CN111663185A - Device and method for preparing powder for PVT method aluminum nitride single crystal growth - Google Patents
Device and method for preparing powder for PVT method aluminum nitride single crystal growth Download PDFInfo
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- CN111663185A CN111663185A CN202010573693.9A CN202010573693A CN111663185A CN 111663185 A CN111663185 A CN 111663185A CN 202010573693 A CN202010573693 A CN 202010573693A CN 111663185 A CN111663185 A CN 111663185A
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- 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
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- 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
- C01B21/0726—Preparation by carboreductive nitridation
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- 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
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Abstract
The invention relates to a device and a method for preparing powder for PVT method aluminum nitride single crystal growth, belonging to the field of crystal growth. The purification is achieved by using a simple apparatus to prepare the starting material for crystal growth. The crucible furnace comprises a pressure combination, a furnace shell, a crucible top cover, a ceramic crucible, a motor, a supporting rod, a tray, an outer crucible, a gasket and a tungsten heater, wherein the motor is arranged at the lower part of the furnace shell, the output end of the motor is connected with the supporting rod positioned inside the furnace shell, the upper end of the supporting rod is fixedly connected with the tray, the outer crucible is arranged on the upper part of the tray, the ceramic crucible is arranged inside the outer crucible, the ceramic cover is arranged on the upper part of the ceramic crucible, the crucible top cover is arranged on the upper side of the outer crucible, the gasket is positioned between the outer crucible and the crucible top cover, the gasket is arranged outside the ceramic cover, the pressure combination is arranged on the upper side of the crucible top cover, the pressure combination is connected with.
Description
Technical Field
The invention relates to a device and a method for preparing powder for PVT method aluminum nitride single crystal growth, belonging to the field of crystal growth.
Background
The aluminum nitride powder is used as a precondition for preparing an aluminum nitride crystal material, the preparation of aluminum nitride and the purity and the property of the aluminum nitride are very important for the crystal growth, the existing equipment and method for preparing the aluminum nitride high-purity powder generally need pretreatment and post-treatment to obtain the powder with high relative purity, and the methods have more or less defects, such as product agglomeration, long reaction time, high temperature, expensive raw materials, low yield, and even the methods (plasma method) for preparing the aluminum nitride powder have large production energy consumption, complex equipment and high cost.
In view of the above problems, it is desirable to provide an apparatus and a method for preparing a powder for PVT aluminum nitride single crystal growth to solve the above technical problems.
Disclosure of Invention
The invention provides a device and a method for preparing powder for PVT method aluminum nitride single crystal growth, aiming at preparing raw materials for crystal growth by using a simple device and achieving the aim of purification. The following presents a simplified summary of the invention in order to provide a basic understanding of some aspects of the invention. It should be understood that this summary is not an exhaustive overview of the invention. It is not intended to determine the key or critical elements of the present invention, nor is it intended to limit the scope of the present invention.
The technical scheme of the invention is as follows:
the utility model provides a device for preparing PVT method aluminium nitride powder for single crystal growth, including capping mechanism, the stove outer covering, the crucible top cap, ceramic cover, ceramic crucible, including a motor, an end cap, a controller, and a cover plate, the bracing piece, a tray, outer crucible, packing ring and tungsten heater, the lower part of stove outer covering is provided with the motor, the output of motor is connected with the bracing piece that is located the stove outer covering inside, the upper end and the tray fixed connection of bracing piece, the upper portion of tray is provided with outer crucible, the inside of outer crucible is provided with ceramic crucible, ceramic crucible's upper portion is provided with ceramic cover, the crucible top cap sets up the upside at outer crucible, the packing ring is located between outer crucible and the crucible top cap, the packing ring sets up in the ceramic cover outside, capping mechanism sets up at crucible top cap upside, capping mechanism establishes with the stove outer covering.
Preferably: the capping mechanism comprises a driving motor, a worm wheel, a worm, a screw rod, a connecting seat and a pressure head, wherein the output end of the driving motor is connected with the worm wheel, the worm wheel is meshed with the worm, the worm is meshed with the screw rod, the screw rod is in threaded connection with the connecting seat, the connecting seat is fixedly connected with the pressure head, the pressure head is positioned on the upper side of the crucible top cover, and the pressure head is in sliding connection with the furnace shell.
Preferably: the crucible top cover, the supporting rod, the tray, the outer crucible and the washer are made of tungsten.
Preferably: the ceramic cover and the ceramic crucible are made of aluminum nitride.
Preferably: the aluminum nitride ceramic crucible material also comprises a mixture, wherein the mixture consists of aluminum nitride ceramic balls, alumina powder and carbon powder, the mixture is placed in a ceramic crucible, and the molar ratio of the carbon powder to the alumina powder is more than 3: 1.
a method for preparing powder for PVT method aluminum nitride single crystal growth comprises the following steps:
the method comprises the following steps: taking a proper amount of carbon powder and alumina powder, filling the carbon powder and the alumina powder into a ceramic crucible, covering a ceramic cover, introducing nitrogen into the ceramic crucible, and ensuring that the pressure in the ceramic crucible reaches more than 2-20 Mpa;
step two: opening a tungsten heater, heating the carbon powder and the alumina powder to 1500-1600 ℃, keeping the temperature for 10-60 hours, enabling the gasket to expand at high temperature and prop between the ceramic cover and the ceramic crucible to realize self-sealing, and under the action of excessive carbon and nitrogen, carrying out the reaction of Al2O3(s) +3C(s) + N2(g) 2Al N(s) +3CO (g) to the right under the action of high temperature;
step three: cooling to 600-700 ℃, shrinking the gasket to diffuse the excessive carbon from the recovered semi-closed ceramic crucible, and vacuumizing again to take away the excessive carbon;
step four: after the reaction is completed, taking out the ceramic crucible, putting the ceramic crucible into a muffle furnace, keeping the air atmosphere, raising the temperature to 600-700 ℃, keeping the temperature for 10-20 hours for decarburization treatment, wherein the air can fully react with excessive carbon powder to take away excessive carbon;
step five: cooling, taking out the prepared raw materials, grinding into powder, washing with water again, and oven drying.
Preferably: and adding aluminum nitride ceramic balls in the step one, mixing the aluminum nitride ceramic balls with carbon powder and alumina powder, then loading the mixture into a ceramic crucible, then covering a ceramic cover, introducing nitrogen into the ceramic crucible, and ensuring that the pressure in the ceramic crucible reaches more than 2-20 Mpa.
The invention has the following beneficial effects:
1. the mixture is fully mixed under the action of high-speed aluminum nitride ball milling, the reaction speed is accelerated, the reaction is more sufficient, the purpose of fully mixing can be achieved at low temperature, the mixture is further uniformly mixed under the action of high-temperature diffusion at high temperature, the reaction is promoted, and the particle size of the generated powder material is more uniform;
at 2.1600 ℃, the aluminum nitride ceramic can still be kept very stable, and the reactants are effectively prevented from being polluted;
3. the device is in a semi-sealed state through a high-temperature sealing structure, and the sealing structure is self-sealed to reach an internal high-pressure state because the thermal expansion coefficient of tungsten is higher than that of aluminum nitride under the high-temperature state, so that internal reaction is not influenced by external heaters and crucible materials, and more impurities are introduced.
4. After the full reaction at high temperature, the temperature is reduced by 600-.
Drawings
FIG. 1 is a front view of an apparatus for preparing a powder for PVT process aluminum nitride single crystal growth;
FIG. 2 is a schematic structural view of a capping mechanism;
FIG. 3 is a partial schematic view of an apparatus for preparing a powder for PVT method aluminum nitride single crystal growth;
in the figure, 1-a capping mechanism, 1-1-a driving motor, 1-2-a worm wheel, 1-3-a worm, 1-4-a screw rod, 1-5-a connecting seat, 1-6-a pressure head, 2-a furnace shell, 3-a crucible top cover, 4-a ceramic cover, 5-a ceramic crucible, 6-a mixture, 7-a motor, 8-a supporting rod, 9-a tray, 10-an outer crucible, 11-a gasket and 12-a tungsten heater.
Detailed Description
In order that the objects, aspects and advantages of the invention will become more apparent, the invention will be described by way of example only, and in connection with the accompanying drawings. It is to be understood that such description is merely illustrative and not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
The connection mentioned in the present invention is divided into a fixed connection and a detachable connection, the fixed connection (i.e. the non-detachable connection) includes but is not limited to a folding connection, a rivet connection, an adhesive connection, a welding connection, and other conventional fixed connection methods, the detachable connection includes but is not limited to a screw connection, a snap connection, a pin connection, a hinge connection, and other conventional detachment methods, when the specific connection method is not clearly defined, the function can be realized by always finding at least one connection method from the existing connection methods by default, and a person skilled in the art can select the connection method according to needs. For example: the fixed connection selects welding connection, and the detachable connection selects hinge connection.
The first embodiment is as follows: the embodiment is described by combining figures 1-3, the device for preparing powder for PVT method aluminum nitride single crystal growth of the embodiment comprises a capping mechanism 1, a furnace shell 2, a crucible top cover 3, a ceramic cover 4, a ceramic crucible 5, a motor 7, a support rod 8, a tray 9, an outer crucible 10, a gasket 11 and a tungsten heater 12, wherein the motor 7 is arranged at the lower part of the furnace shell 2, the output end of the motor 7 is connected with the support rod 8 positioned inside the furnace shell 2, the upper end of the support rod 8 is fixedly connected with the tray 9, the outer crucible 10 is arranged at the upper part of the tray 9, the ceramic crucible 5 is arranged inside the outer crucible 10, the ceramic cover 4 is arranged at the upper part of the ceramic crucible 5, the crucible top cover 3 is arranged at the upper side of the outer crucible 10, the gasket 11 is positioned between the outer crucible 10 and the crucible top cover 3, the gasket 11 is arranged at the outer side of the ceramic cover 4, the capping mechanism 1 is, capping mechanism 1 establishes with stove outer covering 2 and is connected, the inside tungsten heater 12 that is provided with of stove outer covering 2, tungsten heater 12 is located the outside of outer crucible 10, motor 7 drives bracing piece 8 rotatory, bracing piece 8 drives tray 9 rotatory, tray 9 drives outer crucible 10 rotatory, make the intensive mixing of mixture under the effect of high-speed aluminium nitride ball-milling, accelerate reaction rate, make the reaction more abundant, can reach the mesh of intensive mixing under the low temperature, the purpose that further misce bene promotion reaction goes on under the effect of high temperature diffusion under the high temperature, and make the powder material particle diameter of formation more even.
The second embodiment is as follows: the embodiment is described by combining fig. 1 and fig. 3, the capping mechanism 1 of the embodiment comprises a driving motor 1-1, a worm wheel 1-2, a worm 1-3, a screw rod 1-4, a connecting seat 1-5 and a pressure head 1-6, the output end of the driving motor 1-1 is connected with the worm wheel 1-2, the worm wheel 1-2 is meshed with the worm 1-3, the worm 1-3 is meshed with the screw rod 1-4, the screw rod 1-4 is in threaded connection with the connecting seat 1-5, the connecting seat 1-5 is fixedly connected with the pressure head 1-6, the pressure head 1-6 is positioned on the upper side of a crucible top cover 3, the pressure head 1-6 is in sliding connection with a furnace shell 2, the driving motor 1-1 drives the worm wheel 1-2 to rotate, the worm wheel 1-2 drives the worm 1-3 to rotate, the worm 1-3 drives the screw rod 1-4 to rotate, because the radial position of the screw rod 1-4 is not changed, the radial position of the connecting seat 1-5 is changed, so that the pressure applied by the pressure head 1-6 to the crucible top cover 3 is changed, in this embodiment, the support of the capping mechanism 1 is not shown in the figure, but it should be understood that a person skilled in the art can install the support for bearing the capping mechanism 1 by means of the prior art, for example, a support is formed by welding steel pipes together, and the capping mechanism 1 is fixedly installed on the support welded together by the steel pipes by bolts and is fixed in position relative to the furnace shell 2.
The third concrete implementation mode: the present embodiment is described with reference to fig. 1-2, and the material of the crucible top cover 3, the support rod 8, the tray 9, the outer crucible 10 and the gasket 11 is tungsten, the crucible top cover 3, the support rod 8, the tray 9, the outer crucible 10 and the gasket 11 are in a semi-sealed state when the apparatus is used in a low temperature state, and in a high temperature state, because the thermal expansion coefficient of tungsten is higher than that of aluminum nitride, the volume of the crucible top cover 3, the support rod 8, the tray 9, the outer crucible 10 and the gasket 11 is increased, the apparatus is self-sealed to reach an internal high pressure state, so that the internal reaction is not affected by the material of the external tungsten heater 12, the outer crucible 10 and the gasket 11, and more impurities are introduced.
The fourth concrete implementation mode: the present embodiment is described with reference to fig. 1-2, and the material of the ceramic lid 4 and the ceramic crucible 5 of the apparatus for preparing the powder for PVT aluminum nitride single crystal growth of the present embodiment is aluminum nitride, and the aluminum nitride ceramic can still be kept very stable at 1600 ℃, thereby effectively preventing the reactant from being contaminated.
The fifth concrete implementation mode: the embodiment is described by combining figures 1-3, and the device for preparing the powder for growing the PVT method aluminum nitride single crystal further comprises a mixture 6, wherein the mixture 6 consists of aluminum nitride ceramic balls, alumina powder and carbon powder, the mixture 6 is placed in a ceramic crucible 5, and the molar ratio of the carbon powder to the alumina powder is more than 3: 1.
the sixth specific implementation mode: the present embodiment is described with reference to fig. 1 to 3, and the method for preparing the powder for PVT-method aluminum nitride single crystal growth according to the present embodiment comprises the following steps:
the method comprises the following steps: taking a proper amount of carbon powder and alumina powder, filling the ceramic crucible 5 with the carbon powder and the alumina powder, covering a ceramic cover 4, introducing nitrogen into the ceramic crucible 5, and ensuring that the pressure in the ceramic crucible 5 reaches more than 2-20 Mpa;
step two: the tungsten heater 12 is opened, the carbon powder and the alumina powder are heated to 1500-;
step three: cooling to 600-700 ℃, shrinking the gasket 11, diffusing excessive carbon from the recovered semi-closed ceramic crucible 5, and vacuumizing again to take away the reaction gas CO;
step four: after the reaction is completed, taking out the ceramic crucible 5, putting the ceramic crucible into a muffle furnace, keeping the atmosphere of air, raising the temperature to 600-700 ℃, keeping the temperature for 10-20 hours for decarburization treatment, wherein the air can fully react with excessive carbon powder, and a large amount of excessive raw materials such as carbon and the like can be volatilized and reacted, so that the aluminum nitride material is more pure;
step five: cooling, taking out the prepared raw materials, grinding into powder, washing with water again, and oven drying.
The seventh embodiment: the method is described by combining the figures 1-3, and the method for preparing the powder for PVT method aluminum nitride single crystal growth of the embodiment also comprises the steps of adding aluminum nitride ceramic balls in the first step, mixing the aluminum nitride ceramic balls with carbon powder and alumina powder, then filling the mixture into a ceramic crucible 5, then covering a ceramic cover 4, introducing nitrogen into the ceramic crucible 5, and ensuring that the pressure in the ceramic crucible 5 reaches more than 2-20 MPa; the tungsten heater 12 is opened to heat the carbon powder and the alumina powder to 1500-1600 ℃, the temperature is kept for 10-60 hours, at the moment, the gasket 11 expands at high temperature and is propped between the ceramic cover 4 and the ceramic crucible 5 to realize self-sealing, the motor 7 is started, the motor 7 drives the ceramic crucible 5 to rotate, the aluminum nitride ceramic ball can rotate under the centrifugal action, the aluminum nitride ceramic ball enables the mixture 6 to be fully mixed and react in the friction collision with the alumina powder of the carbon powder, the motor 7 is at a high speed at low temperature, and the motor 7 is at a low speed at high temperature.
It should be noted that, in the above embodiments, as long as the technical solutions can be aligned and combined without contradiction, those skilled in the art can exhaust all possibilities according to the mathematical knowledge of the alignment and combination, and therefore, the present invention does not describe the technical solutions after alignment and combination one by one, but it should be understood that the technical solutions after alignment and combination have been disclosed by the present invention.
This embodiment is only illustrative of the patent and does not limit the scope of protection thereof, and those skilled in the art can make modifications to its part without departing from the spirit of the patent.
Claims (7)
1. The device for preparing the powder for PVT method aluminum nitride single crystal growth is characterized in that: comprises a gland mechanism (1), a furnace shell (2), a crucible top cover (3), a ceramic cover (4), a ceramic crucible (5), a motor (7), a support rod (8), a tray (9), an outer crucible (10), a gasket (11) and a tungsten heater (12), wherein the lower part of the furnace shell (2) is provided with the motor (7), the output end of the motor (7) is connected with the support rod (8) positioned inside the furnace shell (2), the upper end of the support rod (8) is fixedly connected with the tray (9), the upper part of the tray (9) is provided with the outer crucible (10), the ceramic crucible (5) is arranged inside the outer crucible (10), the ceramic cover (4) is arranged on the upper part of the ceramic crucible (5), the crucible top cover (3) is arranged on the upper side of the outer crucible (10), the gasket (11) is positioned between the outer crucible (10) and the crucible top cover (3), the gasket (11) is arranged on the outer side of the, the capping mechanism (1) is arranged on the upper side of the crucible top cover (3), the capping mechanism (1) is connected with the furnace shell (2), the tungsten heater (12) is arranged inside the furnace shell (2), and the tungsten heater (12) is positioned on the outer side of the outer crucible (10).
2. The apparatus for preparing powder for PVT method aluminum nitride single crystal growth according to claim 1, wherein: the cover pressing mechanism (1) comprises a driving motor (1-1), a worm wheel (1-2), a worm (1-3), a screw rod (1-4), a connecting seat (1-5) and a pressure head (1-6), the output end of the driving motor (1-1) is connected with the worm wheel (1-2), the worm wheel (1-2) is meshed with the worm (1-3), the worm (1-3) is meshed with the screw rod (1-4), the screw rod (1-4) is in threaded connection with the connecting seat (1-5), the connecting seat (1-5) is fixedly connected with the pressure head (1-6), the pressure head (1-6) is located on the upper side of the crucible top cover (3), and the pressure head (1-6) is in sliding connection with the furnace shell (2).
3. The apparatus for preparing powder for PVT method aluminum nitride single crystal growth according to claim 1, wherein: the crucible top cover (3), the supporting rod (8), the tray (9), the outer crucible (10) and the washer (11) are made of tungsten.
4. The apparatus for preparing powder for PVT method aluminum nitride single crystal growth according to claim 1, wherein: the ceramic cover (4) and the ceramic crucible (5) are made of aluminum nitride.
5. The apparatus for preparing powder for PVT method aluminum nitride single crystal growth according to claim 1, wherein: the aluminum nitride crucible is characterized by further comprising a mixture (6), wherein the mixture (6) is composed of aluminum nitride ceramic balls, alumina powder and carbon powder, the mixture (6) is placed in the ceramic crucible (5), and the molar ratio of the carbon powder to the alumina powder is more than 3: 1.
6. a method for preparing powder for PVT method aluminum nitride single crystal growth is characterized in that: the method comprises the following steps:
the method comprises the following steps: taking a proper amount of carbon powder and alumina powder, filling the carbon powder and the alumina powder into a ceramic crucible (5), covering a ceramic cover (4), introducing nitrogen into the ceramic crucible (5), and ensuring that the pressure in the ceramic crucible (5) reaches more than 2-20 Mpa;
step two: the tungsten heater (12) is opened, the carbon powder and the alumina powder are heated to 1500-1600 ℃, the temperature is kept for 10-60 hours, at the moment, the gasket (11) expands at high temperature and is propped between the ceramic cover (4) and the ceramic crucible (5) to realize self-sealing, and under the action of excessive carbon and nitrogen, the reaction of Al2O3(s) +3C(s) + N2(g) ═ 2AlN(s) +3CO (g) is carried out towards the right under the action of high temperature;
step three: cooling to 600-700 ℃, shrinking the gasket (11) to diffuse the excessive carbon from the recovered semi-closed ceramic crucible (5), and vacuumizing again to take away the excessive carbon;
step four: after the reaction is completed, taking out the ceramic crucible (5), putting the ceramic crucible into a muffle furnace, keeping the atmosphere of air, raising the temperature to 600-700 ℃, keeping the temperature for 10-20 hours for decarburization treatment, wherein the air can fully react with excessive carbon powder to take away excessive carbon;
step five: cooling, taking out the prepared raw materials, grinding into powder, washing with water again, and oven drying.
7. The method for preparing powder for PVT method aluminum nitride single crystal growth according to claim 6, wherein: and adding aluminum nitride ceramic balls in the step one, mixing the aluminum nitride ceramic balls with carbon powder and alumina powder, putting the mixture into a ceramic crucible (5), then covering a ceramic cover (4), introducing nitrogen into the ceramic crucible (5), and ensuring that the pressure in the ceramic crucible (5) reaches more than 2-20 MPa.
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CN112979335A (en) * | 2021-02-08 | 2021-06-18 | 哈尔滨化兴软控科技有限公司 | Preparation method of aluminum nitride porous raw material |
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CN110790244A (en) * | 2019-10-30 | 2020-02-14 | 大连海事大学 | Method for preparing AlN ceramic powder by carbothermic reduction nitridation method |
CN111364104A (en) * | 2020-04-23 | 2020-07-03 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of high-purity raw material for aluminum nitride single crystal growth |
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