CN212476953U - Heating device of GaN single crystal growth device - Google Patents
Heating device of GaN single crystal growth device Download PDFInfo
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- CN212476953U CN212476953U CN202020789389.3U CN202020789389U CN212476953U CN 212476953 U CN212476953 U CN 212476953U CN 202020789389 U CN202020789389 U CN 202020789389U CN 212476953 U CN212476953 U CN 212476953U
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Abstract
The utility model provides a GaN single crystal growth device's heating device, including an airtight autoclave and be located the outside heating device of autoclave, autoclave fixed mounting is inside the hot isostatic pressing container, and the autoclave outside is equipped with a gaseous kuppe, and the hot isostatic pressing container is inside still to be equipped with a gas circulation device to realize the convection circulation of the outside gas of autoclave. The utility model can realize the step temperature difference between the upper part and the lower part of the autoclave by arranging the heating device, thereby accelerating the rapid growth of the GaN single crystal; the heat insulation layer is arranged, so that the influence of the external temperature of the high-pressure kettle on the internal temperature of the high-pressure kettle is avoided; by arranging the heating device and the gas circulating device, the pressure inside the high-pressure kettle is controlled by the heating device, and the pressure outside the high-pressure kettle is controlled by the gas circulating device, so that the pressure outside the high-pressure kettle is always greater than the pressure inside the high-pressure kettle, the high-pressure kettle is in an external pressure working condition, the safety of the high-pressure kettle is ensured, and the production efficiency is improved.
Description
Technical Field
The utility model relates to the technical field of growing materials in supercritical fluid, in particular to a heating device of a GaN single crystal growing device.
Background
The third generation semiconductor material is a wide bandgap semiconductor material represented by gallium nitride (GaN), silicon carbide (SiC), diamond, and zinc oxide, and is a hot spot in the semiconductor field of all countries in the world. Gallium nitride has unique properties of large forbidden band width, high breakdown electric field, large heat conductivity, high electron saturation drift velocity, small dielectric constant and the like, and has wide market prospect in the aspects of optoelectronic devices, power electronics, radio frequency microwave devices, lasers, detectors and the like.
Because the hot isostatic pressing container is a closed environment, but in the prior art, no convection heat dissipation exists, and the temperature difference between the autoclave raw material area and the growth area is difficult to realize.
In the prior art, chinese patent publication No. CN109930202A discloses a hot isostatic pressing apparatus suitable for ammonothermal process for producing gallium nitride single crystal products, which mainly comprises a working cylinder with a hot zone arranged therein, a gallium nitride single crystal growth container with a corresponding size and a diameter of 200-400 mm or more arranged in the hot zone, and a cooling water pump arranged outside the working cylinder and used for cooling an inner cylinder, an upper end cover, a lower end cover, an upper cooling jacket and a lower cooling jacket of the working cylinder through pipelines, and has the following disadvantages: 1. the structure of a cooling water system additionally arranged in the hot isostatic pressing container is complex, 2, the joint is easy to leak, and potential safety hazards are brought to the hot isostatic pressing container and a high-pressure autoclave for GaN single crystal growth.
In order to overcome the defects of the prior art, an apparatus which is controllable in temperature and simple in structure and is used for growing the GaN single crystal in the hot isostatic pressing container is urgently needed.
SUMMERY OF THE UTILITY MODEL
In view of the above, the present invention provides a heating device for a GaN single crystal growth device.
In order to solve the technical problem, the utility model discloses a technical scheme is: a heating device of a GaN single crystal growth device comprises a closed high-pressure autoclave and a heating device positioned outside the high-pressure autoclave, wherein the high-pressure autoclave is fixedly arranged inside a hot isostatic pressing container, a gas guide cover is arranged outside the high-pressure autoclave, and a gas circulating device is further arranged inside the hot isostatic pressing container to realize the convection circulation of gas outside the high-pressure autoclave.
