CN108275664B - High-temperature sintering purification method for aluminum nitride - Google Patents
High-temperature sintering purification method for aluminum nitride Download PDFInfo
- Publication number
- CN108275664B CN108275664B CN201711481757.7A CN201711481757A CN108275664B CN 108275664 B CN108275664 B CN 108275664B CN 201711481757 A CN201711481757 A CN 201711481757A CN 108275664 B CN108275664 B CN 108275664B
- Authority
- CN
- China
- Prior art keywords
- aluminum nitride
- temperature
- furnace body
- purity nitrogen
- keeping
- 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
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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
-
- 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/89—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by mass-spectroscopy
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a high-temperature sintering purification method for aluminum nitride, which can effectively remove impurities in the aluminum nitride powder through multi-stage heating and heat preservation for many times, and can further reduce the impurities in the aluminum nitride powder through multi-stage sintering; in the heating and heat preservation process, flowing high-purity nitrogen is introduced, so that impurities in the aluminum nitride powder can be efficiently taken away; impurities can be removed more efficiently by increasing the sintering temperature to the crystal growth temperature; and (3) crushing and fine screening the obtained aluminum nitride polycrystal with uneven surface, sintering at high temperature again to remove impurities, and controlling the temperature to be below the crystal growth temperature to obtain an aluminum nitride sintered body with low impurity content, smooth surface and regular shape.
Description
Technical Field
The invention relates to the technical field of growth of aluminum nitride single crystal materials, in particular to a high-temperature sintering purification method for aluminum nitride.
Background
Aluminum nitride (AlN) is one of the third generation wide bandgap semiconductor materials, has excellent properties such as wide bandgap, high melting point, high critical breakdown field strength, high temperature thermal stability, and chemical corrosion resistance, and is mainly applied to devices such as Light Emitting Diodes (LEDs), Laser Diodes (LDs), second harmonic emitters, and surface acoustic waves. AlN crystal is a typical direct bandgap semiconductor, and the theoretical forbidden bandwidth Eg =6.2eV of AlN crystal at normal temperature. Because the AlN crystal has a band gap of 6.2eV, the AlN crystal with high crystallization quality theoretically has very high transmittance in an ultraviolet band, is an ideal substrate material of an LED or LD device with ultra-short wavelength (200-270nm), and at present, the transmittance band of the AlN crystal can reach 200nm at an ultraviolet end.
The theoretical calculated melting point of the material is 2800 ℃ and the decompression pressure is 20MPa, so that the crystal growth is difficult to carry out by adopting the melt Czochralski method or the temperature gradient solidification method. The AlN single crystal was grown by a physical vapor transport method (PVT) in the same manner as the SiC single crystal. The AlN powder used for growing the AlN single crystal by adopting the PVT method contains high-concentration impurities such as oxygen, carbon and the like, and the impurities can seriously influence the nucleation, two-dimensional growth and crystal quality of the AlN single crystal in the growth process, so the AlN raw material must be firstly purified at high temperature before the crystal grows, the impurities such as oxygen, carbon and the like in the AlN raw material are fully removed, and the purity of the raw material is improved.
In order to prevent aluminum nitride from crystallizing in the high-temperature purification process, the purification temperature of the aluminum nitride raw material is controlled below the crystallization temperature, and the higher the temperature is, the higher the impurity removal efficiency is.
Disclosure of Invention
The invention aims to provide a high-temperature sintering purification method for aluminum nitride, which can sinter and obtain an aluminum nitride sintered body with low impurity content.
