CN113122916A - Batch preparation device and method for PVT method single crystals - Google Patents
Batch preparation device and method for PVT method single crystals Download PDFInfo
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- CN113122916A CN113122916A CN202110448564.1A CN202110448564A CN113122916A CN 113122916 A CN113122916 A CN 113122916A CN 202110448564 A CN202110448564 A CN 202110448564A CN 113122916 A CN113122916 A CN 113122916A
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- seed crystal
- middle section
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- 239000013078 crystal Substances 0.000 title claims abstract description 100
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 137
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 137
- 239000010439 graphite Substances 0.000 claims abstract description 137
- 230000006698 induction Effects 0.000 claims abstract description 12
- 238000012545 processing Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 13
- 238000010923 batch production Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 11
- 235000017166 Bambusa arundinacea Nutrition 0.000 abstract description 4
- 235000017491 Bambusa tulda Nutrition 0.000 abstract description 4
- 241001330002 Bambuseae Species 0.000 abstract description 4
- 235000015334 Phyllostachys viridis Nutrition 0.000 abstract description 4
- 239000011425 bamboo Substances 0.000 abstract description 4
- 238000009434 installation Methods 0.000 abstract description 4
- 230000008878 coupling Effects 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- 238000013461 design Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 241000201976 Polycarpon Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a batch preparation device and method of PVT method single crystals, belonging to the field of crystal growth. Solves the problems of low single crystal preparation efficiency and higher preparation cost. The crucible comprises a heater, the graphite lid, the graphite holds in the palm, the seed crystal bearing structure, the seed crystal, the crucible middle section, a graphite section of thick bamboo, induction coil, the graphite dish, the support ring, crucible body and seed crystal hold in the palm, the crucible body is connected with the crucible middle section, at crucible body coupling graphite dish, process circular through-hole on the graphite dish, circular through-hole corresponds position installation graphite section of thick bamboo, the graphite lid is connected in the crucible middle section, crucible middle section and graphite lid junction installation support ring, set up the graphite support on the support ring, the graphite holds in the palm and corresponds position processing round hole with the circular through-hole of graphite dish, seed crystal bearing structure is connected with the seed crystal support, the seed crystal is connected in the seed crystal support, induction coil installation crucible middle section and the outside of. The growth of a plurality of seed crystals is realized simultaneously, the material preparation speed is improved, and the preparation cost is greatly reduced.
Description
Technical Field
The invention relates to a device and a method for preparing single crystals in batches, belonging to the field of crystal growth.
Background
The term "single crystal" means that the particles within a crystal are regularly and periodically arranged in three dimensions, or the entire crystal is composed of a three-dimensional lattice of the same space, and the particles are spatially arranged in a long-range order throughout the crystal. The entire crystal lattice of a single crystal is continuous and has important industrial applications. The physical vapor transport PVT method is a mainstream method for producing a high-melting point semiconductor crystal material such as silicon carbide and aluminum nitride, which is difficult to produce by the liquid phase method. Although the materials have great application prospects in the emerging strategic fields of new energy automobiles and the like, the preparation process has the characteristics of low material preparation speed, high reaction temperature and the like, the preparation cost is high, and the downstream scale application of the materials is greatly influenced.
In view of the above problems, it is desirable to provide an apparatus and a method for batch preparation of PVT single crystal to solve the above technical problems.
Disclosure of Invention
The invention provides a batch preparation device and method of PVT method single crystals, which solve the problems of low single crystal preparation efficiency and high preparation cost. The following presents a simplified summary of the invention in order to provide a basic understanding of some aspects of the invention. It should be understood that this summary is not an exhaustive overview of the invention. It is not intended to determine the key or critical elements of the present invention, nor is it intended to limit the scope of the present invention.
