CN114059170A - Growth method of cadmium telluride crystal - Google Patents
Growth method of cadmium telluride crystal Download PDFInfo
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- CN114059170A CN114059170A CN202111323511.3A CN202111323511A CN114059170A CN 114059170 A CN114059170 A CN 114059170A CN 202111323511 A CN202111323511 A CN 202111323511A CN 114059170 A CN114059170 A CN 114059170A
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- Prior art keywords
- crystal
- cadmium telluride
- cadmium
- crucible
- tellurium
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- 239000013078 crystal Substances 0.000 title claims abstract description 84
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 7
- 229910052714 tellurium Inorganic materials 0.000 claims description 8
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 8
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001514 detection method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The application discloses a growth method of a cadmium telluride crystal, which comprises the following steps: placing a cadmium telluride seed crystal at the bottom of a crucible, placing a tellurium-cadmium mixture on the seed crystal, and sealing the crucible; secondly, putting the crucible into a growth furnace, and heating to melt the tellurium-cadmium mixture; step three, at a speed V1Cooling to 0.5 deg.C/h or below to gradually precipitate cadmium telluride until the temperature is reduced to 450 deg.C, and adding V2Rapidly cooling at a speed of less than or equal to 25 ℃/h to obtain the cadmium telluride crystal. The growth method of the cadmium telluride crystal disclosed by the invention is simple in process, and the single crystal prepared by the method has the advantages of high single crystal rate and low dislocation density.
Description
Technical Field
The invention relates to the field of crystal preparation, in particular to a growth method of a cadmium telluride crystal.
Background
The cadmium telluride crystal is an important semiconductor crystal, namely a sphalerite structure, has a direct transition type energy band structure, and the forbidden band width of the cadmium telluride crystal is 1.45 eV. CdTe can be easily incorporated into n-type or p-type semiconductor materials by doping with various impurities. When the position of Cd is replaced with In, an n-type semiconductor is formed. When the position of Cd is replaced by Cu, Ag and Au, a p-type semiconductor is formed. The cadmium telluride crystal can be used for spectral analysis, infrared electro-optic modulators, infrared detectors, infrared lenses and windows, phosphors, normal-temperature gamma ray detectors, light-emitting devices close to the visible light region and the like.
Cadmium telluride is difficult to make into large diameter bulk single crystals and many materials are often used as epitaxial thin films. The stacking defect energy (stacking fault) of the cadmium telluride crystal is very low, and polycrystalline or twin crystals are easy to grow in the crystal growth process. In order to overcome the difficulty in the crystal growth process, researchers develop various cadmium telluride crystal growth methods including a VB method, a VGF method, a THM method and the like, but the growth problem of large-size single crystals cannot be solved. Therefore, there is a need to develop a new cadmium telluride crystal growth technology.
Disclosure of Invention
In view of the problems in the background art, it is an object of the present disclosure to provide a method for growing a cadmium telluride crystal.
In order to achieve the above object, the present disclosure provides a method for growing a cadmium telluride crystal, comprising the steps of: placing a cadmium telluride seed crystal at the bottom of a crucible, placing a tellurium-cadmium mixture on the seed crystal, and sealing the crucible; secondly, putting the crucible into a growth furnace, and heating to melt the tellurium-cadmium mixture; step three, at a speed V1Cooling to 0.5 deg.C/h or below to gradually precipitate cadmium telluride until the temperature is reduced to 450 deg.C, and adding V2Rapidly cooling at a speed of less than or equal to 25 ℃/h to obtain the cadmium telluride crystal.
In some embodiments, in the step one, the height of the cadmium telluride seed crystal at the bottom of the crucible is 15-30 mm.
In some embodiments, in the first step, the molar ratio of tellurium to cadmium in the tellurium-cadmium mixture is 2-4: 1.
In some embodiments, in step two, the temperature T is related to the molar ratio x of tellurium to cadmium in the tellurium-cadmium mixture as T ═ 74exp (2.426x) + 1339.
In some embodiments, in step three, the V1Is 0.1 ℃/h to 0.5 ℃/h.
In some embodiments, in step three, the V2Is 5 ℃/h to 25 ℃/h.
The beneficial effects of this disclosure are as follows:
the growth method of the cadmium telluride crystal disclosed by the invention is simple in process, and the single crystal prepared by the method has the advantages of high single crystal rate and low dislocation density.
Detailed Description
The method of growing a cadmium telluride crystal according to the present disclosure is explained in detail below.
