CN116892056A - Thermal insulation structure for silicon carbide single crystal growth and manufacturing method and application thereof - Google Patents
Thermal insulation structure for silicon carbide single crystal growth and manufacturing method and application thereof Download PDFInfo
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- CN116892056A CN116892056A CN202310991407.4A CN202310991407A CN116892056A CN 116892056 A CN116892056 A CN 116892056A CN 202310991407 A CN202310991407 A CN 202310991407A CN 116892056 A CN116892056 A CN 116892056A
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- 238000009413 insulation Methods 0.000 title claims abstract description 87
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 65
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000002109 crystal growth method Methods 0.000 title description 2
- 238000004321 preservation Methods 0.000 claims abstract description 88
- 239000013078 crystal Substances 0.000 claims abstract description 66
- 238000004804 winding Methods 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 75
- 229910002804 graphite Inorganic materials 0.000 claims description 74
- 239000010439 graphite Substances 0.000 claims description 74
- 239000004744 fabric Substances 0.000 claims description 26
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 13
- 239000004917 carbon fiber Substances 0.000 claims description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 6
- 238000005096 rolling process Methods 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229920000297 Rayon Polymers 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000002035 prolonged effect Effects 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 229910021384 soft carbon Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- C30B29/36—Carbides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a thermal insulation structure for silicon carbide single crystal growth, a manufacturing method and application thereof, wherein the thermal insulation structure comprises a side thermal insulation unit, a top thermal insulation unit and a bottom thermal insulation unit which are surrounded outside a silicon carbide single crystal growth device; the side heat preservation unit is formed by winding a rectangular heat preservation strip, and two connecting end parts of the rectangular heat preservation strip are respectively and independently provided with a slope structure, wherein the slope structure comprises an outer end slope and an inner end slope; the outer end slope is positioned at the connecting end part far away from the silicon carbide single crystal growing device, and the inner end slope is positioned at the connecting end part close to the silicon carbide single crystal growing device; setting the hypotenuse length of the outer end slope to be L1, and setting the hypotenuse length of the inner end slope to be L2, the heat insulation structure meets the following conditions: l1> L2. The heat insulation structure provided by the invention improves the heat insulation performance and the heat insulation uniformity, prolongs the service life, improves the crystal quality, reduces the manufacturing cost and is beneficial to large-scale popularization and application.
Description
Technical Field
The invention belongs to the technical field of semiconductor preparation, relates to a heat preservation structure, and in particular relates to a heat preservation structure for silicon carbide single crystal growth, and a manufacturing method and application thereof.
Background
Silicon carbide (SiC) is a third-generation semiconductor material with wide forbidden band, high critical electric field and high saturation mobility, has great advantages in power devices, and is widely applied to various fields of new energy automobiles, photovoltaic power generation, railway traffic, power systems and the like.
Because the physical and chemical properties of SiC are extremely stable, making the growth of SiC crystals extremely difficult, the requirements on the temperature and insulation structure of single crystal growth equipment are also very stringent. At present, a main stream of single crystal growth equipment heat preservation parts are graphite carbon felts, wherein the soft carbon felts are one of common heat preservation materials, and the manufacturing process of the soft carbon felt heat preservation layer, the heat conductivity and the heat preservation uniformity of the heat preservation layer have obvious influence on the radial uniformity, the axial gradient control and the energy consumption of a growth temperature field.
The conventional manufacturing method of the soft carbon felt heat insulation structure is to manually wind the carbon felt with the same specification in a concentric core winding way and match with a graphite felt for up-and-down covering. The operation mode has poor control on the tightness degree and the thermal conductivity uniformity of the heat-insulating structure, the SiC monocrystal is mainly prepared by a Physical Vapor Transport (PVT) method at present, silicon-containing gas is generated in the growth process, the silicon-containing gas is easy to deposit and react in gaps of the heat-insulating structure, the heat-insulating structure is easily layered, embrittled, pulverized and the like, the heat-insulating property and the heat-insulating uniformity are accordingly reduced, the service life is prolonged, the crystal quality and the manufacturing cost are further affected, the influence has unrepeatability in the technological process, and great difficulty is brought to the improvement of the crystal quality.
