CN117107345A - Silicon carbide crystal growth method and growth device thereof - Google Patents
Silicon carbide crystal growth method and growth device thereof Download PDFInfo
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- CN117107345A CN117107345A CN202311181250.5A CN202311181250A CN117107345A CN 117107345 A CN117107345 A CN 117107345A CN 202311181250 A CN202311181250 A CN 202311181250A CN 117107345 A CN117107345 A CN 117107345A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 100
- 238000002109 crystal growth method Methods 0.000 title abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 222
- 239000002994 raw material Substances 0.000 claims abstract description 62
- 238000010438 heat treatment Methods 0.000 claims description 41
- 230000006698 induction Effects 0.000 claims description 17
- 239000000112 cooling gas Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 230000007246 mechanism Effects 0.000 claims description 14
- 230000001276 controlling effect Effects 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 3
- 230000033228 biological regulation Effects 0.000 claims description 2
- 230000004888 barrier function Effects 0.000 claims 4
- 238000000354 decomposition reaction Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 239000011229 interlayer Substances 0.000 description 11
- 238000001914 filtration Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 238000013461 design Methods 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000004321 preservation Methods 0.000 description 4
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 230000005674 electromagnetic induction Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
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- 238000002360 preparation method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
-
- 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
Abstract
The application discloses a silicon carbide crystal growth device and a silicon carbide crystal growth method, wherein the silicon carbide crystal growth device comprises a crucible unit, a growth unit and a raw material unit, the crucible unit comprises a crucible cover and a crucible barrel, the growth unit is arranged below the crucible cover, and the raw material unit is arranged in the crucible barrel. The silicon carbide crystal growth device can expand and grow to obtain large-diameter silicon carbide crystals, improve the yield of products and avoid edge cracks and polycrystal.
Description
Technical Field
The application relates to the technical field of crystal growth, in particular to a silicon carbide crystal growth method and a silicon carbide crystal growth device.
Background
Silicon carbide (SiC) has the characteristics of wide forbidden band, high critical breakdown electric field, high thermal conductivity, high carrier saturation migration speed and the like, has huge application potential in the aspects of high temperature, high frequency, high power, microelectronic devices and the like, and is a single crystal compound most significant in the current third-generation semiconductor materials. Silicon carbide crystal growth is currently mostly performed using PVT techniques, physical vapor transport: the solid silicon carbide powder is placed in a crucible made of graphite, and the top of the crucible is adhered with seed crystals of a required crystal form. The whole crucible is wrapped by a certain amount of graphite felt, and is heated by electromagnetic induction of an induction coil to form a specific temperature field. When crystal growth is performed, non-stoichiometric decomposition and sublimation of solid SiC powder as a growth raw material occurs and various forms of gas phase components are generated. The gas phase component is transported to a crystal growth interface with a relatively low temperature under the drive of an axial temperature gradient, and recrystallized into SiC crystals at the growth interface.
Currently, conductive silicon carbide substrates are mainly 6 inches in size, and the development of silicon carbide substrates is gradually advancing to 8 inches. In the same crystal preparation time, the increase of the substrate area can greatly reduce the cost, and the number of chips prepared on a single substrate increases with the increase of the substrate size, so that the cost of unit chips also decreases, and therefore, both the conductive silicon carbide substrate and the semi-insulating silicon carbide substrate are developed towards the direction of increasing the size.
The main challenges faced in the process of the silicon carbide crystal expanding growth method include: 1. expansion growth problem: the crystal is expanded from 6 inches to 8 inches, seed crystals are required to be processed, and a Physical Vapor Transport (PVT) method is used for preparing the silicon carbide substrate, so that the transportation efficiency of raw materials in a growth furnace is required to be improved, the problems of polycrystal nucleation at the edge of the seed crystals and multiple phase changes are solved, and the crystallization quality is improved. 2. Temperature field control problem: in the crystal growth process, a larger radial temperature gradient is required to be maintained, the cracking caused by the increase of internal stress of the crystal is avoided, the 6-inch crystal growth furnace is adjusted to be an 8-inch crystal growth furnace, and the temperature regulation accuracy of the growth furnace is required to be higher.
Disclosure of Invention
The application aims to provide a silicon carbide crystal growth device and a silicon carbide crystal growth method, which enable silicon carbide crystals to grow in an expanded diameter manner and improve the yield of large-diameter crystals.