In order to achieve the purpose, the invention adopts the technical scheme that:
a high-temperature sintering purification method for aluminum nitride comprises the steps (a) and (b) which are sequentially carried out; wherein step (a) is performed at least once in a cycle, and all are performed before step (b);
step (a):
(1) putting aluminum nitride powder into an open crucible, placing the open crucible into a furnace body, and vacuumizing the furnace body;
(2) heating the open crucible to make the temperature of the aluminum nitride powder reach 900-1200 ℃, keeping the temperature for 4-8h, and carrying away part of impurities through the following reaction:
2Al(OH)3=Al2O3+3H2O(g)；
2Al(OOH)=Al2O3+H2O(g)；
aluminum nitride powder is sintered in the open crucible to an aluminum nitride sintered body;
(3) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to enable the temperature of the aluminum nitride sintered body to reach 1400-1600 ℃, keeping the temperature for 4-8h, and carrying away part of impurities through the following reactions:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by reaction out of the furnace body;
(4) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to enable the temperature of the aluminum nitride sintered body to reach 2000-2300 ℃, keeping the temperature for 6-10h, and carrying away part of impurities through the following reactions:
Al2O3+4Al(g)=3Al2O(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by reaction out of the furnace body;
(5) cooling the open crucible to reduce the temperature of the aluminum nitride sintered body to 100 ℃;
(6) cooling the aluminum nitride sintered body to room temperature, taking out and crushing the aluminum nitride sintered body, and meanwhile, carrying out fine screening to obtain aluminum nitride powder;
step (b):
(7) placing the aluminum nitride powder obtained after fine screening into the open crucible, and placing the open crucible into the furnace body;
(8) heating the open crucible to make the temperature of the aluminum nitride powder reach 900-1200 ℃, keeping the temperature for 2-4h, and carrying away part of impurities through the following reaction:
2Al(OH)3=Al2O3+3H2O(g)；
2Al(OOH)=Al2O3+H2O(g)；
aluminum nitride powder is sintered in the open crucible to an aluminum nitride sintered body;
(9) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to enable the temperature of the aluminum nitride sintered body to reach 1400-1600 ℃, keeping the temperature for 2-4h, and carrying away part of impurities through the following reactions:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by reaction out of the furnace body;
(10) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to enable the temperature of the aluminum nitride sintered body to reach 1800-2000 ℃, keeping the temperature for 4-8h, and carrying away part of impurities through the following reactions:
Al2O3+4Al(g)=3Al2O(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by reaction out of the furnace body.
Preferably, in the step (6), the crushed aluminum nitride sintered body is finely sieved through a 50-mesh sieve, a 100-mesh sieve, a 200-mesh sieve and a 500-mesh sieve in this order to obtain the aluminum nitride powder.
Preferably, in step (5), the cooling rate is 5-10 ℃/min.
Preferably, in the step (3), high-purity nitrogen gas of 60 to 80kPa is introduced into the furnace body.
Preferably, in the step (4), high-purity nitrogen gas of 60 to 80kPa is introduced into the furnace body.
Preferably, in the step (9), high-purity nitrogen gas of 60 to 80kPa is introduced into the furnace body.
Preferably, in the step (10), high-purity nitrogen gas of 60 to 80kPa is introduced into the furnace body.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: according to the high-temperature sintering purification method for aluminum nitride, impurities in the aluminum nitride powder can be effectively removed through multi-section heating and heat preservation, and the impurities in the aluminum nitride powder can be further reduced through multiple times of sintering; impurities can be removed more efficiently by increasing the sintering temperature to the crystal growth temperature; and (3) crushing and fine screening the obtained aluminum nitride polycrystal with uneven surface, sintering at high temperature again to remove impurities, and controlling the temperature to be below the crystal growth temperature to obtain an aluminum nitride sintered body with low impurity content, smooth surface and regular shape.
Detailed Description
The technical solution of the present invention is further illustrated below with reference to specific examples.
In the above-mentioned high-temperature sintering purification method for aluminum nitride, which is used for sintering the aluminum nitride powder containing a trace amount of impurities, the purity of the aluminum nitride powder is 99% in this embodiment. During the production and storage of aluminum nitride, aluminum nitride reacts with water and oxygen in the air to produce AlOOH and Al (OH)3、Al2O3And the like, and brings impurity elements such as hydrogen, oxygen, carbon and the like.
In the production process of the aluminum nitride powder:
Al2O3(s)+3C(s)+N2(g)→2AlN(s)+3CO(g)；
the reaction results in the production of aluminum nitride powder containing C impurities and Al2O3Impurities.