Therefore, how to provide a thermal insulation structure for silicon carbide single crystal growth and a manufacturing method thereof, which improve the thermal insulation performance and the thermal insulation uniformity, prolong the service life, improve the crystal quality, and reduce the manufacturing cost at the same time, is an urgent problem to be solved by the current technicians in the field.
Disclosure of Invention
The invention aims to provide a thermal insulation structure for silicon carbide single crystal growth, and a manufacturing method and application thereof.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a thermal insulation structure for silicon carbide single crystal growth, the thermal insulation structure comprising a side thermal insulation unit, a top thermal insulation unit, and a bottom thermal insulation unit surrounding an exterior of a silicon carbide single crystal growth apparatus.
The side heat preservation unit is formed by winding a rectangular heat preservation strip, and two connecting end parts of the rectangular heat preservation strip are respectively and independently provided with a slope structure, and the slope structure comprises an outer end slope and an inner end slope.
The outer end slope is located at a connection end far from the silicon carbide single crystal growth device, and the inner end slope is located at a connection end near the silicon carbide single crystal growth device.
Setting the hypotenuse length of the outer end slope to be L1, and setting the hypotenuse length of the inner end slope to be L2, the heat insulation structure meets the following conditions: l1> L2.
Compared with the traditional heat-insulating structure with only side heat-insulating units, the heat-insulating structure provided by the invention has the advantages that the side heat-insulating units, the top heat-insulating unit and the bottom heat-insulating unit which are matched with each other wrap the silicon carbide single crystal growing device in an omnibearing manner, so that the heat-insulating performance and the heat-insulating uniformity are obviously improved, and the growth quality of the silicon carbide single crystal is improved.
In addition, the slope structure is arranged at the connecting end part of the side heat preservation unit, so that the gap between the heat preservation unit and the silicon carbide single crystal growing device is reduced, the consistency of heat preservation performance is ensured, and meanwhile, the phenomena of layering, embrittlement, pulverization and the like of the heat preservation structure caused by deposition reaction of silicon-containing gas in the gap of the heat preservation structure are avoided, so that the service life of the heat preservation structure is prolonged.
Further, the invention ensures that the thick edge of the outer end slope and the thick edge of the inner end slope and the thick edge of the outer end slope and the thin edge of the inner end slope are mutually overlapped in the radial direction by controlling the length of the inclined edge of the outer end slope to be larger than the length of the inclined edge of the inner end slope, thereby meeting the thickness consistency of the side heat preservation unit in the circumferential direction and improving the heat insulation performance and the heat preservation uniformity to the greatest extent.
Preferably, the material of the thermal insulation structure comprises a graphite soft felt, and the graphite soft felt comprises an adhesive-based graphite soft felt or a polyacrylonitrile-based graphite soft felt.
Preferably, the thickness of the graphite soft felt is 2-20mm, for example, 2mm, 4mm, 6mm, 8mm, 10mm, 12mm, 14mm, 16mm, 18mm or 20mm, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the density of the graphite soft felt is 0.8-1.3g/cm 3 For example, it may be 0.8g/cm 3 、0.85g/cm 3 、0.9g/cm 3 、0.95g/cm 3 、1g/cm 3 、1.05g/cm 3 、1.1g/cm 3 、1.15g/cm 3 、1.2g/cm 3 、1.25g/cm 3 Or 1.3g/cm 3 But are not limited to, the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the ash content of the graphite soft felt is less than or equal to 50ppm, and for example, 5ppm, 10ppm, 15ppm, 20ppm, 25ppm, 30ppm, 35ppm, 40ppm, 45ppm or 50ppm can be used, but the ash content is not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
Preferably, the material of the thermal insulation structure comprises graphite soft felt and auxiliary sheets which are alternately laminated.
