CN115838963B - Crucible device applied to growth of silicon carbide single crystal by sublimation method - Google Patents
Crucible device applied to growth of silicon carbide single crystal by sublimation method Download PDFInfo
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Abstract
The invention relates to the technical field of single crystal preparation, and particularly discloses a crucible device for growing silicon carbide single crystals by a sublimation method. The crucible component comprises a crucible top wall, a crucible side wall, a crucible bottom wall and a crucible inner wall. The space between the inner wall of the crucible and the side wall of the crucible is a first accommodating space, and the silicon carbide raw material powder source is accommodated in the first accommodating space; a second diversion component is arranged below the inner wall of the crucible, and a flaring space is formed between the outer walls of the second diversion component and the crucible; a third diversion component is arranged below the second diversion component, a diversion space is formed between the outer walls of the third diversion component, a porous graphite component is arranged at the top of the diversion space, and seed crystals are arranged at the bottom of the diversion space. The crucible device can reduce the influence of factors such as gravity on the growth of single crystals, can reduce carbon wrapping materials in the crystal growth process, and is beneficial to improving the crystal quality.
Description
Technical Field
The invention relates to the technical field of single crystal preparation, in particular to a crucible device for growing silicon carbide single crystals by a sublimation method.
Background
Silicon carbide (SiC) is attracting attention as an environmentally-resistant semiconductor material because of its excellent heat resistance and mechanical strength and its physical and chemical properties such as high resistance to radiation.
Silicon carbide single crystal growth currently uses physical vapor deposition (PVT) as the primary growth method, and has proven to be the most mature method for growing SiC crystals. The sublimation method for preparing the silicon carbide crystal comprises the following steps: and (3) placing the silicon carbide solid raw material into a crucible body, sublimating the silicon carbide solid raw material in an endophytic heat environment of a growth furnace, and crystallizing on seed crystals adhered to the bottom of a top cover of the crucible to complete the growth of crystals.
In the long term, sublimation-based silicon carbide crystal growth will dominate the future of large-size high-quality silicon carbide crystal growth. With the development of the semiconductor industry, the requirements on the quality of silicon carbide crystals are also increasing. Optimizing the crystal growth thermal environment is important to improve the crystal quality.
In the process of preparing silicon carbide single crystal by the conventional PVT method, a silicon carbide raw material powder source is contained at the bottom of a crucible, a seed crystal is arranged at the bottom of a top cover of the crucible, so that the growth process of the crystal is greatly influenced by factors such as gravity, the growth size and the growth quality of the crystal are limited to a certain extent, and carbon particles are easily mixed in a gas phase tissue in the sublimation process of the silicon carbide raw material powder source, so that carbon wrappage remains in the grown crystal, and the growth quality of the crystal is seriously influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a crucible device applied to the growth of silicon carbide single crystals by a sublimation method, so that the silicon carbide single crystals start to grow from the bottom of the crucible, the generation of thermal stress in the crystal growth process is reduced, the generation probability of carbon wrappage in the crystal growth process is reduced, and the crystal growth quality is improved.
