CN115353082B - Method for sintering high-quality aluminum nitride raw material in one step - Google Patents
Method for sintering high-quality aluminum nitride raw material in one step Download PDFInfo
- Publication number
- CN115353082B CN115353082B CN202211039523.8A CN202211039523A CN115353082B CN 115353082 B CN115353082 B CN 115353082B CN 202211039523 A CN202211039523 A CN 202211039523A CN 115353082 B CN115353082 B CN 115353082B
- Authority
- CN
- China
- Prior art keywords
- sintering
- aluminum nitride
- raw material
- crucible
- raw materials
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002994 raw material Substances 0.000 title claims abstract description 69
- 238000005245 sintering Methods 0.000 title claims abstract description 60
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000013078 crystal Substances 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 10
- 229910052721 tungsten Inorganic materials 0.000 claims description 10
- 239000010937 tungsten Substances 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 238000000746 purification Methods 0.000 abstract description 6
- 238000007796 conventional method Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0728—After-treatment, e.g. grinding, purification
-
- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/007—Apparatus for preparing, pre-treating the source material to be used for crystal growth
Abstract
The invention belongs to the technical field of aluminum nitride raw material treatment, and particularly relates to a method for sintering a high-quality aluminum nitride raw material in one step, which comprises the following steps: taking aluminum nitride powder raw materials and placing the aluminum nitride powder raw materials into a crucible; placing the whole crucible in a furnace body, vacuumizing and filling sintering gas; gradient sintering; cooling the furnace body and taking out the crucible. The invention adopts a gradient sintering method, and sinters different time steps at different temperatures to achieve the purpose of generating high-quality aluminum nitride raw materials by one-time sintering. The method improves the efficiency of raw material treatment to a great extent, and reduces the material cost and labor cost of the baked materials. The raw materials sintered by the one-step method have obvious crystal form characteristics, can be directly used for the subsequent crystal growth of AlN, and compared with the conventional method, the method has the advantages that repeated sintering is not needed, and the sintering and purification of the raw materials can be realized quickly and efficiently.
Description
Technical Field
The invention belongs to the technical field of aluminum nitride raw material treatment, and particularly relates to a method for sintering high-quality aluminum nitride raw materials in one step.
Background
AlN (aluminum nitride) crystal materials are gradually concerned by the excellent physical properties of large forbidden bandwidth (6.2 eV), high thermal conductivity (3.2 W.cm-1K-1), high resistivity, high surface acoustic velocity (5600-6000 m/s) and the like, but mature AlN power electronic devices are difficult to see on the market at present, mainly because the growth difficulty of AlN single crystal materials is extremely high, the growth condition is quite severe, the AlN crystal growth is generally realized under the condition of the temperature above 2000 ℃ and the extremely high pressure, so that the AlN bulk crystal experiment is carried out by adopting a physical vapor transmission method (PVT), the AlN raw materials are sublimated in a high-temperature area below a crucible mainly through an induction heating method, and then the AlN crystal growth is carried out through controlling the pressure transmission to a low-temperature growth area, and the high-temperature high-pressure state inside a furnace body and the directional gas transportation can be effectively ensured in the whole process. The steps of determining the quality of the crystal mainly comprise raw material purification, gas phase transmission, seed crystal induction, thermal field optimization and the like, and the raw material purification is a very difficult point in the AlN growing process at present, and the quality of the ingot depends on the quality of the raw material to a great extent, so that the processing of the raw material is a critical ring in the AlN crystal growing process.
The prior known AlN raw material treatment method generally needs repeated sintering for a plurality of times, the primary sintering is heated to 1000 ℃ to remove H in the raw material 2 O, forming a primary sintered body, then heating to 1800 ℃, removing carbon and oxygen impurities in the raw materials, forming a yellowish secondary sintered body by the raw materials, and then heating to 2100-2250 ℃ to form a crystalline state for growth. Generally, the raw materials must be purified and sintered at least three times through the above three temperature points, and if the sintering effect of each temperature point is not ideal, the sintering may need to be repeated, so that a batch of crystalline raw materials capable of being used for growth is successfully processed, the period is 3-6 furnaces, the time period is approximately 7-14 days, the time period is quite long, and in a laboratory with limited furnace body resources, the improvement of the efficiency of the sintering is necessary.
Therefore, how to improve the efficiency of AlN firing is a problem to be solved in the current AlN bulk crystal growth.