In order to achieve the above purpose, the application adopts the following technical scheme: the utility model provides a carborundum crystal growing device, including crucible unit, growth unit and raw materials unit, the crucible unit includes crucible cover and crucible bucket, the growth unit sets up the crucible cover below, the raw materials unit sets up in the crucible bucket, the raw materials unit includes the filter vat, the inner wall of crucible bucket with form the raw materials chamber of the growth raw materials of placing the crystal between the filter vat, the outer wall of filter vat defines a buffer memory chamber, after growing the raw materials sublimates, through the filter vat gets into the buffer memory chamber, the raw materials chamber contains more than one independent cavity, each cavity is followed the buffer memory chamber arranges from top to bottom, each cavity is outer to set up independent heater respectively in order to realize independent heating.
Preferably, a interlayer heat insulation felt is arranged between each two adjacent chambers, interlayer vent holes which penetrate transversely are arranged in the interlayer heat insulation felt, and the interlayer vent holes are suitable for reducing heat transfer between each two adjacent chambers.
As another preferred, the filter vat includes filtering roof and filtration curb plate, it is in to filter the roof setting the upper portion in raw materials chamber, it is in to filter the curb plate setting the lateral part in raw materials chamber, it includes first curb plate and second curb plate to filter the curb plate, first buffer memory chamber that the first curb plate surrounds and forms reduces from top to bottom diameter gradually, the second buffer memory chamber diameter that the second curb plate surrounds and forms is unchangeable.
As another preferable mode, a temperature control system is further arranged outside each chamber, and the temperature control system is electrically connected with the heater and is suitable for being matched with the heater to detect and adjust the temperature of each chamber.
As another preferable aspect, the growth unit includes a seed crystal support disposed below the crucible cover, and an expanded-diameter crystal growth ring disposed below the seed crystal support, the expanded-diameter crystal growth ring is of a hollow structure and extends a plurality of bars on an inner wall, the expanded-diameter crystal growth ring is communicated with the outside through a plurality of second through holes, and cooling gas is adapted to enter the inside of the expanded-diameter crystal growth ring from the second through holes so as to adjust the temperature of the expanded-diameter crystal growth ring. As a further preference, the method comprises,
as another preferable mode, the heater comprises a long crystal ring induction heater, the temperature control system comprises a long crystal ring heating temperature control system, and the long crystal ring induction heater and the long crystal ring heating temperature control system are matched with each other to adjust the flow of cooling gas so as to detect and adjust the temperature of the expanded long crystal ring.
As another preferred aspect, the growth unit further includes a seed crystal support and a seed crystal module temperature control mechanism, the crucible cover is provided with a plurality of first through holes vertically penetrating, the seed crystal module temperature control mechanism passes through the first through holes to detect the temperature of the seed crystal support, and the first through holes are further suitable for introducing cooling gas to adjust the temperature of the seed crystal support.
As another preference, the crucible barrel is adapted to move up and down such that the feedstock unit is relatively distant or close to the growth unit.
As another preferable mode, the heating barrel comprises a supporting tray, wherein the crucible barrel is arranged on the supporting tray, and the lifting device is connected with the supporting tray to drive the crucible barrel to move up and down, so that the raw material unit and the growth unit can be relatively far away or close to each other.
The application provides another technical scheme that: a silicon carbide crystal growth method, characterized by comprising the steps of S1: setting the temperature of each chamber respectively; s2: controlling the descending speed of the crucible barrel, and respectively adjusting the temperature of the whole chamber; s3: gradually reducing the crystal growth pressure, maintaining the descending speed, and respectively adjusting the temperature of the whole chamber.
Compared with the prior art, the application has the beneficial effects that:
(1) The arrangement of the plurality of raw material cavities with independent controllable temperature is beneficial to adjusting the decomposition rate of crystal raw materials, and avoids overlarge gas composition change in the early and later stages of crystal growth, so that the silicon-carbon ratio is unbalanced, and the crystal yield is reduced;
(2) The expanded diameter crystal growth ring is designed into a hollow structure, cooling gas can be introduced inwards to control the growth temperature of seed crystals in the growth cavity, so that the expanded diameter growth of crystals is facilitated, and the phenomenon of edge cracking is reduced;
(3) Through the structural design of filtering roof and filtering curb plate in the filter vat, be favorable to slowing down the piling up of raw materials in seed crystal department, be favorable to crystal expanding growth.
