CN118028969B - Device and method for growing silicon carbide single crystal - Google Patents
Device and method for growing silicon carbide single crystal Download PDFInfo
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- CN118028969B CN118028969B CN202410431329.7A CN202410431329A CN118028969B CN 118028969 B CN118028969 B CN 118028969B CN 202410431329 A CN202410431329 A CN 202410431329A CN 118028969 B CN118028969 B CN 118028969B
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- 239000013078 crystal Substances 0.000 title claims abstract description 92
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000007789 sealing Methods 0.000 claims abstract description 17
- 230000000694 effects Effects 0.000 claims abstract description 5
- 230000005484 gravity Effects 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000002093 peripheral effect Effects 0.000 claims 1
- 239000000428 dust Substances 0.000 abstract description 9
- 235000012431 wafers Nutrition 0.000 description 7
- 238000013461 design Methods 0.000 description 6
- 230000000149 penetrating effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000013022 venting Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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
-
- 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
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- 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 belongs to the technical field of growing silicon carbide single crystals, and particularly relates to a device and a method for growing silicon carbide single crystals, wherein the device comprises an exhaust assembly arranged on the outer surface of a crucible cover, and the exhaust assembly comprises: the support frame is arranged on the upper surface of the part of the crucible cover close to the exhaust channel, and the middle part of the support frame is provided with a guide hole; the support frame is in a cover shape and covers the periphery above the exhaust channel; the lifting rod penetrates out of the support frame along the guide hole to extend upwards continuously, and a first weight is sleeved at the extending end of the lifting rod; and the upper part of the first sphere is fixed at the bottom of the lifting rod, and the lower part of the first sphere is propped against the upper part of the exhaust channel. The invention can maximally discharge residual gas in the crucible, promote sealing effect, prevent the phenomenon that inclination is blocked due to high-temperature deformation, dust adhesion and the like of the lifting mechanism, has good durability, ensures high-quality stable growth of silicon carbide single crystals, has long service life, and can flexibly adapt to the growth of large-size silicon carbide single crystals with different specifications.
Description
Technical Field
The invention belongs to the technical field of growing silicon carbide single crystals, and particularly relates to a device and a method for growing silicon carbide single crystals.
Background
At present, a physical vapor transport method (PVT method) has become a mainstream process technology for growing silicon carbide single crystals, and the technology is characterized in that silicon carbide polycrystalline raw materials are filled in a closed cavity formed by a crucible body (such as a graphite crucible) and a crucible cover in a vacuum environment or an atmosphere environment, the crucible body and the crucible cover are arranged together to form a crucible, a seed crystal sheet is adhered to the inner wall of the crucible cover, and the silicon carbide polycrystalline raw materials at the bottom of the crucible body are heated and sublimated, so that the silicon carbide single crystals grow on silicon carbide seed crystals.
In the process of the silicon carbide single crystal growth technology, the air in the crucible needs to be pumped out to form a vacuum environment, and the silicon carbide raw material in the crucible is required not to run out during crystal growth, so that the stable growth of the silicon carbide single crystal is ensured. There is a crucible with a lifting assembly in the prior art. However, in the practical use process of the lifting assembly, under certain scenes, the technical problem that the quality of the produced single crystal is poor after the silicon carbide single crystal grows for a long time still exists.
It should be noted that this section of the disclosure only provides a background related to the present disclosure, and does not necessarily constitute prior art or known technology.
Disclosure of Invention
The inventor of the invention has found through a great deal of research that for the growth of silicon carbide single crystals with different sizes (especially large sizes), under the same production process conditions, the quality of the single crystals produced after long-time use is poor, and further has found that, in the growth of the silicon carbide single crystals with large sizes, the cavity of the crucible body is larger, the raw material loading amount is more, and the air in the crucible is difficult to be pumped out when the crucible body and the crucible cover are arranged together and are in relatively airtight vacuum pumping, so that residual air is often generated, namely the residual air is difficult to be thoroughly exhausted, further the influence on the quality of the grown single crystals is larger, and the high-quality stable growth of the silicon carbide single crystals with large sizes cannot be ensured. Even with the design of the lift assembly, this problem is not effectively solved during large-scale silicon carbide growth, as set forth in the background section above. The inventor finds that in the growth process of large-size silicon carbide, after long-time use, the lifting assembly of the silicon carbide can have the problems of insufficient exhaust and poor sealing caused by blocking during exhaust. According to analysis, the lifting assembly is designed to be suspended and penetrates through the crucible cover to be in contact with the crucible body, and the gap at the penetrating position is small (the gap is small due to the need of avoiding air leakage), so that in the process of growing silicon carbide with large size for many times, the suspended lifting mechanism is more easily inclined and clamped in the gap at the penetrating position due to uneven thermal deformation or high-temperature dust bonding, and further the phenomenon that the air is blocked during air discharge in certain scenes is caused to be insufficient, the silicon carbide is not tightly sealed during growth, and then the silicon carbide single crystal cannot stably grow with high quality is caused.
