162570A (en) * | 1989-11-20 | 1991-07-12 | Toshiba Corp | Sputtering target and production thereof |
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2021
- 2021-07-30 CN CN202110874417.0A patent/CN113526955A/en active Pending
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| JPH03162570A (en) * | 1989-11-20 | 1991-07-12 | Toshiba Corp | Sputtering target and production thereof |
| CN102492927A (en) * | 2011-12-08 | 2012-06-13 | 上海太阳能电池研究与发展中心 | Method for preparing tellurium-zinc-cadmium film material with adjustable forbidden bandwidth |
| CN106380198A (en) * | 2016-09-20 | 2017-02-08 | 广东先导稀材股份有限公司 | Cadmium zinc telluride target material as well as preparation method and application thereof |
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