The technical scheme of the invention is as follows:
a batch preparation device of PVT method single crystal comprises a heater, a graphite cover, a graphite support, a seed crystal supporting structure, a seed crystal, a crucible middle section, a graphite cylinder, an induction coil, a graphite disc, a supporting ring, a crucible body and a seed crystal support, wherein the crucible body, the crucible middle section and the graphite cover are sequentially connected from bottom to top, install the graphite plate at crucible body and crucible middle section connecting portion, it has a plurality of circular through-holes to process on the graphite plate, circular through-hole corresponds position installation graphite section of thick bamboo, the graphite section of thick bamboo is located inside the crucible middle section, the support ring is installed with graphite lid connecting portion in the crucible middle section, the upper portion of support ring is provided with graphite and holds in the palm, it has the round hole to correspond position department processing with the circular through-hole of graphite plate on the graphite holds in the palm, it holds in the palm to be connected with the seed crystal through seed crystal bearing structure in the round hole that the graphite held in the palm, the sub-unit connection seed crystal that the seed crystal.
Preferably: the graphite support is characterized by further comprising a graphite sheet, and the graphite sheet is arranged between the graphite support and the graphite cover.
Preferably: the upper portion processing of the crucible body has the ladder snap ring, and the graphite plate is installed in the ladder snap ring department of the crucible body.
Preferably: the lower end of the graphite cylinder is connected with a porous graphite cylinder, and the porous graphite cylinder is inserted into the reaction raw materials in the crucible body.
A batch preparation method of PVT method single crystal comprises the following steps:
the method comprises the following steps: placing the connected graphite barrel and the porous graphite barrel into a crucible body, placing reaction raw materials into the crucible body, and connecting the circular through hole of the graphite disc with the graphite barrel in a matching manner to fix the positions of the graphite barrel and the porous graphite barrel;
step two: the upper end of the graphite plate is connected with the middle section of the crucible, a support ring is placed on the inner side above the middle section of the crucible, and a graphite support is placed above the support ring;
step three: placing a seed crystal support bearing seed crystals on a seed crystal support structure, fixing the seed crystal support structure at a round hole of a graphite support, placing graphite flakes on the upper side of the graphite support, and covering a graphite cover;
step four: starting a heater and an induction coil and entering a crystal growth stage;
step five: after the crystal growth stage is finished, cooling to room temperature;
step six: and (3) disassembling the graphite cover and the graphite flake in sequence, taking out the graphite support, and taking off the seed crystal supporting structure from the graphite support to obtain a monocrystal.
The invention has the following beneficial effects:
1. after the crystal growth is finished each time, only the seed crystal supporting structure needs to be replaced, so that the time cost and the labor cost are reduced, the working efficiency is improved, and the preparation of a plurality of crystal materials can be realized by one-time operation;
2. the graphite barrel plays a role in guiding reaction raw materials, so that the reaction raw materials are collected to seed crystals for growth, the crystal growth rate is improved, the raw material utilization rate is improved, the induction coil is arranged at the middle section of the crucible and on the outer side of the crucible body to provide heat for heating the whole crucible, the heaters are arranged on the upper side and the lower side of the device and can be set at different temperatures to provide heat field temperatures required by the two sides, and through reasonable heat field design and guiding design, under the condition of reducing the consumption of materials as much as possible, the growth of a plurality of seed crystals at the same time is realized, the material preparation rate is improved, and the preparation cost is greatly reduced.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus and a method for batch preparation of single crystals by PVT method;
FIG. 2 is a schematic view of the structure at A in FIG. 1;
FIG. 3 is a schematic diagram of the structure at B in FIG. 1;
fig. 4 is a schematic diagram of the structure at C in fig. 1.
In the figure, 1-a heater, 2-a graphite cover, 3-a graphite support, 4-a seed crystal supporting structure, 5-a seed crystal, 6-a graphite sheet, 7-a crucible middle section, 8-a graphite cylinder, 9-an induction coil, 10-a graphite disc, 11-a supporting ring, 12-a crucible body, 14-a seed crystal support, 102-reaction raw materials and 16-a porous graphite cylinder.
Detailed Description
In order that the objects, aspects and advantages of the invention will become more apparent, the invention will be described by way of example only, and in connection with the accompanying drawings. It is to be understood that such description is merely illustrative and not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
The connection mentioned in the invention is divided into fixed connection and detachable connection, the fixed connection is non-detachable connection and includes but is not limited to folding edge connection, rivet connection, bonding connection, welding connection and other conventional fixed connection modes, the detachable connection includes but is not limited to threaded connection, snap connection, pin connection, hinge connection and other conventional detachment modes, when the specific connection mode is not clearly limited, at least one connection mode can be found in the existing connection modes by default to realize the function, and the skilled person can select according to the needs. For example: the fixed connection selects welding connection, and the detachable connection selects hinge connection.