Reaction of aluminum nitride powder in air:
AlN(s)+2H2O(g)→AlOOH(s)+NH3（g）；
AlN(s)+3H2O(g)→Al(OH)3(s)+NH3（g）；
AlN(s)+O2(g)→Al2O3(s)+N2（g）；
the reaction results in aluminum nitride powder containing AlOOH impurity Al (OH)3Impurities, Al2O3Impurities.
The following is a specific example of a high-temperature purification method of an aluminum nitride raw material, which comprises the steps (a) and (b) performed in this order; wherein step (a) is performed at least once in a cycle, and all are performed before step (b); in this example, step (a) is performed only once.
Step (a):
(1) putting aluminum nitride powder into an open crucible, placing the open crucible into a furnace body, and vacuumizing the furnace body;
(2) heating the open crucible to make the temperature of the aluminum nitride powder reach 900-:
2Al(OH)3=Al2O3+3H2O(g)；
2Al(OOH)=Al2O3+H2O(g)；
aluminum nitride powder is sintered in an open crucible to an aluminum nitride sintered body; in this example, the open crucible was heated to 1000 ℃ and held for 6 hours;
(3) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to ensure that the temperature of the aluminum nitride sintered body reaches 1400-1600 ℃, and keeping the temperature for 4-8h, and carrying away part of impurities through the following reactions:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by the reaction out of the furnace body; in the embodiment, high-purity nitrogen gas with the pressure of 60-80kPa is introduced into the furnace body; heating the open crucible to enable the temperature of the aluminum nitride sintered body to reach 1500 ℃, and keeping for 6 hours;
(4) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to ensure that the temperature of the aluminum nitride sintered body reaches 2000-2300 ℃, keeping the temperature for 6-10h, and carrying away part of impurities through the following reactions:
Al2O3+4Al(g)=3Al2O(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by the reaction out of the furnace body; in the embodiment, high-purity nitrogen gas with the pressure of 60-80kPa is introduced into the furnace body; heating the open crucible to enable the temperature of the aluminum nitride sintered body to reach 2200 ℃ and keeping for 8 hours;
in the step (4), because the heating temperature reaches the crystal growth temperature of the aluminum nitride, although the temperature is high, the impurity removal rate is high and the impurity removal effect is good, the surface of the obtained aluminum nitride polycrystal is uneven and cannot be used for single crystal growth;
(5) cooling the open crucible to reduce the temperature of the aluminum nitride sintered body to 100 ℃; in this embodiment, the cooling rate is 5-10 ℃/min;
(6) cooling the aluminum nitride sintered body to room temperature, taking out and crushing the aluminum nitride sintered body, and meanwhile, carrying out fine screening to obtain aluminum nitride powder; in the embodiment, the aluminum nitride sintered body cooled to room temperature is wrapped by a high-purity aluminum foil in a multi-layer manner, and the wrapped aluminum nitride sintered body is placed in a groove of a high-hardness punching machine to be punched and crushed;
finely sieving the crushed aluminum nitride sintered body by a sieve of 50 meshes, a sieve of 100 meshes, a sieve of 200 meshes and a sieve of 500 meshes in sequence to obtain aluminum nitride powder; the diameter of the aluminum nitride powder screened by the screen is less than 25um, and aluminum foil impurities are filtered by the screen, so that the high purity of the aluminum nitride powder is ensured; the screening of the aluminum nitride powder is carried out in a glove box, and high-purity nitrogen is introduced into the glove box, so that the aluminum nitride powder can be prevented from reacting with water vapor and oxygen in the air, and carbon, oxygen and hydrogen impurities are prevented from being introduced;
step (b):
(7) placing the aluminum nitride powder obtained after fine screening into an open crucible, and placing the open crucible into a furnace body;
(8) heating the open crucible to make the temperature of the aluminum nitride powder reach 900-:
2Al(OH)3=Al2O3+3H2O(g)；
2Al(OOH)=Al2O3+H2O(g)；
aluminum nitride powder is sintered in an open crucible to an aluminum nitride sintered body; in this example, the open crucible was heated to bring the aluminum nitride powder to 1000 ℃ and held for 2 hours;
(9) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to ensure that the temperature of the aluminum nitride sintered body reaches 1400-1600 ℃, and keeping for 2-4h, and carrying away part of impurities through the following reactions:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by the reaction out of the furnace body; in the embodiment, high-purity nitrogen gas with the pressure of 60-80kPa is introduced into the furnace body; heating the open crucible to make the temperature of the aluminum nitride powder reach 1500 ℃, and keeping for 2 h;
(10) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to ensure that the temperature of the aluminum nitride sintered body reaches 1800-2000 ℃, keeping the temperature for 4-8h, and carrying away part of impurities through the following reactions:
Al2O3+4Al(g)=3Al2O(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by the reaction out of the furnace body; in the embodiment, high-purity nitrogen gas with the pressure of 60-80kPa is introduced into the furnace body; the open crucible was heated to bring the aluminum nitride powder to 1900 ℃ and held for 4 hours.