Preferably, the auxiliary sheet layer comprises any one or a combination of at least two of graphite paper, graphite cloth or carbon fiber cloth, and typical but non-limiting combinations include a combination of graphite paper and graphite cloth, a combination of graphite cloth and carbon fiber cloth, a combination of graphite paper and carbon fiber cloth, or a combination of graphite paper, graphite cloth and carbon fiber cloth.
Preferably, the thickness of the auxiliary sheet is 0.1 to 1mm, for example, 0.1mm, 0.2mm, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm or 1mm, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the ash content of the auxiliary sheet is less than or equal to 100ppm, and may be, for example, 10ppm, 20ppm, 30ppm, 40ppm, 50ppm, 60ppm, 70ppm, 80ppm, 90ppm, or 100ppm, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the thickness of the side thermal insulation unit is 20-150mm, for example, 20mm, 30mm, 40mm, 50mm, 60mm, 70mm, 80mm, 90mm, 100mm, 110mm, 120mm, 130mm, 140mm or 150mm, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the side heat insulating unit is divided into an outer heat insulating member and an inner heat insulating member.
Preferably, the thickness of the outer layer heat-insulating member is 10-40mm, for example, 10mm, 15mm, 20mm, 25mm, 30mm, 35mm or 40mm, but not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the thickness of the inner layer insulation member is 10-110mm, for example, 10mm, 20mm, 30mm, 40mm, 50mm, 60mm, 70mm, 80mm, 90mm, 100mm or 110mm, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the height of the outer layer heat-insulating member is set to H1, and the height of the inner layer heat-insulating member is set to H2, then the side heat-insulating unit satisfies: 10 mm.ltoreq.H 1-H2.ltoreq.50 mm, for example, H1-H2=10 mm, 15mm, 20mm, 25mm, 30mm, 35mm, 40mm, 45mm or 50mm, but not limited to the values recited, other values not recited in the range of values being equally applicable.
Preferably, a graphite soft felt ring is transversely paved at the top of the inner-layer heat-insulating part, the inner diameter of the graphite soft felt ring is consistent with the inner diameter of the inner-layer heat-insulating part, and the outer diameter of the graphite soft felt ring is consistent with the outer diameter of the inner-layer heat-insulating part.
Preferably, the graphite felt ring has a thickness of 10-50mm, for example, 10mm, 15mm, 20mm, 25mm, 30mm, 35mm, 40mm, 45mm or 50mm, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the length of the hypotenuse of the ramp structure is 50-300mm, for example, 50mm, 60mm, 80mm, 100mm, 120mm, 140mm, 160mm, 180mm, 200mm, 220mm, 240mm, 260mm, 280mm or 300mm, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the included angle between the oblique side and the right-angle side of the slope structure is 1-15 °, for example, 1 °, 2 °, 3 °, 4 °, 5 °, 6 °, 7 °, 8 °, 9 °, 10 °, 11 °, 12 °, 13 °, 14 ° or 15 °, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the difference between the hypotenuse length L1 of the outer end ramp and the hypotenuse length L2 of the inner end ramp satisfies: 0mm < (L1-L2) < 200mm, for example, L1-L2=1 mm, 10mm, 20mm, 40mm, 60mm, 80mm, 100mm, 120mm, 140mm, 160mm, 180mm or 200mm, but not limited to the values listed, the other non-listed values within the range of values are equally applicable.
Preferably, the top and bottom insulation units each independently comprise a circular insulation sheet.
Preferably, the diameter of the circular heat-insulating sheet is consistent with the outer diameter of the silicon carbide single crystal growth device.