The application discloses a growth method of a cadmium telluride crystal, which comprises the following steps: placing a cadmium telluride seed crystal at the bottom of a crucible, placing a tellurium-cadmium mixture on the seed crystal, and sealing the crucible; secondly, putting the crucible into a growth furnace, and heating to melt the tellurium-cadmium mixture; step three, at a speed V1Cooling to 0.5 deg.C/h or below to gradually precipitate cadmium telluride until the temperature is reduced to 450 deg.C, and adding V2Rapidly cooling at a speed of less than or equal to 25 ℃/h to obtain the cadmium telluride crystal.
In some embodiments, in step one, the cadmium telluride seed crystal is 15mm to 30mm in height at the bottom of the crucible. The cadmium telluride seed crystal is too high at the bottom of the crucible, which causes waste; the height of the cadmium telluride seed crystal at the bottom of the crucible is too low, and the seed crystal can be completely melted in the material melting stage.
In some embodiments, in the first step, the molar ratio of tellurium to cadmium in the tellurium-cadmium mixture is 2-4: 1. the waste is caused by too high tellurium content, the crystal growth temperature is increased by too low tellurium content, and the crystal defects are increased.
In some embodiments, in step two, the temperature T is related to the molar ratio x of tellurium to cadmium in the tellurium-cadmium mixture as T ═ 74exp (2.426x) + 1339. Temperatures above this will cause the seed to dissolve too much, or even completely melt. Temperatures below this temperature will cause the mix to not melt completely, resulting in the formation of inclusions or polycrystallites in the crystals.
In some embodiments, in step three, the V1Is 0.1 ℃/h to 0.5 ℃/h. The higher cooling rate easily causes the crystal to grow too fast, and twin crystals or polycrystal is generated in the crystal. In the second step, after the temperature is reduced to 450 ℃, the temperature is reduced for the second time, and when the temperature is higher than 450 ℃, the crystal growth is not completed.
In some embodimentsIn step three, the V2Is 5 ℃/h to 25 ℃/h. The temperature reduction rate is higher than 25 ℃, which causes excessive crystal stress and crystal cracking.
[ test procedures and test results ]
Example 1
Placing a cadmium telluride seed crystal at the bottom of a crucible with the height of 30mm, placing a tellurium-cadmium mixture with the molar ratio of 2: 1 on the seed crystal, and sealing the crucible;
step two, putting the crucible into a growth furnace, heating to 966 ℃ to melt the tellurium-cadmium mixture;
and step three, cooling at the speed of 0.5 ℃/h to gradually precipitate cadmium telluride until the temperature is reduced to 450 ℃, and then rapidly cooling at the speed of 25 ℃/h to obtain the cadmium telluride crystal.
Through detection, the cadmium telluride single crystal rate is 75 percent, and the dislocation density is 3 multiplied by 103cm-2。
Example 2
Placing a cadmium telluride seed crystal at the bottom of a crucible, wherein the height of the cadmium telluride seed crystal is 15mm, placing a tellurium-cadmium mixture with a molar ratio of 4: 1 on the seed crystal, and sealing the crucible;
step two, putting the crucible into a growth furnace, heating to 823 ℃, and melting the tellurium-cadmium mixture;
and step three, cooling at the speed of 0.1 ℃/h to gradually precipitate cadmium telluride until the temperature is reduced to 450 ℃, and then rapidly cooling at the speed of 5 ℃/h to obtain the cadmium telluride crystal.
Through detection, the cadmium telluride single crystal rate is 85 percent, and the dislocation density is 1.5 multiplied by 103cm-2。
Comparative example 1
Step one, placing a cadmium telluride seed crystal at the bottom of a crucible with the height of 5mm, placing a tellurium-cadmium mixture with the molar ratio of 4: 1 on the seed crystal, and sealing the crucible;
the second and third steps are the same as in example 2.
Through detection, the seed crystal is fused, the cadmium telluride single crystal rate is 15%, and the dislocation density is 8 multiplied by 104cm-2。
Comparative example 2
Step two, putting the crucible into a growth furnace, heating to 1093 ℃ to melt the tellurium-cadmium mixture;
the rest is the same as example 1.
Through detection, the seed crystal is fused, the cadmium telluride single crystal rate is 10%, and the dislocation density is 1 multiplied by 105cm-2。
Comparative example 3
Step two, putting the crucible into a growth furnace, heating to 900 ℃ to melt the tellurium-cadmium mixture;
the rest is the same as example 1.
After detection, the crystal is taken out, and a large amount of polycrystal is mixed in the crystal, so that no single crystal is produced.
Comparative example 4
And step three, cooling at the speed of 0.6 ℃/h to gradually precipitate cadmium telluride until the temperature is reduced to 450 ℃, and then rapidly cooling at the speed of 25 ℃/h to obtain the cadmium telluride crystal.
The rest of the procedure is the same as in example 1
After detection, the crystal is taken out, a small amount of impurities and bubbles exist in the crystal, and no complete single crystal is produced.