Drawings
FIG. 1 is a cross-sectional view of a silicon carbide crystal growth apparatus according to one embodiment of the present application;
FIG. 2 is a cross-sectional view of a silicon carbide crystal growth apparatus according to one embodiment of the present application;
FIG. 3 is a partial enlarged view of the structure of the expanded diameter long crystal ring of the present application;
FIG. 4 is a schematic view of a telescoping mechanism in a silicon carbide crystal growth apparatus according to one embodiment of the present application, with other structures not shown;
FIG. 5 is a sectional view of a silicon carbide crystal growth apparatus B in comparative example 1;
FIG. 6 is a sectional view of a silicon carbide crystal growth apparatus C of comparative example 2;
FIG. 7 is a sectional view of a silicon carbide crystal growth apparatus D of comparative example 3;
FIG. 8 is a silicon carbide crystal A obtained by growth in example 1;
FIG. 9 is a view showing a silicon carbide crystal B obtained by growth in comparative example 1;
FIG. 10 is a view showing a silicon carbide crystal C grown in comparative example 2;
FIG. 11 is a view showing a silicon carbide crystal D obtained by growth in comparative example 3;
FIG. 12 is a silicon carbide crystal F grown in comparative example 4;
in the figure: 1. a crucible unit; 11. a crucible cover; 111. a first through hole; 12. a crucible barrel; 13. a telescoping mechanism; 2. heating the barrel; 21. heating the side wall; 22. a thermal insulation felt; 23. a support tray; 24. a lifting device; 3. a growth unit; 31. a seed crystal support; 32. a seed crystal module temperature control mechanism; 33. expanding a crystal ring; 331. a second through hole; 332. a stop bar; 4. a raw material unit; 41. a filter vat; 411. a filter top plate; 412. a filtering side plate; 42. a raw material cavity; 421. an upper chamber; 422. a middle chamber; 423. a lower chamber; 43. a buffer cavity; 44. an interlayer insulation blanket; 45. an interlayer vent; 5. a heater; 51. an upper induction heater; 52. a middle induction heater; 53. a lower induction heater; 54. a crystal growth ring induction heater; 6. a temperature control system; 61. an upper heating temperature control system; 62. the middle part heats the temperature control system; 63. a lower heating temperature control system; 64. a crystal growth ring heating temperature control system; 65. and (5) detecting the hole.
Detailed Description
The present application will be further described with reference to the following specific embodiments, and it should be noted that, on the premise of no conflict, new embodiments may be formed by any combination of the embodiments or technical features described below.
In the description of the present application, it should be noted that, for the azimuth words such as terms "center", "lateral", "longitudinal", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc., the azimuth and positional relationships are based on the azimuth or positional relationships shown in the drawings, it is merely for convenience of describing the present application and simplifying the description, and it is not to be construed as limiting the specific scope of protection of the present application that the device or element referred to must have a specific azimuth configuration and operation.
It should be noted that the terms "first," "second," and the like in the description and in the claims are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order.
The terms "comprises" and "comprising," along with any variations thereof, in the description and claims, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
As shown in fig. 1, the present application provides a silicon carbide crystal growth apparatus comprising a crucible unit 1, a heating barrel 2, a growth unit 3 and a raw material unit 4, wherein the heating barrel 2 is arranged outside the crucible unit 1 for generating heat and conducting the heat to the crucible to reach a temperature conforming to the growth of silicon carbide crystals; the crucible unit 1 comprises a crucible barrel 12 and a crucible cover 11 arranged at the top of the crucible barrel 12, wherein the bottom of the crucible barrel 12 is provided with a raw material unit 4 for placing silicon carbide crystal growth raw materials, the lower part of the crucible cover 11 forms a crystal growth unit 3, and the silicon carbide crystal growth raw materials sublimate from the raw material unit 4 to a seed crystal below the crucible cover 11 for crystal growth, so that the silicon carbide crystal is obtained.
As shown in fig. 2, the silicon carbide crystal growth apparatus further includes a heater 5 and a temperature control system 6, which collectively control the evaporation rate of the raw material in the raw material unit 4, thereby adjusting the growth rate of the crystal.
The heating barrel 2 is arranged on the outer side of the crucible unit 1, the heating side wall 21 of the heating barrel 2 is tightly attached to the outer wall of the crucible barrel 12, and the temperature of the crucible barrel 12 is increased due to the temperature rise of the heating side wall 21. The heating barrel 2 further comprises a heat preservation felt 22 arranged at the bottom outside the crucible barrel 12, and the heat preservation felt 22 can reduce the heat loss at the bottom of the crucible barrel 12.