The first embodiment is as follows: the embodiment is described with reference to fig. 1-4, and the batch preparation device of single crystal by PVT method of the embodiment comprises a heater 1, a graphite cover 2, a graphite holder 3, a seed crystal support structure 4, a seed crystal 5, a crucible middle section 7, a graphite cylinder 8, an induction coil 9, a graphite disc 10, a support ring 11, a crucible body 12 and a seed crystal holder 14, wherein the upper part of the crucible body 12 is fixed with the crucible middle section 7 by screw thread connection or embedding, the height of the crucible middle section 7 can be changed according to different requirements, the adjustment of the device height can be realized without changing the crucible body 12, the crucible middle section 7 has lower cost as spare parts of various models, and is convenient to install, disassemble, maintain and maintain, the graphite disc 10 is connected to the upper part of the crucible body 12, a plurality of circular through holes are processed on the graphite disc 10, the corresponding positions of the circular through holes are inserted into the graphite cylinder 8 and positioned inside the crucible middle section 7, the upper part of the crucible middle section 7 is in threaded connection or embedded fixation with the graphite cover 2, the sealing performance is high, an inner ring groove is formed at the joint of the crucible middle section 7 and the graphite cover 2, the support ring 11 is installed at the inner ring groove, the upper part of the support ring 11 is provided with the graphite support 3, the edge of the graphite support 3 is supported by the support ring 11, a round hole is processed at the position corresponding to the round through hole of the graphite tray 3 and the graphite plate 10, the seed crystal support structure 4 is detachably connected in the round hole of the graphite support 3, the inner wall of the round hole of the graphite support 3 is provided with threads, the outer wall of the seed crystal support structure 4 is provided with external threads matched with the threads on the inner wall of the round hole, compared with the conventional method that the seed crystal is fixed on the crucible cover, and the like, the seed crystal 5 is fixed on the graphite support 3 by the seed crystal support, seed crystal bearing structure 4 is connected with seed crystal support 14, seed crystal 5 bonds in the lower part of seed crystal support 14, graphite cylinder 8 plays the effect of water conservancy diversion to reaction raw materials, make it collect seed crystal 5 and grow, improve crystal growth rate, improve the utilization ratio of raw materials, induction coil 9 is installed in the outside of crucible middle section 7 and crucible body 12, the heat of the inside heating of whole crucible is provided, heater 1 is located the upper and lower both sides of device, can set up different temperatures, provide the required thermal field temperature in both sides, through reasonable thermal field design and water conservancy diversion design, under the condition that the minimize consumptive material used, it grows simultaneously to have realized many seed crystals, speed with the material preparation has promoted more than the triple, preparation cost has been reduced by a wide margin.
The second embodiment is as follows: referring to fig. 1, the batch preparation apparatus for single crystal by PVT method of the present embodiment further includes a graphite sheet 6, the graphite sheet 6 is installed between the graphite tray 3 and the graphite cover 2, and the graphite sheet 6 provides a longitudinally uniform temperature field.
The third concrete implementation mode: referring to fig. 1, the embodiment, which is a batch preparation apparatus for single crystals by PVT method, is described, wherein a stepped snap ring is formed at an upper portion of a crucible body 12, and a graphite plate 10 is installed at the stepped snap ring of the crucible body 12.
The fourth concrete implementation mode: in the present embodiment, the porous graphite cylinder 16 is connected to the lower end of the graphite cylinder 8, and the porous graphite cylinder 16 is inserted into the reaction raw material 15 to separate the reaction raw material 15 from the graphite plate 10 at the corresponding position of the circular through hole, thereby realizing a filtering function and improving the crystal growth quality.