Disclosure of Invention
Aiming at the problems of complicated sintering steps and overlong sintering period of powder for AlN crystal growth in the prior art, the invention provides a crystal raw material purification method for sintering high-quality aluminum nitride in one step. The invention directly sinters the low impurity raw material with crystalline state in one step by simplifying the material sintering step and adopting a gradient heating method, the raw material sintered by adopting the method has low impurity content and crystalline state, shortens the material sintering period from the previous 7-14 days to 3-5 days, and can greatly improve the AlN raw material purification efficiency.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a method for sintering a high quality aluminum nitride raw material in one step, comprising the steps of:
s1: 500g of AlN powder raw material is taken and filled in a special crucible for firing, sealing is ensured above the crucible, and a tungsten plate for depositing powder is arranged;
s2: placing the whole crucible in a furnace body, vacuumizing, and filling nitrogen, wherein the pressure of the nitrogen reaches more than 1 atmosphere;
s3: gradient sintering, namely heating to 2050-2100 ℃, preserving heat for 18-22 hours, heating to 2220-2250 ℃, preserving heat for 24 hours, slowly pumping and pressing the inside of the crucible to the growth pressure, and preserving heat for 24 hours;
s4: cooling the furnace body, and taking out the crucible to obtain the high-quality aluminum nitride raw material.
In step S1, the raw materials are preferably not excessive, which may otherwise lead to non-uniform sintering.
In accordance with the preferred embodiment of the invention, in step S1, the crucible must be sealed, and during sintering, a large amount of aluminum vapor will be present, and the tungsten plate will be placed to assist in the deposition of the aluminum vapor.
In step S2, the initial sintering pressure is preferably maintained at about 1 to 1.5 atmospheres.
According to a preferred embodiment of the invention, in step S2, the sintering atmosphere used is nitrogen.
According to the invention, in the step S3, 3 sections of sintering technology are adopted, and the temperature is directly raised without disassembling the furnace between each two sections of technology.
According to a preferred embodiment of the invention, in step S3, the sintering process is initially carried out at 2050-2100 ℃ and the solidification of the powder material is carried out at 1 atmosphere.
In step S3, after the sintering is completed at 2050-2100 ℃, the temperature is raised to 2220-2250 ℃ and the sintering is performed for 24 hours.
According to the invention, in the step S3, after high-temperature sintering, slow pumping is performed, pumping is performed to the growth pressure, and gaseous aluminum vapor is sublimated and deposited on the tungsten plate above.
According to the invention, the method is preferably suitable for the treatment of raw materials in the early stage of AlN growth by a resistance method and an induction method.
According to the invention, the AlN raw material treated by the method has obvious lattice shape on the surface, and can be directly used for crystal growth.
The invention adopts a gradient sintering method, and sinters different time steps at different temperatures to achieve the purpose of generating high-quality aluminum nitride raw materials by one-time sintering. The method improves the efficiency of raw material treatment to a great extent, and reduces the material cost and labor cost of the baked materials. The raw materials sintered by the one-step method have obvious crystal form characteristics, can be directly used for the subsequent crystal growth of AlN, and compared with the conventional method, the method has the advantages that repeated sintering is not needed, and the sintering and purification of the raw materials can be realized quickly and efficiently.
Advantageous effects
The invention discloses a method for sintering high-quality aluminum nitride raw materials in one step, which adopts a method for carrying out gradient heating and then carrying out pumping pressure induced growth on the raw materials, and a high-quality raw material with low impurity content and crystalline state is formed on an upper tungsten sheet and a lower material surface. According to the AlN sintering method, the sintering efficiency is improved according to the sintering condition, the sintering period and the sintering time are shortened, and the time cost and the experiment cost are reduced. Secondly, the utilization rate is higher, and the common method can not take out the raw materials deposited on the side wall of the crucible due to repeated temperature rise and reduction, so that the utilization rate can only reach about 2/3, and the AlN raw materials sintered by the method can not deposit the raw materials on the side wall of the crucible due to the fact that the AlN raw materials are directly heated to high temperature, so that the utilization rate of the raw materials can be improved to a great extent, and is close to more than 90%. The method provided by the invention can basically judge that the burned crystal raw material with a crystal form can be directly used for the growth of an AlN ingot because the burned crystal raw material stays in a high-temperature area for a long time.
Drawings
Fig. 1 shows AlN material before sintering.
Fig. 2 is an AlN source deposited on an upper tungsten plate.
Fig. 3 shows AlN material after sintering in a lower one-step process.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description, it is to be understood that the terms used in this specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description set forth herein is merely a preferred example for the purpose of illustration and is not intended to limit the scope of the invention, so that it should be understood that other equivalents or modifications may be made thereto without departing from the spirit and scope of the invention.