As shown in fig. 2 and 3, the growth unit 3 comprises a seed crystal support 31, a seed crystal module temperature control mechanism 32 and an expanded diameter crystal growth ring 33, the seed crystal support 31 is arranged below the crucible cover 11, a seed crystal is arranged below the seed crystal support 31, a growth cavity 34 is formed below the seed crystal support 31, and after the silicon carbide raw material is biochemically grown, crystal growth is continued at the growth cavity 34. In some preferred embodiments, the seed crystal holder 31 is uniformly provided with a plurality of temperature measuring points, and the temperature of the seed crystal holder 31 is accurately regulated and controlled by detecting the temperature of the seed crystal holder 31 and feeding back to the seed crystal module temperature control mechanism 32.
The expanded-diameter crystal growth ring 33 is arranged below the seed crystal holder 31, and the expanded-diameter crystal growth ring 33 limits the growth cavity 34 and plays a role in guiding sublimated raw material gas. Therefore, the inner diameter of the hollow growth chamber 34 formed around the expanded growth ring 33 is gradually increased from top to bottom, so that the growth chamber 34 under the seed crystal is gradually increased from top to bottom. The diameter of the growth cavity 34 formed by encircling the top of the expanded diameter crystal ring 33 is not smaller than the diameter of the seed crystal support 31, so that the silicon carbide crystal can grow in an expanded diameter mode, the influence of the expanded diameter crystal ring 33 during the growth and expansion of the silicon carbide crystal is avoided, the crystal stress is reduced, the cracks of the edge of the silicon carbide crystal are reduced, the generation of edge polycrystal is prevented, and the silicon carbide crystal with high quality and large diameter can be grown.
In some preferred embodiments, the crucible cover 11 has a hollow structure, and a plurality of first through holes 111 are provided corresponding to a plurality of temperature measuring points on the seed crystal support 31, so as to facilitate connection between the connection line of the seed crystal module temperature control mechanism 32 and the temperature measuring points on the seed crystal support 31. In a more preferred embodiment, a cooling gas is introduced into the first through hole 111 to cooperate with the seed crystal module temperature control mechanism 32 to adjust the temperature of the seed crystal holder 31, so that the temperature of each temperature measuring point on the seed crystal holder 31 is simply controlled by the flow of the cooling gas, and the temperature of the seed crystal holder 31 is accurately adjusted and controlled.
As shown in fig. 3, in some embodiments, the expanded-diameter crystal ring 33 is a side ring with a hollow interior, and the side wall of the expanded-diameter crystal ring 33 connected to the crucible 12 is provided with a second through hole 331, where the second through hole 331 transversely penetrates through the heating side wall 21 and the side wall of the crucible 12, so that the hollow interior of the expanded-diameter crystal ring 33 is communicated with the exterior of the silicon carbide crystal growth device, and is suitable for introducing external cooling gas, and the cooling gas can enter the interior of the expanded-diameter crystal ring 33, thereby facilitating the growth of the silicon carbide crystal by cooling. The expanded-diameter long crystal ring 33 is connected with the heater 5, the temperature control system 6 and the cooling gas flow controller, so that the temperature detection accuracy of the expanded-diameter long crystal ring 33 can be improved.
The inner wall of the expanded-diameter crystal growth ring 33 extends out of the baffle strip 332, so that the contact area between the cooling gas and the expanded-diameter crystal growth ring 33 is increased, and the cooling effect is improved. The structure design of the expanded-diameter crystal growth ring 33 and the combination of the expanded-diameter crystal growth ring 33 with the heater 5 and the temperature control system 6 enable the temperature adjustment of the expanded-diameter crystal growth ring 33 to be more accurate, thereby being beneficial to the improvement of the quality of large-diameter silicon carbide crystals and avoiding the problems of edge cracking, phase change and the like.
Preferably, the expanded diameter crystal ring 33 is made of tungsten or tantalum, so that the use of graphite is reduced, the phenomenon of unbalance of silicon-carbon ratio in the process of decomposing silicon carbide raw materials is avoided by providing extra carbon source for crystal growth, the carbon package entering the inside of the crystal is reduced, and the quality and yield of the crystal are improved.
The source unit 4 comprises a filter vat 41, a source chamber 42 is formed between the filter vat 41 and the inner wall of the crucible vat 12, the source chamber 42 comprises more than one independent chamber, and each chamber is suitable for placing the growth source of silicon carbide crystal. The buffer chamber 43 is defined between the walls of the filter drum 41, so that sublimated raw materials are mixed more fully and more uniformly in the buffer chamber 43 and then rise to the seed crystal for crystallization.