The fifth concrete implementation mode: the present embodiment will be described with reference to fig. 1 to 4, and the PVT method single crystal batch production method of the present embodiment includes the steps of:
the method comprises the following steps: placing the connected graphite cylinder 8 and the porous graphite cylinder 16 into a crucible body 12, placing a reaction raw material 15 into the crucible body 12, and connecting the circular through hole of the graphite plate 10 with the graphite cylinder 8 in a matching manner to fix the positions of the graphite cylinder 8 and the porous graphite cylinder 16;
step two: the upper end of the graphite plate 10 is connected with the middle crucible section 7, a support ring 11 is placed on the inner side above the middle crucible section 7, and a graphite support 3 is placed above the support ring 11;
step three: placing a seed crystal support 14 bearing a seed crystal 5 on a seed crystal supporting structure 4, fixing the seed crystal supporting structure 4 at a round hole of a graphite support 3, placing a graphite sheet 6 on the upper side of the graphite support 3, and covering a graphite cover 2;
step four: starting the heater 1 and the induction coil 9, and entering a crystal growth stage;
step five: after the crystal growth stage is finished, cooling to room temperature;
step six: the graphite cover 2 and the graphite flake 6 are disassembled in sequence, the graphite support 3 is taken out, the seed crystal supporting structure 4 is taken down from the graphite support 3, a single crystal is obtained, and the multiple preparation of single crystal materials is realized.
It should be noted that, in the above embodiments, as long as the technical solutions can be aligned and combined without contradiction, those skilled in the art can exhaust all possibilities according to the mathematical knowledge of the alignment and combination, and therefore, the present invention does not describe the technical solutions after alignment and combination one by one, but it should be understood that the technical solutions after alignment and combination have been disclosed by the present invention.
This embodiment is only illustrative of the patent and does not limit the scope of protection thereof, and those skilled in the art can make modifications to its part without departing from the spirit of the patent.
Claims (5)
1. A PVT method single crystal batch preparation device is characterized in that: comprises a heater (1), a graphite cover (2), a graphite support (3), a seed crystal supporting structure (4), a seed crystal (5), a crucible middle section (7), a graphite cylinder (8), an induction coil (9), a graphite disc (10), a supporting ring (11), a crucible body (12) and a seed crystal support (14), wherein the crucible body (12), the crucible middle section (7) and the graphite cover (2) are sequentially connected from bottom to top, the graphite disc (10) is arranged at the connecting part of the crucible body (12) and the crucible middle section (7), a plurality of circular through holes are processed on the graphite disc (10), the graphite cylinder (8) is arranged at the corresponding position of the circular through holes, the graphite cylinder (8) is positioned inside the crucible middle section (7), the supporting ring (11) is arranged at the connecting part of the crucible middle section (7) and the graphite cover (2), the graphite support (3) is arranged at the upper part of the supporting ring (11), and circular through holes corresponding to the graphite disc (10) are, a seed crystal support (14) is connected in a circular hole of the graphite support (3) through a seed crystal supporting structure (4), the lower part of the seed crystal support (14) is connected with a seed crystal (5), an induction coil (9) is installed on the outer sides of the crucible middle section (7) and the crucible body (12), and the heater (1) is located on the upper side and the lower side of the device.
2. The apparatus for single crystal batch production by PVT method according to claim 1, wherein: the graphite plate (6) is arranged between the graphite support (3) and the graphite cover (2).
3. The apparatus for single crystal batch production by PVT method according to claim 1, wherein: the upper portion processing of the crucible body (12) has the ladder snap ring, and the ladder snap ring department at the crucible body (12) is installed in graphite dish (10).
4. The apparatus for single crystal batch production by PVT method according to any one of claims 1 to 3, wherein: the lower end of the graphite cylinder (8) is connected with a porous graphite cylinder (16), and the porous graphite cylinder (16) is inserted into a reaction raw material (15) in the crucible body (12).