Since the temperature in the step (10) does not reach the crystal growth temperature of the aluminum nitride, the surface of the aluminum nitride sintered body is flat after the step (10) is finished, and the crystal growth requirement can be met.
By the method, the aluminum nitride sintered body with low impurity content, flat surface and regular shape can be obtained.
In this example, two (three each) high-temperature sinters gave an aluminum nitride sintered body having an oxygen content of 150ppm and a carbon content of 100ppm as measured by Glow Discharge Mass Spectrometry (GDMS), which was a high-purity aluminum nitride sintered body. According to actual needs, the sintering times are properly increased to achieve the required purity.
The above-mentioned embodiments are merely illustrative of the technical idea and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered in the scope of the present invention.
Claims (7)
1. A high-temperature sintering purification method for aluminum nitride is characterized by comprising the following steps: comprises the steps (a) and (b) which are carried out in sequence; wherein step (a) is performed at least once in a cycle, and all are performed before step (b);
step (a):
(1) putting aluminum nitride powder into an open crucible, placing the open crucible into a furnace body, and vacuumizing the furnace body;
(2) heating the open crucible to make the temperature of the aluminum nitride powder reach 900-1200 ℃, keeping the temperature for 4-8h, and carrying away part of impurities through the following reaction:
2Al(OH)3=Al2O3+3H2O(g)；
2Al(OOH)=Al2O3+H2O(g)；
aluminum nitride powder is sintered in the open crucible to an aluminum nitride sintered body;
(3) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to enable the temperature of the aluminum nitride sintered body to reach 1400-1600 ℃, keeping the temperature for 4-8h, and carrying away part of impurities through the following reactions:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by reaction out of the furnace body;
(4) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to enable the temperature of the aluminum nitride sintered body to reach 2000-2300 ℃, keeping the temperature for 6-10h, and carrying away part of impurities through the following reactions:
Al2O3+4Al(g)=3Al2O(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by reaction out of the furnace body;
(5) cooling the open crucible to reduce the temperature of the aluminum nitride sintered body to 100 ℃;
(6) cooling the aluminum nitride sintered body to room temperature, taking out and crushing the aluminum nitride sintered body, and meanwhile, carrying out fine screening to obtain aluminum nitride powder;
step (b):
(7) placing the aluminum nitride powder obtained after fine screening into the open crucible, and placing the open crucible into the furnace body;
(8) heating the open crucible to make the temperature of the aluminum nitride powder reach 900-1200 ℃, keeping the temperature for 2-4h, and carrying away part of impurities through the following reaction:
2Al(OH)3=Al2O3+3H2O(g)；
2Al(OOH)=Al2O3+H2O(g)；
aluminum nitride powder is sintered in the open crucible to an aluminum nitride sintered body;
(9) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to enable the temperature of the aluminum nitride sintered body to reach 1400-1600 ℃, keeping the temperature for 2-4h, and carrying away part of impurities through the following reactions:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by reaction out of the furnace body;
(10) introducing high-purity nitrogen with the pressure of 50-90kPa into the furnace body, simultaneously heating the open crucible to enable the temperature of the aluminum nitride sintered body to reach 1800-2000 ℃, keeping the temperature for 4-8h, and carrying away part of impurities through the following reactions:
Al2O3+4Al(g)=3Al2O(g)；
keeping the circulation state of high-purity nitrogen in the furnace body, and taking impurity gas generated by reaction out of the furnace body.