The filter tub 41 includes a filter top plate 411 and a filter side plate 412, and the filter top plate 411 is disposed at the top end of the raw material chamber 42 and is disposed laterally inward along the inner wall of the crucible tub 12. The filtering side plate 412 extends downwards from the end of the filtering top plate 411 to the bottom of the crucible 12, so that the growth raw materials in each chamber pass through the filtering top plate 411 or the filtering side plate 412 to enter the buffer chamber 43, and finally are transported to the seed crystal holder 31 for crystal growth.
Preferably, the filtering side plate 412 comprises a first side plate and a second side plate, the inner diameter of a first buffer cavity formed by surrounding the first side plate is gradually increased from bottom to top, the second side plate is connected with the first side plate and the bottom of the crucible barrel 12, and the inner diameter of a second buffer cavity formed by surrounding the second side plate is unchanged. The volume of the first buffer cavity near the growth unit 3 gradually increases, which is beneficial to the crystallization of sublimated raw materials at the seed crystal slowly.
Preferably, the material of the filter vat 41 is porous graphite, and the gas component Si after the growth raw material is decomposed and sublimated at high temperature m C n The silicon carbide crystal can be crystallized and grown by being transported to a seed crystal interface through a porous graphite barrel.
The feedstock chamber 42 includes a plurality of separate chambers that separate the growth feedstock of silicon carbide into a plurality of separate feedstock layers and a heater 5 and temperature control system 6 are provided for each chamber accordingly to detect and control the rate of evaporation and decomposition of the growth feedstock in each chamber and thereby control the rate of crystal growth.
The design that a plurality of cavities set up and independent accuse temperature can make the even decomposition of growth raw materials in the cavity, avoids growth raw materials to decompose earlier stage and the gas composition of decomposition later stage and changes too big, is favorable to reducing the silicon-carbon ratio.
The design of a plurality of chambers and independent temperature control is beneficial to regulating the decomposition rate of the growth raw materials according to the crystallization rate of the crystals, avoiding excessive decomposition of the growth raw materials and rapid crystallization at the seed crystal, and the chambers can independently control the decomposition rate of the growth raw materials in the chambers and slow down the decomposition rate of the growth raw materials, so that the crystallization rate of the crystals is slowed down, the growth of the silicon carbide crystals with higher quality is facilitated, and the crystal yield is improved.
In some preferred embodiments, a thermal insulation blanket 44 is disposed between two adjacent chambers, the thermal insulation blanket 44 separating the growth materials to form separate chambers and preventing thermal conduction between the growth materials, so that the growth materials in each chamber can be independently controlled in temperature.
The interlayer vent holes 45 are formed in the interlayer insulating felt 44, and the interlayer vent holes 45 transversely penetrate through the interlayer insulating felt 44 and the crucible barrel 12, so that the heat blocking effect of the interlayer insulating felt 44 is enhanced, heat is prevented from being transferred between adjacent chambers, and the temperature of each chamber is controlled more accurately.
Correspondingly, a plurality of heaters 5 and temperature control systems 6 are provided to independently detect and control the temperature of the growth materials in each chamber.
The heater 5 is provided at the outer circumferential side of the heating tub 2 to uniformly surround the heating tub 2, and the heater 5 can better control the heating temperature, and the heating heats up the heating tub 2 and transfers heat into the crucible tub 12, so that the growth raw material in the raw material chamber 42 is decomposed.
The temperature control system 6 is connected with the heater 5, and the temperature control system and the heater are matched to detect the temperature inside the crucible barrel 12 and feed back and adjust the decomposition temperature of the growth raw materials. Preferably, a detection hole 65 is provided, and the detection hole 65 penetrates through the heating barrel 2 so as to directly detect the temperature of each chamber, so that temperature control is more accurate, and a detection line is conveniently connected.
In some embodiments, the feedstock cavity 42 includes at least three separate chambers. The feed chamber 42 includes an upper chamber 421, a middle chamber 422, and a lower chamber 423. Accordingly, the heater 5 includes an upper induction heater 51, a middle induction heater 52, and a lower induction heater 53. The temperature control system 6 includes an upper heating temperature control system 61, a middle heating temperature control system 62, and a lower heating temperature control system 63. The plurality of heaters 5 and the plurality of temperature control systems 6 are positioned in a one-to-one correspondence with the plurality of raw material chambers 42.