5. A batch preparation method of PVT method single crystal is characterized by comprising the following steps:
the method comprises the following steps: placing the connected graphite cylinder (8) and the porous graphite cylinder (16) into a crucible body (12), placing a reaction raw material (15) into the crucible body (12), and connecting the circular through hole of the graphite disc (10) with the graphite cylinder (8) in a matching way to fix the positions of the graphite cylinder (8) and the porous graphite cylinder (16);
step two: the upper end of the graphite plate (10) is connected with the middle crucible section (7), a support ring (11) is placed on the inner side above the middle crucible section (7), and a graphite support (3) is placed above the support ring (11);
step three: placing a seed crystal support (14) bearing a seed crystal (5) on a seed crystal supporting structure (4), fixing the seed crystal supporting structure (4) at a round hole of a graphite support (3), placing a graphite sheet (6) on the upper side of the graphite support (3), and covering a graphite cover (2);
step four: starting the heater (1) and the induction coil (9) and entering a crystal growth stage;
step five: after the crystal growth stage is finished, cooling to room temperature;
step six: sequentially disassembling the graphite cover (2) and the graphite flake (6), taking out the graphite support (3), and taking down the seed crystal supporting structure (4) from the graphite support (3) to obtain a single crystal.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110448564.1A CN113122916A (en) | 2021-04-25 | 2021-04-25 | Batch preparation device and method for PVT method single crystals |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110448564.1A CN113122916A (en) | 2021-04-25 | 2021-04-25 | Batch preparation device and method for PVT method single crystals |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10291899A (en) * | 1997-04-21 | 1998-11-04 | Showa Denko Kk | Production of silicon carbide single crystal and apparatus for production therefor |
| WO1999014405A1 (en) * | 1997-09-12 | 1999-03-25 | Showa Denko Kabushiki Kaisha | Method and apparatus for producing silicon carbide single crystal |
| US6336971B1 (en) * | 1997-09-12 | 2002-01-08 | Showa Denko Kabushiki Kaisha | Method and apparatus for producing silicon carbide single crystal |
| JP2009040637A (en) * | 2007-08-09 | 2009-02-26 | Denso Corp | Manufacturing method and manufacturing apparatus for silicon carbide single crystal |
| KR20100066072A (en) * | 2008-12-09 | 2010-06-17 | 한국전기연구원 | Growth apparatus for multiple silicon carbide single crystal |
| US20150361580A1 (en) * | 2014-06-16 | 2015-12-17 | Usi Optronics Corporation | Device and method for producing multi silicon carbide crystals |
| JP2017100920A (en) * | 2015-12-02 | 2017-06-08 | 昭和電工株式会社 | Method for manufacturing silicon carbide sintered body raw material, silicon carbide sintered body raw material and method for manufacturing silicon carbide single crystal |
| CN111235631A (en) * | 2020-03-19 | 2020-06-05 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Multi-seed-crystal crucible device for crystal preparation based on physical vapor transport method |
| CN111394788A (en) * | 2020-04-03 | 2020-07-10 | 江苏超芯星半导体有限公司 | Method and device for preparing cubic silicon carbide crystals |
-
2021
- 2021-04-25 CN CN202110448564.1A patent/CN113122916A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10291899A (en) * | 1997-04-21 | 1998-11-04 | Showa Denko Kk | Production of silicon carbide single crystal and apparatus for production therefor |
| WO1999014405A1 (en) * | 1997-09-12 | 1999-03-25 | Showa Denko Kabushiki Kaisha | Method and apparatus for producing silicon carbide single crystal |
| US6336971B1 (en) * | 1997-09-12 | 2002-01-08 | Showa Denko Kabushiki Kaisha | Method and apparatus for producing silicon carbide single crystal |
| JP2009040637A (en) * | 2007-08-09 | 2009-02-26 | Denso Corp | Manufacturing method and manufacturing apparatus for silicon carbide single crystal |
| KR20100066072A (en) * | 2008-12-09 | 2010-06-17 | 한국전기연구원 | Growth apparatus for multiple silicon carbide single crystal |
| US20150361580A1 (en) * | 2014-06-16 | 2015-12-17 | Usi Optronics Corporation | Device and method for producing multi silicon carbide crystals |
| JP2017100920A (en) * | 2015-12-02 | 2017-06-08 | 昭和電工株式会社 | Method for manufacturing silicon carbide sintered body raw material, silicon carbide sintered body raw material and method for manufacturing silicon carbide single crystal |
| CN111235631A (en) * | 2020-03-19 | 2020-06-05 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Multi-seed-crystal crucible device for crystal preparation based on physical vapor transport method |
| CN111394788A (en) * | 2020-04-03 | 2020-07-10 | 江苏超芯星半导体有限公司 | Method and device for preparing cubic silicon carbide crystals |
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Application publication date: 20210716 |