The following examples are merely illustrative of embodiments of the present invention and are not intended to limit the invention in any way, and those skilled in the art will appreciate that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
In the embodiment, the AlN raw material is white powder initially, the particle size is about um level, the porosity is small, and the environment of a furnace body is a W-graphite system.
Example 1
A method for sintering a high quality aluminum nitride raw material in one step, comprising the steps of:
s1, 500g of AlN powder raw material is taken and put into a special crucible for firing, sealing is ensured above the crucible, and a tungsten plate for depositing powder is arranged;
s2, placing the whole crucible in a furnace body, vacuumizing, and then filling nitrogen, wherein the pressure of the nitrogen reaches more than 1 atmosphere;
s3, gradient sintering, namely firstly heating to 2050-2100 ℃, preserving heat for 18-22 hours, then heating to 2220-2250 ℃, preserving heat for 24 hours, then slowly pumping the interior of the crucible to the growth pressure, and preserving heat for 24 hours;
s4: cooling the furnace body, and taking out the crucible to obtain the high-quality aluminum nitride raw material.
The invention adopts a gradient heating method, and then the raw materials are subjected to pumping pressure induced growth, so that a high-quality raw material with low impurity content and crystalline state is formed on the upper tungsten sheet and the lower material surface.
FIG. 1 shows AlN powder in an initial state, which is a powder material with higher density, and the sintered material has formed into a crystalline state after gradient temperature rise by a one-step method.
Fig. 2 shows an AlN feedstock deposited on an upper tungsten plate, and it can be seen that after pumping, the thickness of the upper deposited layer has reached about 20mm, and the quality of the feedstock for growth may be better due to the primary crystals that have been grown.
Fig. 3 shows the sintered shape of the bottom material, it can be seen that the level of the material has small grains formed and that the whole material exhibits a crystalline state, which can be used directly for crystal growth.
According to the sintering condition, the method for sintering the high-quality aluminum nitride raw material in one step firstly improves the material sintering efficiency, shortens the material sintering period and the material sintering time, and reduces the time cost and the experiment cost. Secondly, the utilization rate is higher, and the common method can not take out the raw materials deposited on the side wall of the crucible due to repeated temperature rise and reduction, so that the utilization rate can only reach about 2/3, and the AlN raw materials sintered by the method can not deposit the raw materials on the side wall of the crucible due to the fact that the AlN raw materials are directly heated to high temperature, so that the utilization rate of the raw materials can be improved to a great extent, and is close to more than 90%. The method provided by the invention can basically judge that the burned crystal raw material with a crystal form can be directly used for the growth of an AlN ingot because the burned crystal raw material stays in a high-temperature area for a long time.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be apparent to one skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (4)
1. A method for sintering a high quality aluminum nitride raw material in one step, comprising the steps of:
s1: the method comprises the steps of (1) loading aluminum nitride powder raw materials into a crucible, ensuring sealing above the crucible, and placing a tungsten plate for depositing powder;
s2: placing the whole crucible in a furnace body, vacuumizing, and filling sintering atmosphere, wherein the used sintering atmosphere is nitrogen, and the pressure of the sintering atmosphere is more than 1 atmosphere;
s3: gradient sintering, namely heating to 2050-2100 ℃, preserving heat for 18-22 hours, and solidifying the powder material under 1 atmosphere; heating to 2220-2250 deg.C, and keeping the temperature for 24 hours; slowly pumping and pressing the inside of the crucible to the growth pressure, and preserving the heat for 24 hours to enable gaseous aluminum vapor to sublimate and deposit on the tungsten plate above; the sintering process adopts 3 sections, and the furnace is not required to be disassembled between each two sections of the process, so that the temperature is directly raised;
s4: cooling the furnace body, and taking out the crucible to obtain the high-quality aluminum nitride raw material.
2. The method for one-step sintering of high quality aluminum nitride raw material according to claim 1, wherein in step S2, the initial sintering pressure is maintained at 1 to 1.5 atmospheres.
3. The method for sintering a high quality aluminum nitride raw material according to claim 1, wherein the method is suitable for raw material treatment in a pre-growth stage of aluminum nitride by a resistance method and an induction method.