Specifically, the upper heating temperature control system 61 detects the temperature of the upper chamber 421 and controls the upper induction heater 51 so that the decomposition rate of the growth material in the upper chamber 421 can be precisely controlled. The central heating temperature control system 62 detects the temperature of the central chamber 422 and controls the heating temperature of the central induction heater 52 so that the decomposition rate of the feedstock within the central chamber 422 can be precisely regulated. The lower heating temperature control system 63 detects the temperature of the lower chamber 423 and controls the heating temperature of the lower induction heater 53 so that the decomposition rate of the growth material in the lower chamber 423 can be precisely controlled.
In some embodiments, the heater 5 further comprises a grower ring induction heater 54, and the temperature control system 6 further comprises a grower ring heating temperature control system 64, wherein the grower ring induction heater 54 is disposed at the periphery of the expanded grower ring 33 and connected to the grower ring heating temperature control system 64 for detecting and controlling the temperature of the expanded grower ring 33.
In some embodiments, the crucible barrel 12 may be moved up and down to enable the source chamber 42 to be moved closer to or farther from the seed holder 31. As shown in fig. 4, in a specific implementation manner, for example, a telescopic mechanism 13 is arranged below the crucible cover 11, a supporting tray 23 and a lifting device 24 are arranged at the lower end of the heat preservation felt 22, and the lifting device 24 is connected to the bottom of the supporting tray 23 so that the crucible 12 can move up and down relative to the seed crystal holder 31. The telescopic mechanism 13 is arranged below the expanded-diameter crystal growing ring 33, and under the traction of the lifting device 24, the supporting tray 23 drives the heat preservation felt 22 to move, so that the telescopic mechanism 13 stretches, the crucible barrel 12 is separated from the crucible cover 11, and the raw material cavity 42 is further away from the seed crystal support 31.
The liftable design of the raw material unit 4 can enable the silicon carbide crystal growth process to be more stable, supersaturated vapor formed after sublimation of the growth raw material can not change due to the change of the volume of the growth cavity 34, the growth speed of the crystal can not be influenced, and the high-quality silicon carbide crystal can be grown.
Preferably, in order to avoid the detection deviation of the temperature control system 6 during the lifting movement of the crucible 12, a plurality of detection holes 65 are provided on the inner wall of the heating barrel 2, so as to detect the temperature of the raw material unit 4 after the lifting movement of the crucible 12.
The application provides a silicon carbide crystal growth method, which comprises the following three steps:
s1: setting the temperature of each chamber respectively;
s2: controlling the descending speed of the crucible barrel, and respectively adjusting the temperature of each chamber;
s3: gradually reducing the crystal growth pressure, maintaining the descending speed, and respectively adjusting the temperature of each chamber.
Preferably, the steps S1, S2 and S3 are maintained for 30-50 hours, so that the severe influence of temperature change on crystal growth is avoided.
Preferably, the lifting device is linked with the downward moving speed of the raw material cavity in the crucible to be 0.1-0.3 mm/min.
The S1 specifically comprises the following steps: introducing inert gas into the silicon carbide crystal growth device to maintain the growth pressure of the silicon carbide crystal at 150-250 pa, controlling the temperature of the central point of the seed crystal support at 2000-2400 ℃, respectively setting two temperature measuring points at two sides of the center, and controlling the temperature gradient between each temperature measuring point and the central point at 1-3 ℃/cm; introducing cooling gas into the expanded-diameter crystal growth ring, setting the temperatures of the expanded-diameter crystal growth ring and the upper chamber to 2000-2500 ℃, and setting the temperatures of the middle chamber and the lower chamber to 1200-1800 ℃; and maintaining S1 step 40h.
The step S2 specifically comprises the following steps: maintaining the crystal growth pressure at 150-250 pa, controlling the lifting device to separate the raw material cavity from the growth cavity, and downwards moving the raw material cavity to be far away from the seed crystal support, wherein the downwards moving speed of the lifting device is 0.1-0.3 mm/min; raising the temperature of the upper chamber, the middle chamber and the lower chamber; and maintaining S2, step 40h.
The step S3 specifically comprises the following steps: slowly reducing the growth pressure of the crystal to 100-150 pa, keeping the same downward moving speed of S2 by a lifting device, and raising the temperature of a middle chamber and a lower chamber; maintaining the step S3 for 40h to obtain the silicon carbide crystal prepared by the application.
Example 1
A silicon carbide crystal growth apparatus a shown in fig. 1 was used.