In a second aspect, the present invention provides a method for manufacturing the insulation structure according to the first aspect, the method comprising the steps of:
(1) Selecting a rectangular heat preservation bar suitable for the height of a silicon carbide single crystal growing device, and correspondingly cutting an outer end slope and an inner end slope at two connecting ends of the rectangular heat preservation bar respectively;
(2) And winding the rectangular heat preservation strip to obtain a side heat preservation unit, and combining the cut top heat preservation unit and the cut bottom heat preservation unit to obtain the heat preservation structure for silicon carbide single crystal growth.
Preferably, the rectangular heat-insulating strip in the step (1) is made of graphite soft felt.
Preferably, in the step (2), an auxiliary sheet layer is further attached to the rectangular heat-insulating strip in the winding process, and the auxiliary sheet layer includes any one or a combination of at least two of graphite paper, graphite cloth or carbon fiber cloth, and typical but non-limiting combinations include a combination of graphite paper and graphite cloth, a combination of graphite cloth and carbon fiber cloth, a combination of graphite paper and carbon fiber cloth, or a combination of graphite paper, graphite cloth and carbon fiber cloth.
Preferably, the winding process in step (2) is performed in a felt rolling machine, and the felt rolling tension is 1-100N, for example, 1N, 10N, 20N, 30N, 40N, 50N, 60N, 70N, 80N, 90N or 100N, but not limited to the recited values, and other non-recited values within the range are equally applicable.
In a third aspect, the present invention provides the use of an insulating structure as described in the first aspect for surrounding a silicon carbide single crystal growth apparatus, the silicon carbide single crystal growth apparatus comprising a crucible or a heating element.
Compared with the prior art, the invention has the following beneficial effects:
(1) Compared with the traditional heat-insulating structure with only side heat-insulating units, the heat-insulating structure provided by the invention has the advantages that the side heat-insulating units, the top heat-insulating unit and the bottom heat-insulating unit which are matched with each other wrap the silicon carbide single crystal growing device in an omnibearing manner, so that the heat-insulating performance and heat-insulating uniformity are obviously improved, and the growth quality of the silicon carbide single crystal is improved;
(2) According to the invention, the slope structure is arranged at the connecting end part of the side heat-insulating unit, so that the gap between the heat-insulating unit and the silicon carbide single crystal growing device is reduced, the consistency of heat-insulating performance is ensured, and the phenomena of layering, embrittlement, pulverization and the like of the heat-insulating structure caused by deposition reaction of silicon-containing gas in the gap of the heat-insulating structure are avoided, thereby prolonging the service life of the heat-insulating structure;
(3) According to the invention, by controlling the length of the inclined edge of the outer end slope to be larger than that of the inclined edge of the inner end slope, the thick edge of the outer end slope and the thick edge of the inner end slope are ensured to be mutually overlapped in the radial direction, so that the thickness consistency of the side heat preservation unit in the circumferential direction is met, and the heat insulation performance and the heat preservation uniformity are improved to the greatest extent.
Drawings
Fig. 1 is a schematic view of a thermal insulation structure provided by the invention.
Wherein: 10-a side thermal insulation unit; 11-an outer layer heat preservation part; 12-an inner layer heat preservation component; 20-a top insulation unit; 30-a bottom insulation unit; 40-graphite soft felt ring; a 50-silicon carbide single crystal growth apparatus; 60-induction coil.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
The present invention provides a thermal insulation structure for silicon carbide single crystal growth, which comprises a side thermal insulation unit 10, a top thermal insulation unit 20 and a bottom thermal insulation unit 30, which are surrounded on the outside of a silicon carbide single crystal growth apparatus 50, as shown in fig. 1. The side heat-insulating unit 10 is formed by winding a rectangular heat-insulating strip, and two connecting end parts of the rectangular heat-insulating strip are respectively and independently provided with a slope structure, wherein the slope structure comprises an outer end slope and an inner end slope; the outer end slope is located at a connection end portion distant from the silicon carbide single crystal growth apparatus 50, and the inner end slope is located at a connection end portion close to the silicon carbide single crystal growth apparatus 50; setting the hypotenuse length of the outer end slope to be L1, and setting the hypotenuse length of the inner end slope to be L2, the heat insulation structure meets the following conditions: l1> L2.
In the invention, the material of the heat insulation structure comprises a graphite soft felt and an auxiliary sheet layer which are alternately laminated, and the graphite soft felt comprises a viscose-based graphite soft felt or a polyacrylonitrile-based graphite soft felt; the auxiliary sheet layer comprises any one or a combination of at least two of graphite paper, graphite cloth or carbon fiber cloth; the thickness of the graphite soft felt is 2-20mm, and the density is 0.8-1.3g/cm 3 Ash content less than or equal to 50ppm; the thickness of the auxiliary sheet layer is 0.1-1mm, and ash content is less than or equal to 100ppm.
In the invention, the thickness of the side heat preservation unit 10 is 20-150mm; the side heat preservation unit 10 is divided into an outer heat preservation part 11 and an inner heat preservation part 12, wherein the thickness of the outer heat preservation part 11 is 10-40mm, and the thickness of the inner heat preservation part 12 is 10-110mm; setting the height of the outer layer heat-insulating member 11 to be H1 and the height of the inner layer heat-insulating member 12 to be H2, the side heat-insulating unit 10 satisfies: the thickness of H1-H2 is less than or equal to 10mm and less than or equal to 50mm.
In the invention, a graphite soft felt ring 40 is transversely paved on the top of the inner-layer heat-insulating part 12, the inner diameter of the graphite soft felt ring 40 is consistent with the inner diameter of the inner-layer heat-insulating part 12, and the outer diameter of the graphite soft felt ring 40 is consistent with the outer diameter of the inner-layer heat-insulating part 12; the graphite felt ring 40 has a thickness of 10-50mm.
In the invention, the length of the inclined edge of the slope structure is 50-300mm, and the included angle between the inclined edge and the right-angle edge is 1-15 degrees; the difference between the hypotenuse length L1 of the outer end slope and the hypotenuse length L2 of the inner end slope satisfies the following conditions: the diameter of the L1-L2 is less than or equal to 0mm and less than or equal to 200mm. The top thermal insulation unit 20 and the bottom thermal insulation unit 30 each independently include a circular thermal insulation sheet, and the diameter of the circular thermal insulation sheet is identical to the outer diameter of the silicon carbide single crystal growth apparatus 50.
In addition, the invention also provides a manufacturing method of the heat insulation structure, which comprises the following steps:
(1) Selecting a rectangular heat preservation bar suitable for the height of the silicon carbide single crystal growing device 50, and correspondingly cutting an outer end slope and an inner end slope at two connecting ends of the rectangular heat preservation bar respectively; the rectangular heat preservation strip is made of graphite soft felt;
(2) And (3) attaching the rectangular heat preservation strip to an auxiliary sheet layer, wherein the auxiliary sheet layer comprises any one or a combination of at least two of graphite paper, graphite cloth or carbon fiber cloth, winding the graphite paper, the graphite cloth or the carbon fiber cloth in a felt rolling machine with the felt rolling tension of 1-100N to obtain a side heat preservation unit 10, and combining the cut top heat preservation unit 20 and the cut bottom heat preservation unit 30 to obtain the heat preservation structure for the growth of the silicon carbide single crystal.
The heat-insulating structure provided by the invention is used for surrounding the silicon carbide single crystal growth device 50, and the silicon carbide single crystal growth device 50 comprises a crucible or a heating body (such as an induction coil 60).
Compared with the traditional heat-insulating structure with only side heat-insulating units, the heat-insulating structure provided by the invention has the advantages that the side heat-insulating units, the top heat-insulating unit and the bottom heat-insulating unit which are matched with each other wrap the silicon carbide single crystal growing device in an omnibearing manner, so that the heat-insulating performance and the heat-insulating uniformity are obviously improved, and the growth quality of the silicon carbide single crystal is improved.
In addition, the slope structure is arranged at the connecting end part of the side heat preservation unit, so that the gap between the heat preservation unit and the silicon carbide single crystal growing device is reduced, the consistency of heat preservation performance is ensured, and meanwhile, the phenomena of layering, embrittlement, pulverization and the like of the heat preservation structure caused by deposition reaction of silicon-containing gas in the gap of the heat preservation structure are avoided, so that the service life of the heat preservation structure is prolonged.
Further, the invention ensures that the thick edge of the outer end slope and the thick edge of the inner end slope and the thick edge of the outer end slope and the thin edge of the inner end slope are mutually overlapped in the radial direction by controlling the length of the inclined edge of the outer end slope to be larger than the length of the inclined edge of the inner end slope, thereby meeting the thickness consistency of the side heat preservation unit in the circumferential direction and improving the heat insulation performance and the heat preservation uniformity to the greatest extent.
Example 1
The present embodiment provides a thermal insulation structure for silicon carbide single crystal growth, which includes a side thermal insulation unit 10, a top thermal insulation unit 20, and a bottom thermal insulation unit 30, which surround the outside of a silicon carbide single crystal growth apparatus 50, as shown in fig. 1. The side heat-insulating unit 10 is formed by winding a rectangular heat-insulating strip, two connecting end parts of the rectangular heat-insulating strip are respectively and independently provided with a slope structure, the slope structure comprises an outer end slope and an inner end slope, and an included angle between the inclined side of the slope structure and the right-angle side is 8 degrees; the outer end slope is located at a connection end portion distant from the silicon carbide single crystal growth apparatus 50, and the inner end slope is located at a connection end portion close to the silicon carbide single crystal growth apparatus 50; the length of the inclined edge of the outer end slope is 200mm, and the length of the inclined edge of the inner end slope is 175mm.
In this embodiment, the heat insulation structure is made of alternate laminated polyacrylonitrile-based graphite soft felt and graphite paper; the thickness of the polyacrylonitrile-based graphite soft felt is 10mm, and the density is 1.0g/cm 3 Ash content 40ppm; the thickness of the graphite paper is 0.5mm, and the ash content is 80ppm.
In this embodiment, the thickness of the side thermal insulation unit 10 is 85mm; the side heat-insulating unit 10 is divided into an outer heat-insulating part 11 and an inner heat-insulating part 12, wherein the thickness of the outer heat-insulating part 11 is 25mm, and the thickness of the inner heat-insulating part 12 is 60mm; setting the height of the outer layer heat-insulating member 11 to be H1 and the height of the inner layer heat-insulating member 12 to be H2, the side heat-insulating unit 10 satisfies: h1-h2=20 mm.
In this embodiment, a graphite flexible felt ring 40 is transversely laid on top of the inner layer heat insulation member 12, and the inner diameter of the graphite flexible felt ring 40 is consistent with the inner diameter of the inner layer heat insulation member 12, and the outer diameter of the graphite flexible felt ring 40 is consistent with the outer diameter of the inner layer heat insulation member 12; the graphite felt ring 40 has a thickness of 30mm.
In this embodiment, the top thermal insulation unit 20 and the bottom thermal insulation unit 30 each independently include a circular thermal insulation sheet, and the diameter of the circular thermal insulation sheet is consistent with the outer diameter of the silicon carbide single crystal growth apparatus 50.
Example 2
The embodiment provides a method for manufacturing a heat insulation structure as described in embodiment 1, the method comprises the following steps:
(1) Selecting a rectangular heat preservation bar suitable for the height of the silicon carbide single crystal growing device 50, and correspondingly cutting an outer end slope and an inner end slope at two connecting ends of the rectangular heat preservation bar respectively; the rectangular heat-insulating strip is made of polyacrylonitrile-based graphite soft felt;
(2) And (3) attaching the rectangular heat preservation strips to graphite paper, winding the graphite paper in a felt winding machine under the felt winding tension of 50N to obtain a side heat preservation unit 10, and combining the cut top heat preservation unit 20 and bottom heat preservation unit 30 to obtain the heat preservation structure for silicon carbide monocrystal growth.
Comparative example 1
The comparative example provides a thermal insulation structure for silicon carbide single crystal growth, and the other structures and conditions are the same as those of example 1 except that the length of the hypotenuse of the inner end slope is changed to 200mm, so that the description thereof will not be repeated here.
Compared with the embodiment 1, the comparative example changes the length of the inclined edge of the inner end slope to be consistent with that of the outer end slope, so that the thick edge of the outer end slope and the thick edge of the inner end slope and the thick edge of the outer end slope and the thin edge of the inner end slope cannot be completely overlapped in the radial direction, the thickness consistency of the side heat preservation unit in the circumferential direction is lower than that of the embodiment 1, and the heat insulation performance and the heat preservation uniformity of the heat preservation structure are further reduced.
Comparative example 2
The comparative example provides a heat-insulating structure for silicon carbide single crystal growth, and the other structures and conditions are the same as those of example 1 except that the slope structure of the connecting end part of the rectangular heat-insulating strip is changed to a conventional flat end surface, so that the description thereof is omitted.
Compared with the embodiment 1, the slope structure is not arranged at the connecting end part of the side heat preservation unit in the comparative example, so that an obvious gap exists between the heat preservation unit and the silicon carbide single crystal growing device, the consistency of heat preservation performance is reduced, and the silicon-containing gas is easy to generate deposition reaction in the gap of the heat preservation structure, so that the heat preservation structure is layered, embrittled, pulverized and the like, and finally the service life of the heat preservation structure is shortened.
Comparative example 3
This comparative example provides a thermal insulation structure for silicon carbide single crystal growth, which is identical to that of example 1 except that the top thermal insulation unit and the bottom thermal insulation unit are removed, and only the side thermal insulation units are left, so that the description thereof will be omitted.
Compared with the embodiment 1, the heat insulation structure provided by the comparative example only has the side heat insulation units, so that the heat insulation structure cannot wrap the silicon carbide single crystal growth device in an omnibearing manner, the heat insulation performance and the heat insulation uniformity are further remarkably reduced, and finally the growth quality of the silicon carbide single crystal is lower than that of the embodiment 1.
Therefore, compared with the traditional heat-insulating structure with only side heat-insulating units, the heat-insulating structure provided by the invention has the advantages that the side heat-insulating units, the top heat-insulating unit and the bottom heat-insulating unit which are matched with each other wrap the silicon carbide single crystal growing device in an omnibearing manner, so that the heat-insulating performance and the heat-insulating uniformity are obviously improved, and the growth quality of the silicon carbide single crystal is improved.
In addition, the slope structure is arranged at the connecting end part of the side heat preservation unit, so that the gap between the heat preservation unit and the silicon carbide single crystal growing device is reduced, the consistency of heat preservation performance is ensured, and meanwhile, the phenomena of layering, embrittlement, pulverization and the like of the heat preservation structure caused by deposition reaction of silicon-containing gas in the gap of the heat preservation structure are avoided, so that the service life of the heat preservation structure is prolonged.
Further, the invention ensures that the thick edge of the outer end slope and the thick edge of the inner end slope and the thick edge of the outer end slope and the thin edge of the inner end slope are mutually overlapped in the radial direction by controlling the length of the inclined edge of the outer end slope to be larger than the length of the inclined edge of the inner end slope, thereby meeting the thickness consistency of the side heat preservation unit in the circumferential direction and improving the heat insulation performance and the heat preservation uniformity to the greatest extent.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (10)
1. The heat-insulating structure for the growth of the silicon carbide single crystal is characterized by comprising a side heat-insulating unit, a top heat-insulating unit and a bottom heat-insulating unit which are surrounded outside the silicon carbide single crystal growth device;
the side heat preservation unit is formed by winding a rectangular heat preservation strip, and two connecting end parts of the rectangular heat preservation strip are respectively and independently provided with a slope structure, wherein the slope structure comprises an outer end slope and an inner end slope;
the outer end slope is positioned at the connecting end part far away from the silicon carbide single crystal growing device, and the inner end slope is positioned at the connecting end part close to the silicon carbide single crystal growing device;
setting the hypotenuse length of the outer end slope to be L1, and setting the hypotenuse length of the inner end slope to be L2, the heat insulation structure meets the following conditions: l1> L2.
2. The insulation structure of claim 1, wherein the insulation structure comprises a graphite felt, and the graphite felt comprises a viscose-based graphite felt or a polyacrylonitrile-based graphite felt;
the thickness of the graphite soft felt is 2-20mm, and the density is 0.8-1.3g/cm 3 Ash content is less than or equal to 50ppm.
3. The insulation structure of claim 2, wherein the insulation structure comprises alternating layers of graphite felt and auxiliary sheets;
the auxiliary sheet layer comprises any one or a combination of at least two of graphite paper, graphite cloth or carbon fiber cloth;
the thickness of the auxiliary sheet layer is 0.1-1mm, and ash content is less than or equal to 100ppm.
4. The insulation structure of claim 1, wherein the side insulation units have a thickness of 20-150mm;
the side heat-insulating unit is divided into an outer heat-insulating part and an inner heat-insulating part, wherein the thickness of the outer heat-insulating part is 10-40mm, and the thickness of the inner heat-insulating part is 10-110mm;
setting the height of the outer-layer heat-insulating part as H1, setting the height of the inner-layer heat-insulating part as H2, and enabling the side heat-insulating unit to meet the following conditions: the thickness of H1-H2 is less than or equal to 10mm and less than or equal to 50mm.
5. The insulation structure according to claim 4, wherein a graphite felt ring is transversely laid on top of the inner insulation member, and an inner diameter of the graphite felt ring is consistent with an inner diameter of the inner insulation member, and an outer diameter of the graphite felt ring is consistent with an outer diameter of the inner insulation member;
the thickness of the graphite soft felt ring is 10-50mm.
6. The insulation structure of claim 1, wherein the slope structure has a hypotenuse length of 50-300mm and an included angle between the hypotenuse and the right angle side of 1-15 °;
the difference between the hypotenuse length L1 of the outer end slope and the hypotenuse length L2 of the inner end slope satisfies the following conditions: the diameter of the L1-L2 is less than or equal to 0mm and less than or equal to 200mm.
7. The insulating structure of claim 1, wherein the top insulating unit and the bottom insulating unit each independently comprise a circular insulating sheet;
the diameter of the round heat-insulating sheet is consistent with the outer diameter of the silicon carbide single crystal growing device.
8. A method of making a thermal insulation structure according to any one of claims 1 to 7, comprising the steps of:
(1) Selecting a rectangular heat preservation bar suitable for the height of a silicon carbide single crystal growing device, and correspondingly cutting an outer end slope and an inner end slope at two connecting ends of the rectangular heat preservation bar respectively;
(2) And winding the rectangular heat preservation strip to obtain a side heat preservation unit, and combining the cut top heat preservation unit and the cut bottom heat preservation unit to obtain the heat preservation structure for silicon carbide single crystal growth.
9. The method of claim 8, wherein the rectangular insulating strip of step (1) comprises a graphite felt;
an auxiliary sheet layer is attached to the rectangular heat-insulating strip in the winding treatment process, and the auxiliary sheet layer comprises any one or a combination of at least two of graphite paper, graphite cloth and carbon fiber cloth;
the winding treatment in the step (2) is carried out in a felt rolling machine, and the felt rolling tension is 1-100N.
10. Use of an insulating structure as claimed in any one of claims 1 to 7 for surrounding a silicon carbide single crystal growth apparatus, wherein the silicon carbide single crystal growth apparatus comprises a crucible or a heating body.
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