In addition, when facing large-size silicon carbide single crystals with different specification requirements (corresponding to different sizes), the generated air pressure is different, the residual air allowance is different, the existing lifting assembly cannot be suitable for exhausting under the growth condition of the silicon carbide single crystals with different specifications, and the device cannot be flexibly adjusted to adapt to the problem of high-quality stable growth of the large-size silicon carbide single crystals with different specifications.
The invention aims to overcome the defect that the silicon carbide single crystal cannot stably grow with high quality after long-time use in the prior art, and provides a device and a method for growing the silicon carbide single crystal, which can remarkably improve the vacuumizing effect, maximize the discharge of residual gas in a crucible, improve the sealing effect, prevent the phenomenon that the silicon carbide single crystal is clamped due to high-temperature deformation and dust bonding of a lifting mechanism and the design of a suspended lifting mechanism, and further ensure that the silicon carbide single crystal with large size is high-quality and stably grown with good durability, and have long service life and can flexibly adapt to the growth of the silicon carbide single crystal with large size with different specifications.
In order to achieve the above object, in a first aspect, the present invention provides an apparatus for growing silicon carbide single crystals, comprising a crucible body and a crucible cover, wherein the middle part of the lower surface of the crucible cover is used for mounting seed wafers, an exhaust channel extending along a vertical direction is formed in an edge area of the periphery of the middle part of the crucible cover, the crucible body and the crucible cover form a crucible, and an exhaust assembly arranged on the outer surface of the crucible cover is further provided.
The exhaust assembly of the present invention includes:
The support frame is arranged on the upper surface of the part of the crucible cover close to the exhaust channel, the middle part of the support frame is provided with a guide hole, and the guide hole and the central axis of the exhaust channel are positioned on the same vertical line; the support frame is in a cover shape and covers the periphery above the exhaust channel;
the lifting rod penetrates out of the support frame along the guide hole to extend upwards continuously, a first weight is sleeved at the extending end of the lifting rod, and the lower surface of the first weight is not contacted with the support frame;
The upper part of the first ball body is fixed at the bottom of the lifting rod, the lower part of the first ball body is propped against the upper part of the exhaust channel, the first ball body can automatically fall down to form a seal through gravity under the natural state without vacuumizing, and the first ball body can be sucked upwards when the crucible is vacuumized, and the air in the crucible is discharged outwards through the exhaust channel.
In some preferred embodiments of the present invention, the upper portion of the exhaust passage is an inner concave surface, and the inner concave surface is arc-shaped or tapered.
Further preferably, the radial dimension of the concave surface increases sequentially from bottom to top.
Further preferably, the shape of the concave surface is the same as the outer contour of the partial sphere of the first sphere.
Further preferably, the lower portion of the exhaust passage is cylindrical, and the radial dimension of the cylindrical portion is smaller than the radial dimension of the concave surface.
In some preferred embodiments of the present invention, the upper portion of the lifting rod continues to extend upward along the first weight, and a plurality of second weights continue to be sleeved on the extending end.
In some preferred embodiments of the invention, the radial dimension of the guide hole is smaller than the radial dimension of the exhaust passage.
In some preferred embodiments of the invention, the first weight is fixed to the lifting rod.
In some preferred embodiments of the present invention, the first weight is movably sleeved on the lifting rod, and a baffle is fixedly arranged on the lifting rod, and the baffle is located between the first weight and the supporting frame and is not in contact with the supporting frame.
In some preferred embodiments of the present invention, the cover-shaped circumferential direction is provided with vent holes.
In some preferred embodiments of the present invention, the apparatus for growing a silicon carbide single crystal further comprises a single crystal growth furnace, a heater, the crucible being disposed within a working chamber of the single crystal growth furnace, the heater being located between the crucible and a furnace wall of the single crystal growth furnace.