The silicon carbide crystal growth method comprises the following steps:
s1: introducing inert gas into the crucible to maintain the growth pressure of the silicon carbide crystal at 200pa, controlling the temperature of the central point of the seed crystal support at 2200 ℃, respectively setting two temperature measuring points at two sides of the center, and controlling the temperature gradient between each temperature measuring point and the central point at 1 ℃/cm; introducing cooling gas into the expanded crystal ring, setting the temperature of the expanded crystal ring to 2210+/-2 ℃, setting the temperature of an upper chamber to 2250+/-2 ℃, setting the temperature of a middle chamber to 1600+/-2 ℃ and setting the temperature of a lower chamber to 1300+/-2 ℃; maintaining S1, namely maintaining the step 40h;
s2: maintaining the crystal growth pressure at 200pa, controlling the lifting device to separate the raw material cavity from the growth cavity, and downwards moving the raw material cavity to be far away from the seed crystal support, wherein the downwards moving speed of the lifting device is 0.2mm/min; raising the temperature of the upper chamber to 2260+/-2 ℃, uniformly raising the temperature of the middle chamber to 2250+/-2 ℃ in 40h, and uniformly raising the temperature of the lower chamber to 1600+/-2 ℃ in 40h; maintaining S2 for 40h;
s3: slowly reducing the growth pressure of the crystal to 150pa in 40h, keeping the same downward moving speed of S2 by a lifting device, uniformly increasing the temperature of a middle chamber to 2260+/-2 ℃ in 40h, and uniformly increasing the temperature of a lower chamber to 2280+/-2 ℃ in 40h; maintaining the step S3 for 40h to obtain the silicon carbide crystal A prepared by the method.
Comparative example 1
A silicon carbide crystal growth apparatus B as shown in fig. 5 was employed in which the source chamber was a monolithic chamber and was not partitioned into a plurality of independent chambers.
The silicon carbide crystal growth method was identical to that in example 1, and a silicon carbide crystal B was obtained by growth.
Comparative example 2
A silicon carbide crystal growth apparatus C shown in fig. 6 was employed in which the expanded diameter growth ring had a hollow closed structure.
In the silicon carbide crystal growth method, cooling gas is not introduced into the expanded-diameter crystal ring, the step of adjusting the temperature of the expanded-diameter crystal ring is removed in the step S1-S3, the temperature of the expanded-diameter crystal ring is freely changed under the heating of a heating barrel, the temperature is basically maintained at 2300-2600 ℃, and a silicon carbide crystal C is obtained through growth.
Comparative example 3
A silicon carbide crystal growth apparatus D as shown in fig. 7 was employed in which the inside diameter of the filter vat was unchanged.
The silicon carbide crystal growth method was identical to that in example 1, and a silicon carbide crystal D was obtained by growth.
Comparative example 4
A silicon carbide crystal growth apparatus a shown in fig. 1 was used.
In the steps of the silicon carbide crystal growing methods S1-S3, the step of slowly descending the raw material cavity is eliminated, the distance between the raw material cavity and the seed crystal support is kept unchanged, and the silicon carbide crystal F is obtained through growth.
Analysis of Crystal growth results
Silicon carbide crystal a: as shown in FIG. 8, the crystal was grown with successful expansion, 150mm seed was expanded to 175mm, convexity was 3.5mm, and growth rate was 0.12mm/h. The crystal quality is good, no obvious cracks are observed at the edges, and polycrystal is not generated.
Silicon carbide crystal B: as shown in fig. 9, the silicon carbide crystal B grew too fast to be polycrystalline, and the expanding growth failed;
silicon carbide crystal C: as shown in FIG. 10, the silicon carbide crystal C was grown with successful expansion, 150mm seed crystal expansion to 173mm, convexity of 8.9mm and growth rate of 0.13mm/h. The edge of the crystal is cracked by 5-7 mm due to the overlarge convexity.
Silicon carbide crystal D: as shown in fig. 11, seed ablation failed to expand the growth.
Silicon carbide crystal F: as shown in FIG. 12, the silicon carbide crystal F was grown with successful expansion, 150mm seed crystal expansion to 175mm, convexity of 6.5mm and growth rate of 0.07mm/h. The silicon carbide crystal growth rate was too slow, about 1/2 of that of the silicon carbide crystal a in example 1, too slow growth rate consumed excessive resources, and production rate was low, which was disadvantageous for mass production.