Comparative example 5
And step three, cooling at the speed of 0.5 ℃/h to gradually precipitate cadmium telluride until the temperature is reduced to 450 ℃, and then rapidly cooling at the speed of 30 ℃/h to obtain the cadmium telluride crystal.
The rest of the procedure is the same as in example 1
And (5) taking out the crystal after detection, and cracking the crystal.
The above-disclosed features are not intended to limit the scope of practice of the present disclosure, and therefore, all equivalent variations that are described in the claims of the present disclosure are intended to be included within the scope of the claims of the present disclosure.
Claims (6)
1. A growth method of cadmium telluride crystals is characterized by comprising the following steps:
placing a cadmium telluride seed crystal at the bottom of a crucible, placing a tellurium-cadmium mixture on the seed crystal, and sealing the crucible;
secondly, putting the crucible into a growth furnace, and heating to melt the tellurium-cadmium mixture;
step three, at a speed V1Cooling to 0.5 deg.C/h or below to gradually precipitate cadmium telluride until the temperature is reduced to 450 deg.C, and adding V2Rapidly cooling at a speed of less than or equal to 25 ℃/h to obtain the cadmium telluride crystal.
2. The method of growing a cadmium telluride crystal as set forth in claim 1,
in the first step, the height of the cadmium telluride seed crystal at the bottom of the crucible is 15-30 mm.
3. The method of growing a cadmium telluride crystal as set forth in claim 1,
in the first step, the molar ratio of tellurium to cadmium in the tellurium-cadmium mixture is 2-4: 1.
4. The method of growing a cadmium telluride crystal as set forth in claim 1,
in the second step, the relationship between the temperature-rising temperature T and the molar ratio x of the tellurium to the cadmium mixture is T-74 exp (2.426x) + 1339.
5. The method of growing a cadmium telluride crystal as set forth in claim 1,
in step three, the V1Is 0.1 ℃/h to 0.5 ℃/h.
6. The method of growing a cadmium telluride crystal as set forth in claim 1,
in step three, the V2Is 5 ℃/h to 25 ℃/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111323511.3A CN114059170A (en) | 2021-11-09 | 2021-11-09 | Growth method of cadmium telluride crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111323511.3A CN114059170A (en) | 2021-11-09 | 2021-11-09 | Growth method of cadmium telluride crystal |
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| Publication Number | Publication Date |
|---|---|
| CN114059170A true CN114059170A (en) | 2022-02-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202111323511.3A Pending CN114059170A (en) | 2021-11-09 | 2021-11-09 | Growth method of cadmium telluride crystal |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05270995A (en) * | 1992-03-27 | 1993-10-19 | Ngk Insulators Ltd | Production of cadmium-tellurium based single crystal |
| CN101210346A (en) * | 2006-12-30 | 2008-07-02 | 袁诗鑫 | Horizontal zone melting method for growing tellurium zinc cadmium single-crystal |
| CN103114335A (en) * | 2011-11-17 | 2013-05-22 | 通用电气公司 | Method for producing cadmium telluride or cadmium zinc telluride single crystal |
| CN112680781A (en) * | 2020-12-09 | 2021-04-20 | 清远先导材料有限公司 | Cadmium telluride crystal growth device and growth method thereof |
| CN114032609A (en) * | 2021-10-27 | 2022-02-11 | 安徽光智科技有限公司 | Growth method of cadmium telluride crystal |
-
2021
- 2021-11-09 CN CN202111323511.3A patent/CN114059170A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05270995A (en) * | 1992-03-27 | 1993-10-19 | Ngk Insulators Ltd | Production of cadmium-tellurium based single crystal |
| CN101210346A (en) * | 2006-12-30 | 2008-07-02 | 袁诗鑫 | Horizontal zone melting method for growing tellurium zinc cadmium single-crystal |
| CN103114335A (en) * | 2011-11-17 | 2013-05-22 | 通用电气公司 | Method for producing cadmium telluride or cadmium zinc telluride single crystal |
| CN112680781A (en) * | 2020-12-09 | 2021-04-20 | 清远先导材料有限公司 | Cadmium telluride crystal growth device and growth method thereof |
| CN114032609A (en) * | 2021-10-27 | 2022-02-11 | 安徽光智科技有限公司 | Growth method of cadmium telluride crystal |
Non-Patent Citations (2)
| Title |
|---|
| 徐亚东: "大尺寸Cd1-xZnxTe晶体籽晶垂直布里奇曼法生长技术与性能表征", 中国优秀博硕士学位论文全文数据库 (硕士)信息科技辑, no. 6, pages 135 - 91 * |
| 金敏: "Te自助溶剂定向凝固法生长CdTe晶体", 应用技术学报, vol. 20, no. 3, pages 205 - 210 * |
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