The gas guide sleeve comprises a cover body with an opening at one end, and is sleeved between the hot isostatic pressing container and the high-pressure kettle.
The gas guide cover comprises a guide cover end cover and a guide cover cylinder, and a through hole is formed in the middle of the gas guide cover end cover so as to realize air circulation inside and outside the gas guide cover;
the gas guide cover is made of non-breathable heat-resistant materials such as stainless steel, high-temperature nickel alloy, molybdenum alloy or graphite.
The gas circulating devices are arranged on the inner side and the outer side of the closed side of the gas guide cover and are used for realizing the convection circulation of the air outside the high-pressure autoclave between the upper part and the lower part of the gas guide cover, so that the temperature between the hot isostatic pressing container and the high-pressure autoclave is stably controlled, and the accurate control of the axial temperature of the high-pressure autoclave is below 100 ℃.
The heating device comprises an upper resistance wire support and a lower resistance wire support which are positioned at the upper side and the lower side of the high-pressure kettle, the upper resistance wire support and the lower resistance wire support are axially arranged in a segmented manner outside the high-pressure kettle, and at least one group of heating resistance wires are fixedly arranged on the inner sides of the resistance wire supports, so that the upper part and the lower part of the high-pressure kettle are respectively heated, and the upper part and the lower part of the high-pressure kettle generate step temperature difference;
the utility model discloses a quick growth of high pressure kettle, including heating device, cauldron body, bottom resistance wire support, middle part heat insulation layer, upper portion resistance wire support, middle part heat insulation layer, cauldron body lower part heat insulation layer and the bottom heat insulation layer that is located autoclave support upper portion are equipped with the heat insulation layer by last top heat insulation layer, cauldron body upper portion heat insulation layer, middle part heat insulation layer, cauldron body lower part heat insulation layer in proper order down to the heating device upper and lower extreme for the step difference in temperature between two parts about the autoclave, and then the fast growth of ga.
The upper resistance wire support, the lower resistance wire support and the heat insulation layer are made of the same material, and the resistance wire support and the heat insulation layer are made of one of aluminum silicate, zirconium oxide, aluminum nitride or aluminum oxide products.
The inside of the high-pressure autoclave is divided into a first reaction cavity and a second reaction cavity by a partition plate with a through hole.
The first reaction cavity is internally provided with a polycrystal culture material for containing GaN monocrystal required by growth and a mineralizer for adjusting the solubility of the polycrystal culture material in a solvent, and the solvent is supercritical ammonia fluid solution.
And seed crystals for GaN single crystal growth are arranged in the second reaction cavity.
The autoclave is fixedly mounted on an autoclave holder inside the hot isostatic pressing vessel.
The internal pressure of the high-pressure kettle is controlled by the heating temperature of the heating device, the hot isostatic pressing container is filled with inert gas, and the external pressure of the high-pressure kettle is controlled by the amount of the inert gas outside the high-pressure kettle and the temperature of the convection circulation outside the high-pressure kettle by the gas circulation device, so that the external pressure of the high-pressure kettle is always greater than the internal pressure of the high-pressure kettle, and the high-pressure kettle is in an external pressure working condition.
Wherein the temperature in the hot isostatic pressing container is maintained below 100 ℃, and the difference between the pressure in the hot isostatic pressing container and the pressure in the autoclave is not more than 20 MPa.
The utility model has the advantages and positive effects that:
(1) the utility model discloses a heating device and heat insulation layer realize to making the step difference in temperature between the autoclave upper and lower two parts, and then accelerate the fast growth of gaN single crystal.
(2) The utility model discloses a heat insulation layer has avoided the outside temperature of autoclave to influence the inside temperature of autoclave.
(3) The utility model discloses a set up heating device and gas circulating device, realized through the inside pressure of heating device control autoclave, gas circulating device control autoclave outside pressure to realize that the outside pressure of autoclave is greater than the pressure in the autoclave all the time, make the autoclave be in the external pressure operating mode, guaranteed the safety of autoclave, improved production efficiency.