In a second aspect, the present invention provides a method of growing a silicon carbide single crystal, which is carried out in the apparatus for growing a silicon carbide single crystal according to the first aspect, and which comprises the steps of:
the method comprises the steps of putting raw materials into a crucible body in advance, and installing an exhaust assembly on a crucible cover so that a first sphere abuts against an exhaust channel of the crucible cover; then the crucible cover and the crucible body are connected together to form a crucible with a relatively closed space; placing the crucible in a working cavity of a single crystal growth furnace;
Then, the working cavity is vacuumized, the vacuumized suction force is larger than the integral gravity of the first sphere, the lifting rod connected with the first sphere and the first weight, the first sphere is sucked upwards, air in the crucible is discharged through the opened exhaust channel, when the target vacuum degree is pumped, the pressure in the crucible is equal to the pressure in the working cavity, and the first sphere naturally falls into the upper part of the exhaust channel under the action of the integral gravity of the first sphere, the lifting rod connected with the first weight, so that the crucible is sealed, and the air pumping and discharging work in the crucible is completed;
and then introducing process gas into the working cavity, starting heating, and performing crystal growth.
In some preferred embodiments of the present invention, the method of growing a silicon carbide single crystal further comprises: according to the air pressure generated by the silicon carbide monocrystal with the required size in the working cavity, a plurality of second weights with the required gravity are sleeved on the upper part of the lifting rod of the exhaust assembly, are used for naturally falling down to seal the crucible, and can be sucked up during vacuumizing.
The beneficial effects are that:
According to the invention, the exhaust component with a specific structure is arranged on the outer surface of the crucible cover close to the edge area, and particularly, the very fragile lifting rod and the penetrating part of the guide hole where the lifting rod is positioned are far away from the crucible cover and the high-temperature area in the center of the crucible, so that the phenomena of insufficient exhaust and poor sealing when silicon carbide grows due to clamping rods caused by high-temperature deformation and high Wen Nianlian are effectively avoided, and the service life is prolonged; the cooperation is used for sealed first spheroid offset in exhaust passage's upper portion sets up on the side of crucible lid surface for first spheroid keeps away from the high temperature region at crucible center, prevents high temperature deformation, even if still has better sealing performance and exhaust performance after long-term use, and the sphere design, even if can glue a bit dust after using for a long time, first spheroid also can be automatic leveling sealed exhaust passage promptly self-sealing nature is good, still does not influence the use. Moreover, on the one hand, still set up the support frame and be the cover form and cover in exhaust passage's top periphery, the design of cover can block the dust, prevents that the dust from bonding on first spheroid, further promotes exhaust assembly life. On the other hand, under the limiting action of the guide hole of the support frame, the lifting rod and the first ball body thereof are effectively guided, so that the lifting rod and the first ball body thereof fix a lifting route, and the exhaust is sufficient and the service life is long. The lifting rod of the original lifting assembly columnar design is prevented from being clamped by the existing design of penetrating through the crucible cover, dust is bonded, and the problems of uncleanness in air extraction, untight sealing and short service life are further caused. The invention can maximally and rapidly extract the air in the crucible under the condition of not affecting the temperature environment of the single crystal growth interface, improve the working environment in the crucible, better meet the requirement of the crystal growth process, and ensure that the raw materials or the evaporating gas in the crucible cannot escape in the crystal growth process, thereby realizing high-quality and stable growth of large-size silicon carbide single crystals under the condition of long-time use.
In addition, the first weight is arranged on the upper part of the lifting rod (or the second weight is preferably matched with the lifting rod), so that silicon carbide with different sizes can be flexibly used for growth, and the application range is wide.
The invention has simple structure, easy manufacture, stable performance and high repeatability, can be widely applied to stable and high-quality growth of large-size silicon carbide single crystals, and has long service life.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural view showing an embodiment of an apparatus for growing a silicon carbide single crystal according to the present invention.
Description of the reference numerals
1. The crucible comprises a crucible body, 2, a crucible cover, 3, an exhaust channel, 4, an inner concave surface, 5, a first sphere, 6, a support frame, 7, an exhaust hole, 8, a lifting rod, 9, a first weight, 10, a guide hole, 11, a seed crystal sheet, 12 and a raw material.