2. The high-temperature sintering purification method for aluminum nitride according to claim 1, characterized in that: in the step (6), the aluminum nitride sintered body after pulverization was finely sieved through a 50-mesh sieve, a 100-mesh sieve, a 200-mesh sieve and a 500-mesh sieve in this order to obtain an aluminum nitride powder.
3. The high-temperature sintering purification method for aluminum nitride according to claim 1, characterized in that: in the step (5), the cooling rate is 5-10 ℃/min.
4. The high-temperature sintering purification method for aluminum nitride according to claim 1, characterized in that: in the step (3), high-purity nitrogen gas with the pressure of 60-80kPa is introduced into the furnace body.
5. The high-temperature sintering purification method for aluminum nitride according to claim 1, characterized in that: in the step (4), high-purity nitrogen gas with the pressure of 60-80kPa is introduced into the furnace body.
6. The high-temperature sintering purification method for aluminum nitride according to claim 1, characterized in that: in the step (9), high-purity nitrogen gas with the pressure of 60-80kPa is introduced into the furnace body.
7. The high-temperature sintering purification method for aluminum nitride according to claim 1, characterized in that: in the step (10), high-purity nitrogen gas of 60-80kPa is introduced into the furnace body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711481757.7A CN108275664B (en) | 2017-12-29 | 2017-12-29 | High-temperature sintering purification method for aluminum nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711481757.7A CN108275664B (en) | 2017-12-29 | 2017-12-29 | High-temperature sintering purification method for aluminum nitride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108275664A CN108275664A (en) | 2018-07-13 |
| CN108275664B true CN108275664B (en) | 2021-12-07 |
Family
ID=62802782
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711481757.7A Active CN108275664B (en) | 2017-12-29 | 2017-12-29 | High-temperature sintering purification method for aluminum nitride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108275664B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110015648B (en) * | 2019-03-28 | 2021-05-04 | 中材人工晶体研究院有限公司 | High-purity aluminum nitride powder and aluminum nitride powder purification method |
| CN113789573A (en) * | 2021-11-16 | 2021-12-14 | 山西中科潞安紫外光电科技有限公司 | Method for preparing AlN crystal by spontaneous nucleation through PVT method |
| CN114873570B (en) * | 2022-07-11 | 2022-09-27 | 山西中科潞安半导体技术研究院有限公司 | Method and device for purifying aluminum nitride powder by adopting PVT (polyvinyl dichloride) method |
| 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 |
|---|---|---|---|---|
| US4172754A (en) * | 1978-07-17 | 1979-10-30 | National Research Development Corporation | Synthesis of aluminum nitride |
| JP2006315940A (en) * | 2005-04-13 | 2006-11-24 | Sumitomo Electric Ind Ltd | METHOD FOR GROWING AlN SINGLE CRYSTAL AND AlN SINGLE CRYSTAL |
| CN106395770A (en) * | 2016-06-30 | 2017-02-15 | 北京华进创威电子有限公司 | A purifying device and a purifying method for an aluminium nitride raw material |
| 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 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6770135B2 (en) * | 2001-12-24 | 2004-08-03 | Crystal Is, Inc. | Method and apparatus for producing large, single-crystals of aluminum nitride |
| CN106498491B (en) * | 2016-11-02 | 2018-12-14 | 中国电子科技集团公司第四十六研究所 | A kind of purifying plant and its method of purification of vapor phase method crystal growth raw material |
| CN106637411B (en) * | 2016-12-22 | 2019-04-05 | 苏州奥趋光电技术有限公司 | A kind of aluminum-nitride single crystal growing method |
-
2017
- 2017-12-29 CN CN201711481757.7A patent/CN108275664B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4172754A (en) * | 1978-07-17 | 1979-10-30 | National Research Development Corporation | Synthesis of aluminum nitride |