4. The method for sintering a high quality aluminum nitride raw material according to claim 1, wherein the surface of the aluminum nitride raw material treated by the method has a remarkable lattice shape, and can be directly used for crystal growth.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211039523.8A CN115353082B (en) | 2022-08-29 | 2022-08-29 | Method for sintering high-quality aluminum nitride raw material in one step |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211039523.8A CN115353082B (en) | 2022-08-29 | 2022-08-29 | Method for sintering high-quality aluminum nitride raw material in one step |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115353082A CN115353082A (en) | 2022-11-18 |
| CN115353082B true CN115353082B (en) | 2023-10-24 |
Family
ID=84003809
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211039523.8A Active CN115353082B (en) | 2022-08-29 | 2022-08-29 | Method for sintering high-quality aluminum nitride raw material in one step |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115353082B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116143085A (en) * | 2022-12-26 | 2023-05-23 | 奥趋光电技术(杭州)有限公司 | Preparation method of high-purity aluminum nitride raw material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103643295A (en) * | 2013-12-04 | 2014-03-19 | 北京华进创威电子有限公司 | Method for preparing raw material for vapor-method aluminum nitride crystal growth |
| CN106757322A (en) * | 2016-12-22 | 2017-05-31 | 苏州奥趋光电技术有限公司 | A kind of aln raw material high temperature purification method |
| CN109576783A (en) * | 2019-01-23 | 2019-04-05 | 山东大学 | A kind of preprocessing method of raw materials for high quality aluminum nitride crystal growth |
| CN110015648A (en) * | 2019-03-28 | 2019-07-16 | 北京中材人工晶体研究院有限公司 | A kind of high-purity aluminium nitride powder and aluminium nitride powder method of purification |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2628598B2 (en) * | 1988-03-04 | 1997-07-09 | 富士通株式会社 | Manufacturing method of aluminum nitride sintered body |
-
2022
- 2022-08-29 CN CN202211039523.8A patent/CN115353082B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103643295A (en) * | 2013-12-04 | 2014-03-19 | 北京华进创威电子有限公司 | Method for preparing raw material for vapor-method aluminum nitride crystal growth |
| CN106757322A (en) * | 2016-12-22 | 2017-05-31 | 苏州奥趋光电技术有限公司 | A kind of aln raw material high temperature purification method |
| CN109576783A (en) * | 2019-01-23 | 2019-04-05 | 山东大学 | A kind of preprocessing method of raw materials for high quality aluminum nitride crystal growth |
| CN110015648A (en) * | 2019-03-28 | 2019-07-16 | 北京中材人工晶体研究院有限公司 | A kind of high-purity aluminium nitride powder and aluminium nitride powder method of purification |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115353082A (en) | 2022-11-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR20230113829A (en) | SiC CRUCIBLE, SiC SINTERED BODY, AND METHOD OF PRODUCING SiC SINGLE CRYSTAL | |
| CN110592673B (en) | High-quality large-size silicon carbide crystal growth method | |
| KR101760030B1 (en) | The method of Variable scale SiC ingot growth using large scale SiC ingot growing apparatus | |
| CN104357913A (en) | High-temperature annealing treatment method for silicon carbide crystal | |
| JPS6357400B2 (en) | ||
| CN115353082B (en) | Method for sintering high-quality aluminum nitride raw material in one step | |
| CN108624963A (en) | A kind of raw material sintering process of carborundum crystals for the growth of PVT methods | |
| CN112553694A (en) | Method and device for high-temperature annealing of silicon carbide single crystal | |
| JPS5935099A (en) | Method for growing silicon carbide crystal | |
| CN108103575A (en) | A kind of preparation method and its device of low stress single-crystal silicon carbide | |
| CN109183143B (en) | Method for improving AlN single crystal purity by using reducing gas | |
| JP6910168B2 (en) | Silicon Carbide Single Crystal Ingot Manufacturing Equipment and Manufacturing Method | |
| CN116200819A (en) | SiC seed crystal carbonization process | |
| CN108130592B (en) | A kind of preparation method of high-purity semi-insulating silicon carbide monocrystalline | |
| JP6829767B2 (en) | Manufacturing method and manufacturing equipment for SiC raw materials for SiC crystal growth | |
| CN113215655B (en) | Filling method for increasing volatilization amount of bulk material in growth of aluminum nitride single crystal | |
| CN109112634B (en) | Crucible equipment and method for preparing aluminum nitride crystal | |
| JP3970789B2 (en) | Nitride single crystal manufacturing method and manufacturing apparatus thereof | |
| JP2000053493A (en) | Production of single crystal and single crystal production device | |
| JP2004284870A (en) | Method for manufacturing nitride single crystal and manufacturing apparatus therefor | |
| CN214244670U (en) | Crystal growth furnace structure | |
| CN114686970B (en) | Dopant, preparation method thereof and crystal form controllable semi-insulating silicon carbide crystal growth method | |
| CN214327973U (en) | High-temperature annealing device for silicon carbide single crystal | |
| CN116536758B (en) | Equipment and method for epitaxial growth of gallium nitride crystal by high-pressure fluxing agent | |
| CN113215660B (en) | Silicon carbide single crystal growth method capable of reducing heater loss |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |