CN111809231A - Crucible beneficial to growth of silicon carbide crystals - Google Patents

Crucible beneficial to growth of silicon carbide crystals Download PDF

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Publication number
CN111809231A
CN111809231A CN202010490764.9A CN202010490764A CN111809231A CN 111809231 A CN111809231 A CN 111809231A CN 202010490764 A CN202010490764 A CN 202010490764A CN 111809231 A CN111809231 A CN 111809231A
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China
Prior art keywords
inner ring
graphite crucible
crucible
silicon carbide
growth
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CN202010490764.9A
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Chinese (zh)
Inventor
王振军
王静辉
焦博蛟
丁彦芳
和晓旭
于静
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In Power Engineering Construction Co
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In Power Engineering Construction Co
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Priority to CN202010490764.9A priority Critical patent/CN111809231A/en
Publication of CN111809231A publication Critical patent/CN111809231A/en
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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
    • 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
    • C30B29/36Carbides

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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 discloses a crucible beneficial to growth of silicon carbide crystals, belonging to the technical field of new materials and comprising a graphite crucible, a sealing cover arranged at the upper part of the graphite crucible, and a second heat insulation layer, a first heat insulation layer and a quartz vacuum chamber with an induction coil fixed outside, wherein the second heat insulation layer, the first heat insulation layer and the quartz vacuum chamber are sequentially and closely arranged outside the graphite crucible; the sizes of the outer diameters of the graphite crucibles are consistent up and down; the upper end of the inner diameter of the graphite crucible is smaller than the lower end, and the cross section of the graphite crucible is of an isosceles trapezoid structure; the bottom of the graphite crucible is provided with a first inner ring and a second inner ring which have different diameters and consistent heights; a seed crystal carrier with a handle is arranged at the opening position at the upper end of the graphite crucible and is tightly contacted with the sealing cover; the seed crystal is attached to the lower part of the seed crystal carrier; the handle is covered by the sealing cover; holes which are uniformly distributed are arranged on the first inner ring and the second inner ring. The graphite crucible structure designed by the invention is beneficial to the growth of the powdery silicon carbide raw material into seed crystals and the formation of crystals in the sublimation process, improves the production efficiency and reduces the production cost.

Description

Crucible beneficial to growth of silicon carbide crystals
Technical Field
The invention relates to the technical field of new materials, in particular to a crucible beneficial to growth of silicon carbide crystals, which is used for growing the silicon carbide crystals by a sublimation method.
Background
Following the first generation of silicon (Si) semiconductors and the second generation of gallium arsenide (GaAs) semiconductors, third generation wide bandgap semiconductors represented by SiC are receiving increasing attention.
As the most developed material in the third generation semiconductor material, silicon carbide (SiC) has the advantages of wide bandgap, high critical breakdown field strength (10 times of silicon), high thermal conductivity (3.3 times of Si), high carrier saturation mobility (2.5 times of Si), high bonding energy, and the like. The excellent properties of the material meet the new requirements of special fields of modern electronic technology, and the material is particularly suitable for manufacturing high-frequency, high-power, radiation-resistant and corrosion-resistant electronic devices, so the material is regarded as one of the most promising materials in the field of semiconductor materials.
A graphite crucible: the high-temperature-resistant high-. Has strong corrosion resistance to acid and alkaline solutions and excellent chemical stability. In the industrial departments of metallurgy, casting, machinery, chemical engineering and the like, the smelting method is widely used for smelting alloy tool steel and smelting non-ferrous metals and alloys thereof, and has better technical and economic effects.
At present, the silicon carbide crystal has the defects of low growth speed, low yield and high price in growth, and cannot meet the requirement of huge application market.
Disclosure of Invention
The technical problem to be solved by the invention is to provide the crucible beneficial to the growth of the silicon carbide crystal, the inner diameter section of the graphite crucible is set to be in an isosceles trapezoid structure, the two graphite inner rings with different diameters are arranged in the graphite crucible, and the graphite crucible with the structure is beneficial to the growth of the silicon carbide powdery raw material into seed crystals and the formation of crystals in the sublimation process, so that the production efficiency is improved, and the production cost is reduced.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a crucible beneficial to the growth of silicon carbide crystals comprises a graphite crucible, a sealing cover arranged at the upper part of the graphite crucible, a second heat insulation layer, a first heat insulation layer and a quartz vacuum chamber, wherein the second heat insulation layer, the first heat insulation layer and the quartz vacuum chamber are sequentially and closely arranged outside the graphite crucible; the sizes of the outer diameters of the graphite crucibles are consistent up and down; the upper end of the inner diameter of the graphite crucible is smaller than the lower end, and the cross section of the graphite crucible is of an isosceles trapezoid structure; the bottom of the graphite crucible is provided with a first inner ring and a second inner ring which have different diameters and consistent heights; a seed crystal carrier with a handle is arranged at the opening position at the upper end of the graphite crucible and is tightly contacted with the sealing cover; the seed crystal is attached to the lower part of the seed crystal carrier; the handle is covered by the sealing cover; holes which are uniformly distributed are arranged on the first inner ring and the second inner ring.
The technical scheme of the invention is further improved as follows: the outer diameter of the graphite crucible is 120-180 mm, the wall thickness of the outer wall of the graphite crucible at the position with the largest inner diameter of the graphite crucible is 10mm, and the height of the graphite crucible is 100-200 mm; the thickness of the sealing cover is 5-8 mm.
The technical scheme of the invention is further improved as follows: the diameter size of the seed crystal is 100-150 mm, and the thickness is 0.5-1 mm; the thickness of the seed crystal carrier is 5-8 mm.
The technical scheme of the invention is further improved as follows: the height of the inner ring I and the height of the inner ring II are both 20-50% of the height of the graphite crucible; the thickness of the first inner ring and the thickness of the second inner ring are both 5 mm.
The technical scheme of the invention is further improved as follows: the diameter of the inner ring I is 50-75 mm, and the diameter of the inner ring II is 25-35 mm.
The technical scheme of the invention is further improved as follows: the aperture ratio of the inner ring I is 10-20% of the surface area of the inner ring I; the opening rate of the inner ring II is 10-20% of the surface area of the inner ring.
The technical scheme of the invention is further improved as follows: the graphite crucible, the first inner ring and the second inner ring are integrally processed.
The technical scheme of the invention is further improved as follows: and the graphite crucible, the first inner ring and the second inner ring are processed in a two-body mode, and a groove of the first inner ring and a groove of the second inner ring are reserved at the bottom of the graphite crucible.
The technical scheme of the invention is further improved as follows: the first groove and the second groove of the inner ring can be of a whole circular ring shape, and clamping points can be designed symmetrically.
The technical scheme of the invention is further improved as follows: the growth temperature of the silicon carbide crystal in the graphite crucible is 2200-2400 ℃.
Due to the adoption of the technical scheme, the invention has the technical progress that:
1. the graphite crucible is arranged to be in an isosceles trapezoid structure with an angled inner diameter cross section, so that the graphite crucible is beneficial to uniformly heating the silicon carbide raw material in the growth process, is more beneficial to reaching a seed crystal after growing into a crystal and is convenient for extracting a grown finished product.
2. According to the invention, the inner rings I and II with the uniformly distributed pore-forming holes are arranged in the graphite crucible, so that the silicon carbide powder is more favorably and uniformly heated in the growth process than a common crucible structure, and can smoothly reach the seed crystal part, and the silicon carbide crystal is prevented from sliding down to the bottom of the crucible again when meeting cold because the silicon carbide crystal touches the outer wall of the crucible before reaching the seed crystal in the growth process.
3. The inner ring I and the inner ring II in the graphite crucible are provided with the uniformly distributed holes which are mainly used for heat dissipation, certain heat can be dissipated in the growth process of the silicon carbide, and the holes are increased to dissipate redundant heat so as to provide more appropriate environmental conditions for the growth of the silicon carbide.
4. The design of the integral structure of the graphite crucible in the invention ensures that the growth space of the silicon carbide raw material is relatively large, the growth and heating are more favorable for growing crystals, the crystals grow to the positions of seed crystals, and the caliber of the seed crystals is reduced at the positions of the seed crystals, so that the finished products can be more favorably taken out.
5. The integral structure of the invention is beneficial to fully sublimating the silicon carbide raw material, improves the production efficiency, solves the defects of low growth speed, low yield and high price of the silicon carbide, and meets the huge application market demand.
Drawings
FIG. 1 is a sectional view of the overall structure of the present invention;
FIG. 2 is a schematic view of the structure of the graphite crucible of the present invention;
FIG. 3 is a schematic view showing another structure of the graphite crucible of the present invention;
FIG. 4 is a sectional top view of the bottom of the graphite crucible of the present invention.
The device comprises a graphite crucible 1, a graphite crucible 1-1, an inner ring I, a seed crystal carrier 1-6, a handle 1-7, an inner ring I groove 1-8, an inner ring II groove 1-9, a graphite crucible bottom 1-10, a silicon carbide raw material 1-11, a graphite crucible outer wall 2, a thermal insulation layer II, a thermal insulation layer 3, a thermal insulation layer I, a thermal insulation layer II, a quartz vacuum chamber 4, an induction coil 5, a sealing cover 6, and a silicon carbide raw material placing area 1-4.
Detailed Description
The crucible beneficial to the growth of the silicon carbide crystal is developed aiming at the defects of low growth speed, low yield and high price of the growth of the silicon carbide crystal at present and incapable of meeting the requirement of huge application market.
The present invention will be described in further detail with reference to the following examples:
as shown in fig. 1 to 4, a crucible beneficial to the growth of silicon carbide crystals comprises a graphite crucible 1, a sealing cover 6 arranged at the upper part of the graphite crucible 1, and a second heat insulation layer 2, a first heat insulation layer 3 and a quartz vacuum chamber 4 with an induction coil 5 fixed outside, which are sequentially and closely attached to the outside of the graphite crucible 1; the sizes of the outer diameters of the graphite crucibles 1 are consistent up and down; the upper end of the inner diameter of the graphite crucible 1 is smaller than the lower end, the cross section of the graphite crucible is of an isosceles trapezoid structure, and in order to better attach the seed crystals 1-4 to the seed crystal carriers 1-5, the positions, where the seed crystal carriers 1-5 are placed, in the graphite crucible 1 can be set to be cylindrical; the bottom 1-9 of the graphite crucible is provided with a first inner ring 1-1 and a second inner ring 1-2 which have different diameters and consistent heights; a seed crystal carrier 1-5 with a handle 1-6 which is tightly contacted with a sealing cover 6 is arranged at the opening position at the upper end of the graphite crucible 1; the seed crystal 1-4 is attached to the lower part of the seed crystal carrier 1-5; the handles 1-6 are covered by the sealing cover 6, so that the sealing effect of the graphite crucible 1 is ensured; holes which are uniformly distributed are arranged on the inner ring I1-1 and the inner ring II 1-2; the handle 1-6 is arranged to facilitate taking out the seed crystal carrier 1-5 from the graphite crucible 1.
The outer diameter of the graphite crucible 1 is 120-180 mm, the wall thickness of the graphite crucible outer wall 1-11 at the maximum inner diameter of the graphite crucible 1 is 10mm, and the height of the graphite crucible 1 is 100-200 mm; the thickness of the sealing cover 6 is 5-8 mm.
The diameter of the seed crystal 1-4 is 100-150 mm, and the thickness is 0.5-1 mm; the thickness of the seed crystal carrier 1-5 is 5-8 mm.
As shown in fig. 2, the heights of the first inner ring 1-1 and the second inner ring 1-2 are both 20% -50% of the height of the graphite crucible 1; the thicknesses of the inner ring I1-1 and the inner ring II 1-2 are both 5 mm; the diameter of the inner ring I (1-1) is 50-75 mm, and the diameter of the inner ring II (1-2) is 25-35 mm; the aperture ratio of the inner ring I1-1 and the inner ring II 1-2 is 10-20% of the surface area of the inner ring.
As shown in fig. 2, 3 and 4, the graphite crucible 1 is integrally processed with the inner ring I1-1 and the inner ring II 1-2; the graphite crucible 1, the first inner ring 1-1 and the second inner ring 1-2 are processed in a split mode, and a first groove 1-7 of the first inner ring and a second groove 1-8 of the second inner ring are reserved at the bottom 1-9 of the graphite crucible; the first groove 1-7 and the second groove 1-8 can be in the shape of a whole ring or can be symmetrically designed with clamping points.
The growth temperature of the silicon carbide crystal in the graphite crucible 1 is 2200-2400 ℃, and at the temperature, the silicon carbide raw material 1-10 reaches the position of the seed crystal 1-4 after sublimation, so that the silicon carbide crystal is formed.
The working principle is as follows:
as shown in figures 1 and 2, the supporting part of the silicon carbide raw material 1-10 and the seed crystal 1-4 in the graphite crucible body and the internal structure of the graphite crucible body are core parts in the growth process of the silicon carbide crystal, the silicon carbide raw material 1-10 is placed in a silicon carbide raw material placing area 1-3 at the bottom of the graphite crucible 1, the size of the grown silicon carbide crystal is changed by the size of the graphite crucible 1 in the growth process of the silicon carbide crystal, the growth temperature of the silicon carbide crystal is controlled between 2200 and 2400 ℃, the temperature control is adjusted by a second heat insulating layer 2, a first heat insulating layer 3 and a quartz vacuum chamber 4 of an external fixed induction coil 5 which are arranged outside the graphite crucible 1, under the temperature, the silicon carbide raw material 1-10 reaches the position of the seed crystal 1-4 after sublimation, the seed crystal 1-4 is attached to a seed crystal carrier 1-5, forming a silicon carbide crystal; because the silicon carbide crystal formation process takes place in graphite crucible 1, so graphite crucible 1's inner structure is very critical in the growth of crystal, this patent application through the inner structure who changes graphite crucible 1, has improved the growth rate of silicon carbide crystal by a wide margin to effectual growth efficiency who promotes silicon carbide, it is slow to have solved silicon carbide crystal growth rate, and the yield is low, and defect that the price is high can satisfy huge application market demand.
In summary, the invention changes the internal structure, increases the hole design and changes the size design of the crucible by setting the internal shape of the graphite crucible, and achieves the purpose of changing the size of the grown crystal by changing the size of the graphite crucible, the temperature of the crystal growth is between 2200 and 2400 ℃, and at the temperature, the silicon carbide reaches the position of the seed crystal after sublimation, and the silicon carbide crystal is formed; the structure obviously improves the growth rate of the crystal and effectively improves the growth efficiency of the silicon carbide crystal.

Claims (10)

1. The utility model provides a do benefit to crucible that carborundum crystal grows, includes graphite crucible (1), sets up sealed lid (6) on graphite crucible (1) upper portion and hugs closely in proper order and sets up quartz vacuum chamber (4) of thermal insulating layer two (2), thermal insulating layer (3), outside fixed induction coil (5) outside graphite crucible (1), its characterized in that: the sizes of the outer diameters of the graphite crucibles (1) are consistent up and down; the upper end of the inner diameter of the graphite crucible (1) is smaller than the lower end, and the cross section of the graphite crucible is of an isosceles trapezoid structure; the bottom (1-9) of the graphite crucible is provided with a first inner ring (1-1) and a second inner ring (1-2) which have different diameters and consistent heights; a seed crystal carrier (1-5) with a handle (1-6) which is tightly contacted with the sealing cover (6) is arranged at the opening position at the upper end of the graphite crucible (1); the seed crystal (1-4) is attached to the lower part of the seed crystal carrier (1-5); the handle (1-6) is covered by the sealing cover (6); holes which are uniformly distributed are arranged on the inner ring I (1-1) and the inner ring II (1-2).
2. A crucible for facilitating growth of a silicon carbide crystal according to claim 1, wherein: the size of the outer diameter of the graphite crucible (1) is 120-180 mm, the wall thickness of the outer wall (1-11) of the graphite crucible at the position with the largest size of the inner diameter of the graphite crucible (1) is 10mm, and the height of the graphite crucible (1) is 100-200 mm; the thickness of the sealing cover (6) is 5-8 mm.
3. A crucible for facilitating growth of a silicon carbide crystal according to claim 1, wherein: the diameter of the seed crystal (1-4) is 100-150 mm, and the thickness is 0.5-1 mm; the thickness of the seed crystal carrier (1-5) is 5-8 mm.
4. A crucible for facilitating growth of a silicon carbide crystal according to claim 1, wherein: the heights of the inner ring I (1-1) and the inner ring II (1-2) are both 20-50% of the height of the graphite crucible (1); the thickness of the inner ring I (1-1) and the thickness of the inner ring II (1-2) are both 5 mm.
5. A crucible for facilitating growth of a silicon carbide crystal according to claim 1, wherein: the diameter of the inner ring I (1-1) is 50-75 mm, and the diameter of the inner ring II (1-2) is 25-35 mm.
6. A crucible for facilitating growth of a silicon carbide crystal according to claim 1, wherein: the opening rate of the inner ring I (1-1) is 10-20% of the surface area of the inner ring; the opening rate of the inner ring II (1-2) is 10-20% of the surface area of the inner ring.
7. A crucible for facilitating growth of a silicon carbide crystal according to claim 1, wherein: the graphite crucible (1), the first inner ring (1-1) and the second inner ring (1-2) are integrally processed.
8. A crucible for facilitating growth of a silicon carbide crystal according to claim 1, wherein: the graphite crucible (1), the first inner ring (1-1) and the second inner ring (1-2) are processed in a split mode, and a first inner ring groove (1-7) and a second inner ring groove (1-8) are reserved at the bottom (1-9) of the graphite crucible.
9. A crucible for facilitating growth of a silicon carbide crystal according to claim 8, wherein: the inner ring one groove (1-7) and the inner ring two groove (1-8) can be of a whole circular ring shape, and clamping points can also be symmetrically designed.
10. A crucible for facilitating growth of a silicon carbide crystal according to any one of claims 1 to 8, wherein: the growth temperature of the silicon carbide crystal in the graphite crucible (1) is 2200-2400 ℃.
CN202010490764.9A 2020-06-02 2020-06-02 Crucible beneficial to growth of silicon carbide crystals Pending CN111809231A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112853479A (en) * 2020-12-31 2021-05-28 湖南三安半导体有限责任公司 Single crystal growing device

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017178646A (en) * 2016-03-29 2017-10-05 新日鐵住金株式会社 Graphite crucible for producing silicon carbide single crystal
CN206624942U (en) * 2016-12-19 2017-11-10 山东天岳先进材料科技有限公司 A kind of device of physical carbon burdening growth carborundum crystals
CN207498512U (en) * 2017-11-02 2018-06-15 福建北电新材料科技有限公司 A kind of silicon carbide monocrystal growth device for growing high usage
CN110004486A (en) * 2019-05-09 2019-07-12 浙江博蓝特半导体科技股份有限公司 A method of improving growing silicon carbice crystals efficiency

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017178646A (en) * 2016-03-29 2017-10-05 新日鐵住金株式会社 Graphite crucible for producing silicon carbide single crystal
CN206624942U (en) * 2016-12-19 2017-11-10 山东天岳先进材料科技有限公司 A kind of device of physical carbon burdening growth carborundum crystals
CN207498512U (en) * 2017-11-02 2018-06-15 福建北电新材料科技有限公司 A kind of silicon carbide monocrystal growth device for growing high usage
CN110004486A (en) * 2019-05-09 2019-07-12 浙江博蓝特半导体科技股份有限公司 A method of improving growing silicon carbice crystals efficiency

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112853479A (en) * 2020-12-31 2021-05-28 湖南三安半导体有限责任公司 Single crystal growing device

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Application publication date: 20201023

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