| JP2006315940A (en) * | 2005-04-13 | 2006-11-24 | Sumitomo Electric Ind Ltd | METHOD FOR GROWING AlN SINGLE CRYSTAL AND AlN SINGLE CRYSTAL |
| CN106395770A (en) * | 2016-06-30 | 2017-02-15 | 北京华进创威电子有限公司 | A purifying device and a purifying method for an aluminium nitride raw material |
| 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 |
Non-Patent Citations (4)
| Title |
|---|
| Purification and Size control of AlN Powder for AlN Single Crystal Growth;Kang Huk Lee, et al;《Materials Science Forum》;20141001;第804卷;实验部分 * |
| The Advanced Aluminum Nitride Synthesis Methods and Its Applications:Patent Review;Shishkin RA, et al;《Recent Patents On Nanotechnology》;20161231;第10卷(第2期);全文 * |
| 单晶生长用AlN粉料的烧结提纯工艺实验研究;汪佳等;《半导体光电》;20171215(第06期);实验部分，结果与讨论部分 * |
| 氮化铝粉体制备的研究及展望;杨清华等;《陶瓷学报》;20101231(第4期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108275664A (en) | 2018-07-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108275664B (en) | High-temperature sintering purification method for aluminum nitride | |
| TWI409371B (en) | Methods for producing metal nitrides and metal nitrides | |
| CN102674357A (en) | Method for synthesizing high-purity silicon carbide raw material for growing silicon carbide single crystals | |
| JPWO2009066663A1 (en) | Aluminum nitride single crystal polygonal column and method for producing plate-like aluminum nitride single crystal using the same | |
| KR100322374B1 (en) | Method of fabricating nitride crystal, mixture,liquid phase growth method, nitride crystal, nitride crystal powders, and vapor phase growth method | |
| JP2012240869A (en) | Silicon carbide powder and method for producing silicon carbide | |
| CN108193282B (en) | A kind of synthetic method and its application of high-purity silicon carbide raw material | |
| CN108118394B (en) | Method for reducing nitrogen impurity content in silicon carbide single crystal | |
| CN110219050A (en) | A kind of preparation method of aluminum nitride single crystal film | |
| CN103305903A (en) | Method for preparing GaN crystal by high-nitrogen pressure flux-crucible descending process | |
| CN109183143B (en) | Method for improving AlN single crystal purity by using reducing gas | |
| JP2007197274A (en) | Method for manufacturing silicon carbide single crystal | |
| JP6064247B2 (en) | Group III nitride crystal production method and production apparatus | |
| JP2004189549A (en) | Method of manufacturing aluminum nitride single crystal | |
| WO2011065534A1 (en) | Process for producing single-crystal aluminum nitride | |
| WO2014141959A1 (en) | METHOD AND DEVICE FOR MANUFACTURING GALLIUM NITRIDE (GaN) FREE-STANDING SUBSTRATE | |
| JP2013173638A (en) | Method for producing aluminum nitride crystal | |
| JP2009249202A (en) | Method for producing aluminum nitride single crystal | |
| JP4736365B2 (en) | Method for producing aluminum nitride single crystal | |
| JP5326865B2 (en) | Method for producing sapphire single crystal | |
| CN109112634B (en) | Crucible equipment and method for preparing aluminum nitride crystal | |
| JP2006315940A (en) | METHOD FOR GROWING AlN SINGLE CRYSTAL AND AlN SINGLE CRYSTAL | |
| JP2010280546A (en) | Method for producing silicon carbide single crystal | |
| Hsiao et al. | Synthesis and purification of silicon carbide powders for crystal growth | |
| KR101517024B1 (en) | Manufacturing Method of Aluminium Nitride Powder for Single Crystal Growing and Aluminium Nitride Powder |
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 | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20211111 Address after: 310000 Room 518, floor 5, building 3, 503 Shunfeng Road, Yuhang Economic and Technological Development Zone, Yuhang District, Hangzhou, Zhejiang Province Applicant after: Aochao photoelectric technology (Hangzhou) Co., Ltd Address before: 215699 103, building D, international student entrepreneurship Park, No. 1, Guotai North Road, Zhangjiagang City, Suzhou City, Jiangsu Province (Austrian trend Optoelectronics) Applicant before: Suzhou aoxu Photoelectric Technology Co., Ltd |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |