CN111321472B - Device and method for accurately expanding AlN seed crystals - Google Patents

Device and method for accurately expanding AlN seed crystals Download PDF

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Publication number
CN111321472B
CN111321472B CN202010218338.XA CN202010218338A CN111321472B CN 111321472 B CN111321472 B CN 111321472B CN 202010218338 A CN202010218338 A CN 202010218338A CN 111321472 B CN111321472 B CN 111321472B
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crucible
seed crystal
silicon carbide
graphite
carbide seed
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CN111321472A (en
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赵丽丽
范国峰
张胜涛
袁文博
刘德超
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Harbin Keyou Semiconductor Industry Equipment and Technology Research Institute Co Ltd
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Harbin Keyou Semiconductor Industry Equipment and Technology Research Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B35/00Apparatus 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
    • C30B35/007Apparatus for preparing, pre-treating the source material to be used for crystal growth
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B23/00Single-crystal growth by condensing evaporated or sublimed materials
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/40AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/403AIII-nitrides

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  • Crystallography & Structural Chemistry (AREA)
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Abstract

The invention relates to a device and a method for accurately expanding AlN seed crystals, and belongs to the field of crystal growth. The method is simple to operate and high in efficiency, and the AlN crystal with the corresponding size is manufactured according to the requirement. The AlN seed crystal precise expanding device comprises a graphite heater, a crucible and a growth combination, wherein the crucible is positioned in the graphite heater, the growth combination is positioned in the crucible, a silicon carbide seed crystal gasket is detachably connected with the crucible gasket and a crucible body, and AlN seed crystals with corresponding sizes can be obtained by replacing silicon carbide seed crystal gaskets with different sizes.

Description

Device and method for accurately expanding AlN seed crystals
Technical Field
The invention relates to a device and a method for accurately expanding AlN seed crystals, and belongs to the field of crystal growth.
Background
In the process of growing the aluminum nitride crystal by using the PVT method, because the radial growth of the AlN crystal is very difficult, the diameter of the AlN crystal is hardly changed, the seed crystal is very important for the growth of the crystal, the seed crystal does not have high quality and large size, the high-quality crystal can hardly grow, how to use a diameter expansion method (continuously iterative growth and increasing the diameter a little at a time) in the growth process of the crystal such as silicon carbide and the like for the growth of the AlN crystal, the diameter expansion is more difficult, the period and the cost are far superior to the diameter expansion of the crystal such as silicon carbide and the like, and the diameter can not be ensured to reach the expected state at a time of diameter expansion.
Based on the above problems, it is desirable to provide an apparatus and a method for accurately expanding AlN seed crystal to solve the above technical problems.
Disclosure of Invention
The invention provides a device and a method for accurately expanding AlN seed crystals, which have the advantages of simple operation and high efficiency, and can be used for manufacturing AlN crystals with corresponding sizes according to requirements. 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 is as follows:
the invention relates to a device and a method for accurately expanding AlN seed crystals, which comprises the following steps: the crucible is positioned in the graphite heater, and the growth assembly is positioned in the crucible; the graphite heater comprises a graphite heater upper cover, a graphite heater side wall, a graphite heater lower cover and a graphite raw material filter disc, wherein the graphite heater upper cover and the graphite heater lower cover are respectively connected with the upper end and the lower end of the graphite heater side wall; a method for accurately expanding AlN seed crystals comprises the following steps:
the method comprises the following steps: placing a crucible into a graphite heater, adding graphite powder between a graphite raw material filter disc of the graphite heater and a lower cover of the graphite heater, adding graphite powder to the lower side of the raw material filter disc in a crucible body, wherein the crucible cover, a crucible gasket, the raw material filter disc and the crucible body are made of Ta, and a silicon carbide seed crystal gasket is made of Ta silicon carbide;
step two: the graphite heater and crucible were evacuated to 10 deg.f-4-10-5Pa;
Step three: filling nitrogen at a rate of 50mL/min-1000mL/min, wherein the air pressure in the reaction device is between 200 and 700 Torr;
step four: heating a graphite heater at 1800-2230 ℃;
step five: volatilizing graphite powder at the temperature, respectively carrying out surface pre-carbonization processes on the outer side of the crucible and the inner side of the crucible, and keeping the processes for 10-90 hours, wherein the crucible cover, the crucible gasket, the raw material filter disc and the crucible body are made of TaC, and the silicon carbide seed crystal gasket is made of TaC;
step six: after the pre-carbonization process is finished, taking the crucible out of the device, adding high-purity AlN powder on the lower side of a raw material filter disc in the crucible, putting the silicon carbide seed crystal on a silicon carbide seed crystal gasket, wherein the thickness of the silicon carbide seed crystal is 0.1-10 mm, adding a layer of graphite paper on the outer ring and the upper layer of the silicon carbide seed crystal respectively, installing a crucible cover, and putting the crucible into a graphite heater again;
step seven: the graphite heater and crucible were evacuated to 10 deg.f-4-10-5Pa;
Step eight: filling nitrogen and argon at a flow rate of 200mL/min-1000mL/min, wherein the air pressure in the reaction device is between 300 and 750 Torr;
step nine: heating a graphite heater at 1900-2260 ℃;
step ten: the aluminum nitride powder is sublimated at the temperature to grow AIN seed crystals on the lower parts of the silicon carbide seed crystals, the process is kept for 10-100 hours, and the thickness of the layer of the AIN seed crystals is 2-5 mm;
step eleven: after the temperature is reduced, the crucible is taken out of the heater, and the silicon carbide seed crystal and the crucible are not integrated and are embedded on the crucible, so that the silicon carbide seed crystal gasket can support a growth combination on one hand, and does not need to consider how to bond or fix the silicon carbide seed crystal on a crucible cover, on the other hand, the AIN seed crystal is obtained by controlling the size of the silicon carbide seed crystal gasket, wherein the silicon carbide seed crystal can use 4H or 6H type silicon carbide seed crystal, and is finally taken out conveniently without damaging the crucible;
step twelve: after the crucible body is taken down, the crucible gasket and the silicon carbide seed crystal gasket are taken down, and the silicon carbide seed crystal gasket can be directly taken down easily because the outer ring of the silicon carbide seed crystal is provided with a layer of graphite paper;
step thirteen: then taking down the crucible cover, and taking down the growth combination with the AIN seed crystal;
fourteen steps: and cutting and grinding the silicon carbide seed crystal and the graphite paper by using a single-side cutting and grinding machine to obtain the aluminum nitride seed crystal with the determined size.
The crucible comprises a crucible cover, a crucible gasket, a silicon carbide seed crystal gasket, a raw material filter sheet and a crucible body, wherein the raw material filter sheet is arranged in the crucible body;
the growth combination comprises graphite paper and silicon carbide seed crystals, wherein the graphite paper separates the silicon carbide seed crystals placed in the crucible washer from the lower side wall of the crucible cover and the inner wall of the crucible washer, and the silicon carbide seed crystal washer supports the silicon carbide seed crystals. Preferably: the raw material filter disc and the graphite raw material filter disc are of net structures. The silicon carbide seed crystal is 4H or 6H silicon carbide seed crystal
The invention has the following beneficial effects:
1. compared with the prior art, the device and the method for accurately expanding the diameter of the AlN seed crystal accelerate the growth and expansion rate of the aluminum nitride crystal, save the cost and time for the growth and expansion of the aluminum nitride crystal and accelerate the development process of the aluminum nitride crystal growth industry;
2. the outer ring and the upper layer of the silicon carbide seed crystal are provided with graphite paper, so that the growth combination can be easily separated from the crucible;
3. the raw material filter disc and the graphite raw material filter disc can enable graphite powder to be uniformly diffused when volatilized, so that the inner surface and the outer surface of the crucible are uniformly carbonized, the raw material filter disc can filter impurities in raw materials, and the crystal purity is improved.
Drawings
FIG. 1 is a front view of an apparatus and method for precise diameter expansion of an AlN seed crystal;
FIG. 2 is a schematic diagram of a feed filter;
FIG. 3 is a schematic view of the structure of the crucible;
FIG. 4 is a schematic diagram of an AlN seed crystal taking-off step;
in the figure, 1-graphite heater, 1-1-graphite heater upper cover, 1-2-graphite heater side wall, 1-3-graphite heater lower cover, 1-4-graphite raw material filter, 2-crucible, 2-1-crucible cover, 2-2-crucible gasket, 2-3-silicon carbide seed crystal gasket, 2-4-raw material filter, 2-5-crucible body, 3-growth combination, 3-1-graphite paper, 3-2-silicon carbide seed crystal and 3-3-AIN seed crystal are adopted.
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 specific implementation mode is as follows:
the embodiment is described with reference to fig. 1-4, and the AlN seed crystal precise diameter expanding device and the method of the embodiment comprise a graphite heater 1, a crucible 2 and a growth combination 3, wherein the crucible 2 is positioned inside the graphite heater 1, and the growth combination 3 is positioned inside the crucible 2;
the graphite heater 1 comprises a graphite heater upper cover 1-1, a graphite heater side wall 1-2, a graphite heater lower cover 1-3 and a graphite raw material filter sheet 1-4, wherein the graphite heater upper cover 1-1 and the graphite heater lower cover 1-3 are respectively connected with the upper end and the lower end of the graphite heater side wall 1-2, the graphite raw material filter sheet 1-4 is positioned inside the graphite heater side wall 1-2, the graphite raw material filter sheet 1-4 is connected with the graphite heater side wall 1-2, and the graphite raw material filter sheet 1-4 can support the crucible 2;
the crucible 2 comprises a crucible cover 2-1, a crucible washer 2-2, a silicon carbide seed crystal washer 2-3, a raw material filter 2-4 and a crucible body 2-5, the raw material filter 2-4 is arranged in the crucible body 2-5, the silicon carbide seed crystal washer 2-3, the crucible washer 2-2 and the crucible cover 2-1 are sequentially arranged on the upper portion of the crucible body 2-5, the crucible body 2-5 is detachably connected with the silicon carbide seed crystal washer 2-3, the silicon carbide seed crystal washer 2-3 is detachably connected with the crucible washer 2-2, the crucible washer 2-2 is detachably connected with the crucible cover 2-1, the crucible body 2-5 is placed on the graphite raw material filter 1-4, the silicon carbide seed crystal washer 2-3 is detachably connected with the crucible washer 2-2 and the crucible body 2-5, the AIN seed crystal with corresponding size can be obtained by replacing the silicon carbide seed crystal gaskets 2-3 with different sizes, the operation is simple, the problem of difficult diameter expansion in the growth process of the aluminum nitride crystal is fundamentally solved, compared with the prior art, the device and the method for accurately expanding the AlN seed crystal accelerate the diameter expansion rate of the aluminum nitride crystal, save the cost and time for the diameter expansion of the aluminum nitride crystal, accelerate the development process of the growth industry of the AIN seed crystal 3-3, and the crucible 2 and the graphite heater 1 can expand to realize natural sealing at high temperature;
the growth assembly 3 comprises 3-1 parts of graphite paper and 3-2 parts of silicon carbide seed crystals, the graphite paper 3-1 separates the silicon carbide seed crystals 3-2 arranged in the crucible washer 2-2 from the lower side wall of the crucible cover 2-1 and the inner wall of the crucible washer 2-2, and the silicon carbide seed crystal washer 2-3 supports the silicon carbide seed crystals 3-2.
The method comprises the following implementation steps:
the method comprises the following steps: placing a crucible 2 into a graphite heater 1, adding graphite powder between a graphite raw material filter sheet 1-4 of the graphite heater 1 and a graphite heater lower cover 1-3, adding graphite powder to the lower side of the raw material filter sheet 2-4 in a crucible body 2-5, adding the crucible cover 2-1, a crucible gasket 2-2, the raw material filter sheet 2-4, the crucible body 2-5 and a silicon carbide seed crystal gasket 2-3;
step two: the graphite heater 1 and the crucible 2 are vacuumized to 10-4-10-5Pa;
Step three: filling nitrogen at a rate of 50mL/min-1000mL/min, wherein the air pressure in the reaction device is between 200 and 700 Torr;
step four: heating a graphite heater 1 at the temperature of 1800-2230 ℃;
step five: the graphite powder is volatilized at the temperature, the surface pre-carbonization process is respectively carried out on the outer side of the crucible 2 and the inner side of the crucible 2, the process is kept for 10 to 90 hours, and the crucible cover 2-1, the crucible gasket 2-2, the raw material filter 2-4, the crucible body 2-5 and the silicon carbide seed crystal gasket 2-3 are respectively arranged on the crucible body;
step six: after the pre-carbonization process is finished, taking the crucible 2 out of the device, adding high-purity AlN powder at the lower side of a raw material filter 2-4 in the crucible 2, placing a silicon carbide seed crystal 3-2 on a silicon carbide seed crystal gasket 2-3, wherein the thickness of the silicon carbide seed crystal 3-2 is 0.1-10 mm, adding a layer of graphite paper 3-1 on the outer ring and the upper layer of the silicon carbide seed crystal 3-2 respectively, installing a crucible cover 2-1, and putting the crucible cover into a graphite heater 1 again;
step seven: the graphite heater 1 and the crucible 2 are vacuumized to 10-4-10-5Pa;
Step eight: filling nitrogen and argon at a flow rate of 200mL/min-1000mL/min, wherein the air pressure in the reaction device is between 300 and 750 Torr;
step nine: heating a graphite heater 1 at the temperature of 1900-2260 ℃;
step ten: the aluminum nitride powder is sublimated at the temperature to grow the AIN seed crystal 3-3 at the lower part of the silicon carbide seed crystal 3-2, the process is kept for 10-100 hours, and the thickness of the layer of the AIN seed crystal 3-3 is 2-5 mm;
step eleven: after the temperature is reduced, taking the crucible 2 out of the heater, wherein the silicon carbide seed crystal 3-2 and the crucible 2 are not integrated and are embedded on the crucible 2, the silicon carbide seed crystal gasket 2-3 can support the growth combination 3 on one hand, and does not need to consider how to bond or fix the silicon carbide seed crystal 3-2 on the crucible cover 2-1, on the other hand, the AIN seed crystal 3-3 is obtained by controlling the size of the silicon carbide seed crystal gasket 2-3, wherein the silicon carbide seed crystal 3-2 uses 4H or 6H type silicon carbide seed crystals, and is finally convenient to take out without damaging the crucible 2;
step twelve: after the crucible body 2-5 is taken down, the crucible gasket 2-2 and the silicon carbide seed crystal gasket 2-3 are taken down, and the silicon carbide seed crystal 3-2 can be directly taken down easily without damaging the crucible 2 because the outer ring of the silicon carbide seed crystal 3-2 is provided with the graphite paper 3-1;
step thirteen: then taking down the crucible cover 2-1, and taking down the growth assembly 3 with the AIN seed crystal 3-3;
fourteen steps: and (3) cutting and grinding the silicon carbide seed crystal 3-2 and the graphite paper 3-1 by using a single-side cutting and grinding machine to obtain the aluminum nitride seed crystal with the determined size.
The device for accurately expanding the diameter of the AlN seed crystal is described by combining the figures 1-4, the raw material filter 2-4 and the graphite raw material filter 1-4 are of a net structure, the raw material filter 2-4 can uniformly diffuse the graphite powder when volatilizing to uniformly carbonize the inner surface of the crucible, the raw material filter 2-4 can filter impurities in the raw material to improve the crystal purity, and the graphite raw material filter 1-4 can uniformly diffuse the graphite powder when volatilizing to uniformly carbonize the outer surface of the crucible.
The present embodiment will be described with reference to fig. 1 to 4, and the apparatus for precisely expanding AlN seed crystal according to the present embodiment uses a 4H or 6H type silicon carbide seed crystal for silicon carbide seed crystal 3-2, and is easy to take out without damaging crucible 2.
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 (3)

1. A method for accurately expanding AlN seed crystals comprises a device for accurately expanding the AlN seed crystals, and is characterized in that: the crucible growth device comprises a graphite heater (1), a crucible (2) and a growth combination (3), wherein the crucible (2) is positioned in the graphite heater (1), and the growth combination (3) is positioned in the crucible (2);
the graphite heater (1) comprises a graphite heater upper cover (1-1), a graphite heater side wall (1-2), a graphite heater lower cover (1-3) and graphite raw material filter sheets (1-4), wherein the graphite heater upper cover (1-1) and the graphite heater lower cover (1-3) are respectively connected with the upper end and the lower end of the graphite heater side wall (1-2), the graphite raw material filter sheets (1-4) are positioned inside the graphite heater side wall (1-2), and the graphite raw material filter sheets (1-4) are connected with the graphite heater side wall (1-2);
the crucible (2) comprises a crucible cover (2-1), a crucible gasket (2-2) and a silicon carbide seed crystal gasket (2-3), the crucible comprises a raw material filter disc (2-4) and a crucible body (2-5), wherein the raw material filter disc (2-4) is installed in the crucible body (2-5), a silicon carbide seed crystal gasket (2-3), a crucible gasket (2-2) and a crucible cover (2-1) are sequentially installed on the upper portion of the crucible body (2-5), the crucible body (2-5) is detachably connected with the silicon carbide seed crystal gasket (2-3), the silicon carbide seed crystal gasket (2-3) is detachably connected with the crucible gasket (2-2), the crucible gasket (2-2) is detachably connected with the crucible cover (2-1), and the crucible body (2-5) is placed on the graphite raw material filter disc (1-4);
the growth assembly (3) comprises graphite paper (3-1) and silicon carbide seed crystals (3-2), the graphite paper (3-1) separates the silicon carbide seed crystals (3-2) placed in the crucible washer (2-2) from the lower side wall of the crucible cover (2-1) and the inner wall of the crucible washer (2-2), and the silicon carbide seed crystal washer (2-3) supports the silicon carbide seed crystals (3-2);
an AlN seed crystal accurate diameter expanding method comprises the following steps:
the method comprises the following steps: putting a crucible (2) into a graphite heater (1), adding graphite powder between a graphite raw material filter sheet (1-4) of the graphite heater (1) and a graphite heater lower cover (1-3), adding graphite powder into the lower side of the raw material filter sheet (2-4) in a crucible body (2-5), wherein the crucible cover (2-1), a crucible gasket (2-2), the raw material filter sheet (2-4) and the crucible body (2-5) are made of TaC, and the silicon carbide seed crystal gasket (2-3) is made of TaC;
step two: the graphite heater (1) and the crucible (2) are vacuumized to 10-4-10-5Pa;
Step three: filling nitrogen at a rate of 50mL/min-1000mL/min, wherein the air pressure in the reaction device is between 200 and 700 Torr;
step four: heating a graphite heater (1) at the temperature of 1800-2230 ℃;
step five: the graphite powder volatilizes at the temperature, a surface pre-carbonization process is respectively carried out on the outer side of the crucible (2) and the inner side of the crucible (2), the process is kept for 10-90 hours, the crucible cover (2-1), the crucible gasket (2-2), the raw material filter disc (2-4) and the crucible body (2-5) are made of TaC, and the silicon carbide seed crystal gasket (2-3) is made of TaC;
step six: after the pre-carbonization process is finished, taking the crucible (2) out of the device, adding high-purity AlN powder at the lower side of a raw material filter disc (2-4) in the crucible (2), putting the silicon carbide seed crystal (3-2) on a silicon carbide seed crystal gasket (2-3), wherein the thickness of the silicon carbide seed crystal (3-2) is 0.1-10 mm, adding a layer of graphite paper (3-1) on the outer ring and the upper layer of the silicon carbide seed crystal (3-2), installing a crucible cover (2-1), and putting the crucible cover into a graphite heater (1) again;
step seven: the graphite heater (1) and the crucible (2) are vacuumized to 10-4-10-5Pa;
Step eight: filling nitrogen and argon at a flow rate of 200mL/min-1000mL/min, wherein the air pressure in the reaction device is between 300 and 750 Torr;
step nine: heating the graphite heater (1) at the temperature of 1900-2260 ℃;
step ten: the aluminum nitride powder is sublimated at the temperature to grow the AlN seed crystal (3-3) at the lower part of the silicon carbide seed crystal (3-2), the process is kept for 10-100 hours, and the thickness of the layer of the AlN seed crystal (3-3) is 2-5 mm;
step eleven: after the temperature is reduced, the crucible (2) is taken out of the heater, and as the silicon carbide seed crystal (3-2) is not integrated with the crucible (2) and is embedded in the crucible (2), the silicon carbide seed crystal gasket (2-3) supports the growth combination (3) on one hand, no consideration is given to how to bond or fix the silicon carbide seed crystal (3-2) on the crucible cover (2-1), and on the other hand, the AlN seed crystal (3-3) is obtained by controlling the size of the silicon carbide seed crystal gasket (2-3);
step twelve: after the crucible body (2-5) is taken down, the crucible gasket (2-2) and the silicon carbide seed crystal gasket (2-3) are taken down, and the silicon carbide seed crystal (3-2) can be directly taken down easily because the outer ring of the silicon carbide seed crystal (3-2) is provided with a layer of graphite paper (3-1);
step thirteen: then taking down the crucible cover (2-1), and taking down the growth combination (3) with the AlN seed crystals (3-3);
fourteen steps: and (3) cutting and grinding the silicon carbide seed crystal (3-2) and the graphite paper (3-1) by using a single-side cutting and grinding machine to obtain the aluminum nitride seed crystal with a predetermined size.
2. The method for accurately expanding the diameter of the AlN seed crystal according to claim 1, wherein: wherein the silicon carbide seed crystal (3-2) adopts 4H or 6H type silicon carbide seed crystal, is convenient to take out and does not damage the crucible (2).
3. A method of accurately expanding AlN seed crystal according to claim 2, wherein: the raw material filter discs (2-4) and the graphite raw material filter discs (1-4) are of a net structure.
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CN113957521B (en) * 2020-07-20 2022-12-30 北京大学 Method and device for preparing AlN single crystal by using easy-to-expand splicing seed crystal technology
CN113564697B (en) * 2021-07-22 2022-07-22 北京大学 Method for heterologously growing AlN on SiC seed crystal by using PVT method

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