Drawings
FIG. 1 is an overall configuration diagram of a heating apparatus of a GaN single crystal growing apparatus according to the present invention;
FIG. 2 is a schematic view showing the internal structure of a hot isostatic pressing container of a heating apparatus of a GaN single crystal growth apparatus according to the present invention;
FIG. 3 is a schematic view showing the gas circulation direction of the gas circulation device of the heating device of the GaN single crystal growth device of the present invention;
in the figure:
1, a hot isostatic pressing container 101, an autoclave bracket 102, an autoclave 1021, a first reaction chamber 1022, a clapboard 1023 and a second reaction chamber;
2, a heating device 201, an upper resistance wire support 202, a lower resistance wire support 203, a heating resistance wire 204, a polycrystalline culture material 205, a seed crystal 206, a heat insulating layer 2061, a top heat insulating layer 2062, an upper heat insulating layer 2063, a middle heat insulating layer 2064, a lower heat insulating layer 2065 and a bottom heat insulating layer;
3, a gas circulating device 301, a gas guide cover 302, a guide cover end cover 303, a guide cover cylinder 304, a through hole 305, an internal circulating device 306, a motor 307, a fan 308, an external circulating device 309, a gas circulating compressor 310, a gas inlet pipe 311, a gas outlet pipe 312, a gas inlet hole 313 and a gas outlet hole.
Detailed Description
As shown in fig. 1 to fig. 3, the present invention provides a heating device of GaN single crystal growth apparatus, comprising a closed autoclave 102 and a heating device 2 located outside the autoclave 102, wherein the autoclave 102 is fixedly installed inside a hot isostatic pressing container 1, a gas guiding hood 301 is arranged outside the autoclave 102, and a gas circulation device 3 is further arranged inside the hot isostatic pressing container 1 to realize convection circulation of gas outside the autoclave 102.
The gas guiding hood 301 comprises a hood body with an open end, and is sleeved between the hot isostatic pressing container 1 and the autoclave 102.
The gas guide sleeve 301 comprises a guide sleeve end cover 302 and a guide sleeve cylinder 303, and a through hole 304 is formed in the middle of the end cover 302 of the gas guide sleeve 301 to realize air circulation inside and outside the gas guide sleeve 301;
the gas guide sleeve 301 is made of non-gas-permeable heat-resistant materials such as stainless steel, high-temperature nickel alloy, molybdenum alloy or graphite.
In a specific embodiment, during the operation of the gas circulation device 3, the air inside and outside the gas guide sleeve 301 realizes the convection circulation of the air inside and outside the gas guide sleeve 301 through the lower opening of the gas guide sleeve 301 and the through hole 304 in the middle of the guide sleeve end cover 302.
The heating device 2 comprises an upper resistance wire support 201 and a lower resistance wire support 202 which are positioned at the upper side and the lower side of the autoclave 102, the upper resistance wire support 201 and the lower resistance wire support 202 are axially arranged in a segmented manner at the outer side of the autoclave 102, and at least one group of heating resistance wires 203 are fixedly arranged at the inner sides of the resistance wire supports, so that the upper part and the lower part of the autoclave 102 are respectively heated, and the upper part and the lower part of the autoclave 102 generate step temperature difference;
the autoclave 102 is fixedly mounted on the autoclave holder 101 inside the hot isostatic pressing vessel 1, and the inside of the autoclave 102 is divided into a first reaction chamber 1021 and a second reaction chamber 1023 by a partition 1022 having a through hole 304.
The first reaction cavity 1021 is internally provided with a polycrystalline culture material 204 for containing GaN single crystal required for growth and a mineralizer for adjusting the solubility of the polycrystalline culture material 204 in a solvent, and the solvent is supercritical ammonia fluid solution.
A seed crystal 205 for GaN single crystal growth is arranged in the second reaction chamber 1023.
In a specific embodiment, the upper heating resistance wire 203 and the lower heating resistance wire 203 respectively heat the first reaction chamber 1021 and the second reaction chamber 1023, so that a step temperature difference is generated between the first reaction chamber 1021 and the second reaction chamber 1023, the solvent in the autoclave 102 is promoted to generate convection flow in the autoclave, and at this time, the ammonia solvent in the autoclave 102 is in a supercritical state, so as to accelerate the rapid growth of the GaN single crystal on the seed crystal 205 in a supercritical environment.
Further, the upper end and the lower end of the heating device 2 are provided with heat insulating layers 206 for preventing the external temperature from influencing the internal temperature of the autoclave 102, the heat insulating layers 206 sequentially comprise a top heat insulating layer 2061, an upper heat insulating layer 2062, a middle heat insulating layer 2063, a lower heat insulating layer 2064 and a bottom heat insulating layer 2065 positioned at the upper part of the autoclave holder 101 from top to bottom, wherein the middle heat insulating layer 2063 is arranged between the upper resistance wire holder 201 and the lower resistance wire holder 202, so that the step temperature difference between the upper part and the lower part of the autoclave 102 is realized, and the rapid growth of the GaN single crystal is accelerated.
The upper and lower resistance wire brackets 201, 202 and the heat insulating layer 206 are made of the same material, and the resistance wire brackets and the heat insulating layer 206 are made of one of aluminum silicate, zirconium oxide, aluminum nitride or aluminum oxide products.
In a specific embodiment, during the operation of the heating device 2, the heat insulating layer 206 maintains the internal temperature of the autoclave 102, wherein the middle heat insulating layer 2063 separates the upper heating resistance wire 203 from the lower heating resistance wire 203, so that the temperatures of the first reaction chamber 1021 and the second reaction chamber 1023 are not interfered with each other, and a step temperature difference is generated between the first reaction chamber 1021 and the second reaction chamber 1023, thereby accelerating the rapid growth of the GaN single crystal in the crystallization area.
Further, the gas circulation device 3 realizes convection circulation of the gas inside and outside the gas guide sleeve 301, so that the temperature of the temperature difference between the upper part and the lower part of the autoclave 102 is stably controlled, the axial temperature of the autoclave 102 is accurately controlled below 100 ℃, the safety of the autoclave 102 is ensured, and the production efficiency is improved.
Further, in a specific embodiment, the gas circulation device 3 includes:
the air inlet end and the air outlet end of the outer circulation device 308 are respectively arranged on the inner side and the outer side of the gas guide sleeve 301 and are communicated with the outside of the hot isostatic pressing container 1, the air inlet end and the air outlet end of the outer circulation device 308 are respectively provided with a plurality of air inlet holes 312 and a plurality of air outlet holes 313, and the air inlet end and the air outlet end of the outer circulation device 308 are both communicated with a gas circulation compressor 309 arranged on the outside of the hot isostatic pressing container 1 through gas pipelines;
in a specific embodiment of the present invention, the outer circulation device 308 transmits the air outside the gas guiding cover 301 to the gas circulation compressor 309 through the air inlet 312 and the air inlet pipe 310 at the air inlet end, and the air inside the gas circulation compressor 309 is discharged to the inside of the gas guiding cover 301 through the air outlet 313 and the air outlet 311 at the air outlet end, so as to realize the heat exchange between the inside of the hot isostatic pressing container 1 and the outside of the hot isostatic pressing container 1, thereby stably controlling the temperature inside the hot isostatic pressing container 1, and accelerating the growth of the GaN single crystal in the second reaction chamber 1023.
Further, the internal circulation device 305 is arranged inside the gas guide sleeve 301, and drives the gas inside the gas guide sleeve 301 to exchange the gas inside and outside the gas guide sleeve 301, the internal circulation device 305 includes a motor 306 fixedly arranged at the top inside the hot isostatic pressing container 1, and an output end of the motor 306 passes through the through hole 304 and is connected with a fan 307 arranged inside the gas guide sleeve 301, so as to control the flow direction of the air inside the gas guide sleeve 301.
In a specific embodiment, the fan 307 of the internal circulation device 305 blows air inside the gas guide sleeve 301 to the lower part of the gas guide sleeve 301, so as to be discharged to the outside of the gas guide sleeve 301, and meanwhile, due to the internal sealing of the hot isostatic pressing container 1, air above the outside of the gas guide sleeve 301 enters the inside of the gas guide sleeve 301 along with the through hole 304 in the middle of the end cover 302 of the guide sleeve, so that the air at the lower part of the outside of the gas guide sleeve 301 moves to the upper part, and the convection circulation inside and outside the gas guide sleeve 301 is formed.
The pressure inside the autoclave 102 is controlled by the heating temperature of the heating device 2, the hot isostatic pressing container 1 is filled with inert gas, the pressure outside the autoclave 102 is controlled by the amount of the inert gas outside the autoclave 102 and the temperature of the convection circulation outside the autoclave 102 by the gas circulation device 3, so that the pressure outside the autoclave 102 is always greater than the pressure inside the autoclave 102, and the autoclave 102 is under the external pressure condition.
Wherein the temperature in the hot isostatic pressing container 1 is maintained below 100 ℃, and the difference between the pressure in the hot isostatic pressing container 1 and the pressure in the autoclave 102 is not more than 20 MPa.
The utility model discloses a theory of operation and working process as follows: the upper heating resistance wire 203 and the lower heating resistance wire 203 respectively heat the first reaction cavity 1021 and the second reaction cavity 1023, so that a step temperature difference is generated between the first reaction cavity 1021 and the second reaction cavity 1023, the solvent in the high-pressure kettle 102 is promoted to generate convection flow in the kettle, and at the moment, the ammonia solvent in the high-pressure kettle 102 is in a supercritical state, so that the rapid growth of the GaN single crystal on the seed crystal 205 in a supercritical environment is accelerated.
The motor 306 drives the fan 307 to rotate, air inside the gas guide sleeve 301 is blown to the lower portion of the gas guide sleeve 301 and is discharged to the outer side of the gas guide sleeve 301, meanwhile, the fan 307 of the internal circulation device 305 blows air above the outer portion of the gas guide sleeve 301 into the gas guide sleeve 301 from the through hole 304 in the middle of the guide sleeve end cover 302, so that the air at the lower portion of the outer side of the gas guide sleeve 301 moves towards the upper portion, and convection circulation of the air inside and outside the gas guide sleeve 301 is formed;
the air outside the gas guide sleeve 301 is transmitted into the gas circulation compressor 309 through the air inlet hole 312 and the air inlet pipe 310 at the air inlet end by the gas circulation compressor 309, the air inside the gas circulation compressor 309 is discharged into the gas guide sleeve 301 through the air outlet hole 313 and the air outlet pipe 311 at the air outlet end, so that heat exchange between the inside of the hot isostatic pressing container 1 and the outside of the hot isostatic pressing container 1 is realized, the temperature inside the hot isostatic pressing container 1 is further reduced, the accurate control of the axial temperature of the high-pressure autoclave 102 below 100 ℃ is realized, the safety of the high-pressure autoclave 102 is ensured, and the production efficiency is improved.
The utility model is characterized in that: the heating device 2 is arranged, so that the step temperature difference between the upper part and the lower part of the high-pressure kettle 102 is realized, and the rapid growth of the GaN single crystal is accelerated; by arranging the heat insulating layer 206, the influence of the external temperature of the autoclave 102 on the internal temperature of the autoclave 102 is avoided; by arranging the heating device 2 and the gas circulating device 3, the internal pressure of the high-pressure kettle 102 is controlled by the heating device 2, and the external pressure of the high-pressure kettle 102 is controlled by the gas circulating device 3, so that the external pressure of the high-pressure kettle 102 is always greater than the internal pressure of the high-pressure kettle 102, the high-pressure kettle 102 is under the external pressure working condition, the safety of the high-pressure kettle 102 is ensured, and the production efficiency is improved.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention should be covered by the present patent.
Claims (10)
1. The heating device of the GaN single crystal growing device is characterized by comprising a closed high-pressure kettle (102) and a heating device (2) positioned outside the high-pressure kettle (102), wherein the high-pressure kettle (102) is fixedly arranged inside a hot isostatic pressing container (1), a gas guide cover (301) is arranged outside the high-pressure kettle (102), and a gas circulating device (3) is further arranged inside the hot isostatic pressing container (1) so as to realize the convection circulation of gas outside the high-pressure kettle (102).
2. The heating apparatus for a GaN single crystal growth apparatus according to claim 1, wherein the gas guiding enclosure (301) comprises an enclosure with an open end, which is placed between the hot isostatic pressing vessel (1) and the autoclave (102).
3. The heating apparatus for a GaN single crystal growth apparatus according to claim 1, wherein the gas circulation means (3) is provided inside and outside the closed side of the gas dome (301) for realizing convection circulation of the air outside the autoclave (102) between the upper and lower parts of the gas dome (301).
4. The heating device of the GaN single crystal growing device according to claim 1, wherein the heating device (2) comprises an upper resistance wire support (201) and a lower resistance wire support (202) which are located at the upper side and the lower side of the autoclave (102), and the upper resistance wire support (201) and the lower resistance wire support (202) are axially arranged in a segmented manner outside the autoclave (102).
5. The heating device of the GaN single crystal growing device of claim 4, wherein at least one group of heating resistance wires (203) are fixedly arranged on the inner sides of the resistance wire supports, so as to respectively heat the upper part and the lower part of the autoclave (102) and enable the upper part and the lower part of the autoclave (102) to generate a step temperature difference, and the heating device (2) realizes the control of the internal pressure of the autoclave (102).
6. The heating device of GaN single crystal growing device of claim 4, wherein the upper and lower ends of the heating device (2) are provided with heat insulating layers (206) for preventing the influence of the external temperature on the internal temperature of the autoclave (102), wherein a middle heat insulating layer (2063) is provided between the upper resistance wire support (201) and the lower resistance wire support (202) to make the temperature step difference between the upper and lower parts of the autoclave (102) to accelerate the rapid growth of GaN single crystal.
7. The heating device of a GaN single crystal growing device of claim 4, wherein the upper (201) and lower (202) resistance wire supports and the insulating layer (206) are the same material.
8. The heating apparatus for a GaN single crystal growth apparatus according to claim 1, wherein the inside of the autoclave (102) is divided into a first reaction chamber (1021) and a second reaction chamber (1023) by a partition (1022) having a through-hole (304).
9. The heating device of the GaN single crystal growing device of claim 8, wherein a polycrystal culture material (204) for containing GaN single crystal required for growing and a mineralizer for adjusting the solubility of the polycrystal culture material (204) in a solvent are arranged in the first reaction chamber (1021).
10. The heating apparatus of a GaN single crystal growing apparatus according to claim 8, wherein a seed crystal (205) for GaN single crystal growth is provided in the second reaction chamber (1023).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020789389.3U CN212476953U (en) | 2020-05-13 | 2020-05-13 | Heating device of GaN single crystal growth device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020789389.3U CN212476953U (en) | 2020-05-13 | 2020-05-13 | Heating device of GaN single crystal growth device |
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| CN212476953U true CN212476953U (en) | 2021-02-05 |
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| CN202020789389.3U Active CN212476953U (en) | 2020-05-13 | 2020-05-13 | Heating device of GaN single crystal growth device |
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