The silicon carbide crystal growth device can enable the silicon carbide crystal to grow in an expanded mode, obtain the silicon carbide crystal with a large diameter, and is good in crystal quality, small in convexity and free of polycrystalline or edge crack. The growth speed of the silicon carbide crystal is moderate, which is beneficial to improving the production efficiency and saving the resource consumption.
The foregoing has outlined the basic principles, features, and advantages of the present application. It will be understood by those skilled in the art that the present application is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present application, and various changes and modifications may be made therein without departing from the spirit and scope of the application, which is defined by the appended claims. The scope of the application is defined by the appended claims and equivalents thereof.
Claims (10)
1. The silicon carbide crystal growth device comprises a crucible unit, a growth unit and a raw material unit, wherein the crucible unit comprises a crucible cover and a crucible barrel, the growth unit is arranged below the crucible cover, and the raw material unit is arranged in the crucible barrel, the silicon carbide crystal growth device is characterized in that the raw material unit comprises a filter barrel, a raw material cavity for placing growth raw materials of crystals is formed between the inner wall of the crucible barrel and the filter barrel, a buffer cavity is defined by the outer wall of the filter barrel, the growth raw materials enter the buffer cavity through the filter barrel after sublimating,
the raw material cavity comprises more than one independent cavity, each cavity is arranged up and down along the buffer cavity, and independent heaters are respectively arranged outside each cavity to realize independent heating.
2. A silicon carbide crystal growth apparatus according to claim 1, wherein a barrier thermal insulation blanket is disposed between each adjacent chamber, the barrier thermal insulation blanket having a barrier vent disposed therethrough in a transverse direction, the barrier vent adapted to reduce heat transfer between each adjacent chamber.
3. The silicon carbide crystal growth apparatus of claim 1, wherein the filter barrel comprises a filter top plate and a filter side plate, the filter top plate is disposed on an upper portion of the feed cavity, the filter side plate is disposed on a side portion of the feed cavity, the filter side plate comprises a first side plate and a second side plate, a first buffer cavity formed by surrounding the first side plate is gradually reduced in diameter from top to bottom, and a second buffer cavity formed by surrounding the second side plate is unchanged in diameter.
4. A silicon carbide crystal growth apparatus according to claim 1, wherein a temperature control system is further provided outside each of the chambers, the temperature control system being electrically connected to the heater and adapted to cooperate with the heater to detect and regulate the temperature of each of the chambers.
5. The silicon carbide crystal growth apparatus of claim 1, wherein the growth unit comprises a seed crystal holder disposed below the crucible cover, and an expanded-diameter crystal ring disposed below the seed crystal holder, the expanded-diameter crystal ring having a hollow structure and having a plurality of ribs extending on an inner wall, the expanded-diameter crystal ring being in communication with the outside through a plurality of second through holes, and a cooling gas adapted to enter the inside of the expanded-diameter crystal ring from the second through holes to adjust a temperature of the expanded-diameter crystal ring.
6. The silicon carbide crystal growth apparatus of claim 4, wherein the heater comprises a grower ring induction heater, the temperature control system comprises a grower ring heating temperature control system, and the grower ring induction heater, the grower ring heating temperature control system and the cooling gas flow rate are cooperatively regulated to realize detection and regulation of the expanded diameter grower ring temperature.
7. The silicon carbide crystal growth apparatus of claim 1, wherein the growth unit further comprises a seed holder and a seed module temperature control mechanism, the crucible cover being provided with a plurality of first through holes therethrough vertically, the seed module temperature control mechanism passing through the first through holes to detect the temperature of the seed holder, the first through holes being further adapted to be fed with a cooling gas to adjust the temperature of the seed holder.
8. The silicon carbide crystal growth apparatus of claim 1, wherein the crucible barrel is adapted to move up and down such that the feedstock unit is relatively far from or near to the growth unit.
9. The silicon carbide crystal growth apparatus of claim 8, further comprising a heating barrel outside the crucible unit, the heating barrel comprising a support tray, the crucible barrel being disposed on the support tray, the lifting device being coupled to the support tray to move the crucible barrel up and down so that the feedstock unit and the growth unit can be moved relatively far apart or closer together.
10. A method for growing a silicon carbide crystal using the apparatus according to any one of claims 1 to 9, comprising the steps of,
s1: setting the temperature of each chamber respectively;
s2: controlling the descending speed of the crucible barrel, and respectively adjusting the temperature of each chamber;
s3: gradually reducing the crystal growth pressure, maintaining the descending speed, and respectively adjusting the temperature of each chamber.
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