Detailed Description
In the present invention, unless otherwise indicated, terms of orientation such as "upper, lower, left, right" and the like are used generally to refer to the orientation understanding shown in the drawings and in practice, and "inner, outer" refer to the inner, outer of the outline of the components.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein. Wherein the terms "optional" and "optionally" mean either comprising or not comprising (or may not be present).
In a first aspect, the present invention provides an apparatus for growing silicon carbide single crystals, as shown in fig. 1, comprising a crucible body 1 and a crucible cover 2, wherein the middle part of the lower surface of the crucible cover 2 is used for mounting a seed wafer 11, an exhaust channel 3 extending along the vertical direction is formed on the edge area of the middle periphery of the crucible cover 2, the crucible body 1 and the crucible cover 2 form a crucible, and an exhaust assembly arranged on the outer surface of the crucible cover 2 is further included. The exhaust component is far away from the high-temperature area in the center of the high-temperature crucible cover 2 and the crucible body 1, and can prevent the sealability from being reduced due to long-time thermal deformation, thereby affecting the stable growth of the silicon carbide single crystal.
It will be appreciated that the crucible cover 2 is disposed on top of the crucible body 1 and is connected to each other in a sealed manner, so as to form a relatively airtight space in the crucible. The polycrystalline raw material 12 for placing silicon carbide in the crucible body 1 grows a single crystal under the induction of a seed wafer 11 (e.g., a silicon carbide seed wafer).
The exhaust assembly of the present invention includes: a supporting frame 6, a lifting rod 8 and a first sphere 5.
The support frame 6 is installed on the upper surface of the partial crucible cover 2 close to the exhaust channel 3, and the middle part of the support frame is provided with a guide hole 10, and the guide hole 10 and the central axis of the exhaust channel 3 are positioned on the same vertical line, so that smooth lifting movement of the first ball 5 is controlled. The supporting frame 6 is in a cover shape and covers the periphery above the exhaust channel 3, which is favorable for preventing dust adhesion and ensuring effective sealing and smooth exhaust after long-time use. And the guide hole 10 is far away from the high temperature area, so that the high-temperature deformation of the lifting rod 8 in the guide hole 10 and the conditions of inclined blocking and blocking of the exhaust component caused by the adhesion of pollutant high-temperature deposition can be effectively prevented, the air suction is cleaner, the sealing is tighter, and no problem exists in long-time use.
The lifting rod 8 is extended upwards continuously by the lifting rod 6 outwards penetrating out along the guide hole 10 so as to limit the moving direction of the first ball 5, and the moving direction of the first ball 5 is unchanged after long-time use, so that the lifting rod is still effectively sealed and smoothly exhausted after long-time use, is far away from a high-temperature area, and prevents clamping rods and other problems caused by high-temperature deformation and adhesion. The extending end of the lifting rod 8 is sleeved with a first weight 9, the lower surface of the first weight 9 is not contacted with the supporting frame 6, the gravity of the first weight 9 can be completely transferred onto the first ball 5, and the phenomenon that the supporting frame 6 counteracts the gravity of the first weight 9 to cause the sealing of the first ball 5 to be not tight is avoided. The invention can also adjust the weight of the first weight 9 according to the difference of the air pressure caused by the size of the single crystal.
The upper part of the first ball 5 is fixed at the bottom of the lifting rod 8, the lower part of the first ball is propped against the upper part of the exhaust channel 3, the first ball can automatically fall down to form a seal by gravity under the natural state without vacuumizing, and the first ball 5 can be sucked upwards when the crucible is vacuumized, and the air in the crucible is discharged outwards through the exhaust channel 3. The first sphere 5 can automatically level and seal the exhaust channel 3, namely, the self-sealing performance is good, specifically, even if the upper part of the first sphere 5 is partially adhered under special conditions, the first sphere 5 can also form effective sealing against the exhaust channel 3 through other parts of the sphere, so that the self-adaptive sealing under various conditions is realized, and the high-quality stable growth of the silicon carbide single crystal is ensured.
In the invention, the first ball 5 can automatically fall to close the exhaust channel 3 through the integral gravity of the first ball 5 and the lifting rod 8 and the first weight 9 connected with the first ball under the natural state without vacuumizing, wherein the natural state without vacuumizing refers to any state without vacuumizing before and during and after growth of silicon carbide single crystals, and under the states, the exhaust assembly can balance the acting force ranges under different states without vacuumizing and can automatically fall to close the exhaust channel 3 through self gravity, so that the crucible is sealed. When the vacuum pumping needs to be exhausted, the first ball body 5 is jacked up under the action of the pressure difference between the inside and the outside of the crucible, the exhaust channel 3 is opened, and the gas in the crucible is exhausted from the exhaust channel 3 and then exhausted from the guide hole 10 (preferably additionally provided with the exhaust hole 7).
The material of the exhaust component provided by the invention only needs to meet the requirements that the exhaust component can automatically fall down to seal the exhaust channel 3 through self gravity under the natural state without vacuumizing, and can be sucked upwards during vacuumizing, and the air in the crucible can be discharged through the exhaust channel 3.
It can be understood that the exhaust components are in one-to-one correspondence with the exhaust channels 3, which is beneficial to stably exhausting the air in the crucible and realizing effective sealing. Preferably, the venting channels 3 and their mating venting assemblies are evenly spaced along the circumference of the crucible cover 2.
The first sphere 5 of the invention is propped against the upper part of the exhaust channel 3 and is obviously higher than the end surface height of the seed wafer 11 arranged on the lower surface of the crucible cover 2, namely, the lifting rod 8 and the first sphere 5 thereof are far away from the seed wafer 11 and the high temperature area of the single crystal growth interface thereof, the temperature of the first sphere 5 is low, even if the crucible is used for a long time, the silicon carbide is still prevented from being deposited on the first sphere 5, the adhesion and the silicon carbide loss caused by the silicon carbide deposition are avoided, and the single crystal is further promoted to intensively grow on the seed wafer 11 arranged on the end surface of the middle part of the lower surface of the crucible cover 2, so that the stable and high-quality growth of the single crystal is further promoted. And the guide hole 10 is far away from the high temperature area, so that the conditions of inclined clamping, adhesion clamping and the like of the exhaust component caused by high-temperature deposition adhesion of pollutants and the like of the lifting rod 8 in the guide hole 10 can be effectively prevented.
In some preferred embodiments of the present invention, the upper portion of the exhaust channel 3 is an inner concave surface 4, and the inner concave surface 4 is arc-shaped or cone-shaped, which is more beneficial to forming a sealing surface in cooperation with the first sphere 5, so as to further improve the sealing performance.
It is further preferred that the radial dimension of the concave surface 4 increases in order from bottom to top, which is more advantageous for the exertion of the self-leveling seal of the first sphere 5.
Further preferably, the shape of the concave surface 4 is the same as the outer contour of the partial sphere of the first sphere 5.
Further preferably, the lower portion of the exhaust passage 3 is cylindrical, and the radial dimension of the cylindrical portion is smaller than the radial dimension of the concave surface 4. Which is more advantageous for smoothly and rapidly exhausting the residual gas in the crucible.
In some preferred embodiments of the present invention, the upper portion of the lifting rod 8 continues to extend upwards along the first weight 9, and a plurality of second weights are continuously sleeved on the extending end, so that the gravity borne by the first ball 5 can be flexibly adjusted according to the working air pressures of the silicon carbide single crystals with different sizes, and stable and high-quality growth of the silicon carbide single crystals with different sizes can be realized.
The second weight may be the same or different in weight from the first weight. The weight of the first weight can be selected according to practical requirements to adapt to the growth of the silicon carbide single crystal with the required size specification.
In some preferred embodiments of the invention, the radial dimension of the guide hole 10 is smaller than the radial dimension of the exhaust channel 3, which further prevents the risk of dust entering the support 6 and adhering to the first sphere 5, resulting in poor tightness, while ensuring a rapid exhaust.
The mode of non-contact between the lower surface of the first weight 9 and the supporting frame 6 can be widely selected. In some embodiments of the invention, the first weight 9 is fixed on the lifting rod 8 to ensure that the first weight 9 does not contact the supporting frame 6 and to transfer the weight of the first weight 9 to the first ball 5.
In other embodiments of the present invention, the first weight 9 is movably sleeved on the lifting rod 8, and a baffle is fixed on the lifting rod 8, and the baffle is located between the first weight 9 and the supporting frame 6 and is not in contact with the supporting frame 6.
In some preferred embodiments of the present invention, the hood-shaped circumferential direction is provided with a vent hole 7, which is more advantageous for rapid and stable gas discharge.
Further, the number of the exhaust holes 7 may be several, and may be arranged at intervals along the circumferential direction of the cover shape. Or the exhaust holes 7 are stripe-shaped and extend in the circumferential direction.
The apparatus for growing a silicon carbide single crystal may further include other conventional components required for crystal growth. In some preferred embodiments of the present invention, the apparatus for growing a silicon carbide single crystal further comprises a single crystal growth furnace, a heater, the crucible being disposed within a working chamber of the single crystal growth furnace, the heater being located between the crucible and a furnace wall of the single crystal growth furnace.
In a second aspect, the present invention provides a method of growing a silicon carbide single crystal, which is carried out in the apparatus for growing a silicon carbide single crystal according to the first aspect, and which comprises the steps of:
The method comprises the steps of putting a raw material 12 into a crucible body 1 in advance, and installing an exhaust assembly on a crucible cover 2 so that a first sphere 5 abuts against an exhaust channel 3 of the crucible cover 2; then the crucible cover 2 and the crucible body 1 are connected together to form a crucible with a relatively closed space; placing the crucible in a working cavity of a single crystal growth furnace;
Then, the working cavity is vacuumized, the vacuumized suction force is larger than the integral gravity of the first sphere 5 and the lifting rod 8 and the first weight 9 connected with the first sphere, the first sphere 5 is sucked upwards, air in the crucible is discharged through the opened exhaust channel 3, when the target vacuum degree is pumped, the pressure in the crucible is equal to the pressure in the working cavity, and the first sphere 5 naturally falls into the upper part of the exhaust channel 3 under the action of the integral gravity of the first sphere 5 and the lifting rod 8 and the first weight 9 connected with the first sphere, so that the crucible is sealed, and the pumping and discharging of the air in the crucible are completed;
and then introducing process gas into the working cavity, starting heating, and performing crystal growth.
In some preferred embodiments of the present invention, the method of growing a silicon carbide single crystal further comprises: according to the air pressure generated by the silicon carbide monocrystal with the required size in the working cavity, a plurality of second weights with the required gravity are sleeved on the upper part of the lifting rod 8 of the exhaust assembly, are used for naturally falling down to seal the crucible, and can be sucked up during vacuumizing. According to the invention, the second weight is added to the first ball 5 to carry out proper weight balancing according to the growth environment of silicon carbide single crystals with different sizes, so that the tightness of the exhaust assembly is ensured and the exhaust is maximized.
It will be appreciated that the target vacuum may be selected by those skilled in the art as desired, as long as the pressure in the crucible is equal to the pressure in the working chamber.
The method for growing the silicon carbide single crystal can be suitable for growing the silicon carbide single crystals with different sizes and promote the high-quality stable growth of the silicon carbide single crystals.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (9)
1. The utility model provides a device for growing silicon carbide single crystal, includes crucible body and crucible cover, crucible cover lower surface middle part is used for installing the seed wafer, set up the exhaust passage that extends along vertical direction on the peripheral marginal zone in middle part of crucible cover, crucible body and crucible cover constitute the crucible, its characterized in that still includes the exhaust subassembly that sets up at the crucible cover surface, and the exhaust subassembly includes:
The support frame is arranged on the upper surface of the part of the crucible cover close to the exhaust channel, the middle part of the support frame is provided with a guide hole, and the guide hole and the central axis of the exhaust channel are positioned on the same vertical line; the support frame is in a cover shape and covers the periphery above the exhaust channel;
the lifting rod penetrates out of the support frame along the guide hole to extend upwards continuously, a first weight is sleeved at the extending end of the lifting rod, and the lower surface of the first weight is not contacted with the support frame;
The upper part of the first ball body is fixed at the bottom of the lifting rod, the lower part of the first ball body is propped against the upper part of the exhaust channel, the first ball body can automatically fall down to form a seal by gravity under the natural state without vacuumizing, and the first ball body can be sucked upwards when the crucible is vacuumized, and the air in the crucible is discharged outwards through the exhaust channel;
The upper part of the exhaust channel is an inner concave surface, and the shape of the inner concave surface is arc-shaped or conical;
the device can improve the vacuumizing effect, maximize and discharge residual gas in the crucible, and promote the sealing effect.
2. The apparatus for growing a silicon carbide single crystal according to claim 1, wherein the radial dimension of the concave inner surface increases in order from bottom to top.
3. The apparatus for growing a silicon carbide single crystal according to claim 1, wherein the shape of the concave inner surface is the same as the outer contour of a part of the spherical surface of the first sphere.
4. The apparatus for growing a silicon carbide single crystal according to claim 1, wherein the lower portion of the exhaust passage is cylindrical, and a radial dimension of the cylindrical portion is smaller than a radial dimension of the concave surface.
5. The apparatus for growing a silicon carbide single crystal according to claim 1, wherein the upper part of the lifting rod continues to extend upward along the first weight, and a plurality of second weights continue to be sleeved on the extending ends;
and/or the radial dimension of the guide hole is smaller than the radial dimension of the exhaust passage.
6. The apparatus for growing a silicon carbide single crystal according to claim 1, wherein the first weight is fixed to the lifting rod, or
The movable sleeve of the first weight is arranged on the lifting rod, the baffle is fixedly arranged on the lifting rod and is positioned between the first weight and the supporting frame, and the baffle is not contacted with the supporting frame.
7. The apparatus for growing a silicon carbide single crystal according to claim 1, wherein the hood-like circumferential direction is provided with vent holes;
And/or the device for growing the silicon carbide single crystal further comprises a single crystal growth furnace and a heater, wherein the crucible is arranged in a working cavity of the single crystal growth furnace, and the heater is arranged between the crucible and the furnace wall of the single crystal growth furnace.
8. A method of growing a silicon carbide single crystal, characterized in that it is carried out in an apparatus for growing a silicon carbide single crystal according to any one of claims 1 to 7, and that it comprises the steps of:
the method comprises the steps of putting raw materials into a crucible body in advance, and installing an exhaust assembly on a crucible cover so that a first sphere abuts against an exhaust channel of the crucible cover; then the crucible cover and the crucible body are connected together to form a crucible with a relatively closed space; placing the crucible in a working cavity of a single crystal growth furnace;
Then, the working cavity is vacuumized, the vacuumized suction force is larger than the integral gravity of the first sphere, the lifting rod connected with the first sphere and the first weight, the first sphere is sucked upwards, air in the crucible is discharged through the opened exhaust channel, when the target vacuum degree is pumped, the pressure in the crucible is equal to the pressure in the working cavity, and the first sphere naturally falls into the upper part of the exhaust channel under the action of the integral gravity of the first sphere, the lifting rod connected with the first weight, so that the crucible is sealed, and the air pumping and discharging work in the crucible is completed;
and then introducing process gas into the working cavity, starting heating, and performing crystal growth.
9. The method for growing a silicon carbide single crystal according to claim 8, wherein the method for growing a silicon carbide single crystal further comprises: according to the air pressure generated by the silicon carbide monocrystal with the required size in the working cavity, a plurality of second weights with the required gravity are sleeved on the upper part of the lifting rod of the exhaust assembly, are used for naturally falling down to seal the crucible, and can be sucked up during vacuumizing.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113026106A (en) * | 2021-05-19 | 2021-06-25 | 浙江大学杭州国际科创中心 | Growth process of silicon carbide crystal |
| CN113249784A (en) * | 2021-05-12 | 2021-08-13 | 中科汇通(内蒙古)投资控股有限公司 | Silicon carbide single crystal growth device capable of balancing growth system atmosphere |
| CN218863356U (en) * | 2021-11-26 | 2023-04-14 | 艾华(无锡)半导体科技有限公司 | Balance valve device for adjusting internal pressure and external pressure of semiconductor coating equipment |
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| JP3623405B2 (en) * | 1999-08-30 | 2005-02-23 | Ｎｅｃマシナリー株式会社 | Single crystal growth equipment |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113249784A (en) * | 2021-05-12 | 2021-08-13 | 中科汇通(内蒙古)投资控股有限公司 | Silicon carbide single crystal growth device capable of balancing growth system atmosphere |
| CN113026106A (en) * | 2021-05-19 | 2021-06-25 | 浙江大学杭州国际科创中心 | Growth process of silicon carbide crystal |
| CN218863356U (en) * | 2021-11-26 | 2023-04-14 | 艾华(无锡)半导体科技有限公司 | Balance valve device for adjusting internal pressure and external pressure of semiconductor coating equipment |
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