In order to achieve the purpose, the invention adopts the following technical scheme based on the improved design of the crucible structure and combined with the growth environment of silicon carbide:
the invention provides a crucible device for growing silicon carbide single crystals by a sublimation method, which comprises: the crucible component, the rotating component, the flow guiding component and the porous graphite component;
the crucible component comprises a crucible outer wall and a crucible inner wall, wherein the crucible outer wall comprises a crucible top wall, a crucible side wall and a crucible bottom wall, and the crucible outer wall encloses a crucible inner cavity; a first accommodating space is formed between the side wall of the crucible and the inner wall of the crucible and is used for accommodating a silicon carbide raw material powder source;
the flow guiding component comprises a first flow guiding component, a second flow guiding component and a third flow guiding component, which are all arranged close to the inner side of the side wall of the crucible;
the first flow guiding component is arranged above a first storage space outlet formed on the inner wall of the crucible, the second flow guiding component is arranged below the inner wall of the crucible, and the third flow guiding component is arranged below the second flow guiding component;
the space between the first flow guiding component and the upper surface of the inner wall of the crucible is a first flow guiding space, a second flow guiding space is formed between the outer side walls of the inner wall of the crucible, a flaring space is formed between the outer side walls of the second flow guiding component, the inner diameter of the flaring space gradually increases from top to bottom, and a third flow guiding space is formed between the outer side walls of the third flow guiding component;
the first storage space is communicated with the first diversion space, and the first diversion space, the second diversion space, the flaring space and the third diversion space are communicated in sequence;
the bottom of the third diversion space comprises a seed crystal placing space for placing silicon carbide seed crystals, the top of the third diversion space comprises a porous graphite component placing space for placing a porous graphite component, and the space between the porous graphite component and the seed crystals is used for gas phase substance transmission and accommodating grown single crystals;
the rotating component is arranged on the top wall of the crucible.
In the process of silicon carbide single crystal growth, the space above the flaring space in the crucible device is a high-temperature space, the high-temperature space provides heat to promote sublimation and transmission of silicon carbide raw material powder sources, the flaring space and the space below the flaring space are heat-preserving spaces, the temperature of the heat-preserving spaces is lower than that of the high-temperature space, and a temperature environment for promoting condensation and crystal growth of gas-phase substances in the crucible on the surface of a seed crystal can be provided.
The mode of the heat source in the high-temperature space is not particularly limited, for example, the heat source can be a resistance heater at the periphery of the crucible, or the heat source can be heat generated by the action of an induction magnetic field on the crucible, or the heat source generated by other modes.
In the process of silicon carbide single crystal growth, the silicon carbide raw material powder source is heated and decomposed in the first storage space to sublimate, sublimated gas phase substances are transferred to the first diversion space, meanwhile, the rotation of the rotating part enables the gas phase substances in the first diversion space to be fully mixed and then directionally transferred to the second diversion space, so that the gas phase substances enter the flaring space and the third diversion space, the radial distribution range of the gas phase substances is enlarged by the flaring space, and the gas phase substances are driven to be conveyed towards the third diversion space. The top of the third diversion space is provided with a porous graphite component, and the porous graphite material can absorb carbon wrappage mixed in the gas phase substance, so that the generation of the carbon wrappage in the crystal growth process can be reduced.
Preferably, the second guide member includes a second accommodation space, and the third guide member includes a third accommodation space. The second accommodating space is internally provided with a first heat source, and the third accommodating space is internally provided with a second heat source. Due to the existence of the second flow guiding component and the third flow guiding component, the temperature distribution uniformity in the radial direction of the inner cavity of the crucible, especially the lower part of the inner cavity of the crucible, is poor, the endogenous thermal stress in the crystal growth process is increased, the gas phase components near the long crystal boundary surface are unevenly distributed, defects and dislocation are increased, and the preparation of high-quality silicon carbide crystals is not facilitated. In this preferred embodiment, the heat source is provided in the second accommodation space and the third accommodation space, so that the problem of uneven temperature distribution in the crystal growth space can be effectively improved.
The second accommodation space and the third accommodation space may be communicated, and may be spaced apart from each other so as not to be communicated.
Preferably, the power of the second heat source is greater than the power of the third heat source. In the axial direction, the temperature difference is properly increased, so that the temperature near the seed crystal region is lower, and the gas phase substance is beneficial to flow towards the seed crystal region.
Optionally, the first accommodating space may be a plurality of the first accommodating spaces distributed along the inner side of the crucible sidewall, or may be a round of the inner side of the crucible sidewall, and more preferably is a round of structure, so that the generation of the gas phase is more uniform, and the temperature distribution in the first accommodating space and the second guiding space after being heated is more uniform.
Preferably, the outer wall of the first diversion component is obliquely arranged, and an included angle between the outer wall and a plane where the top of the inner wall of the crucible is positioned is 30-60 degrees. The first flow guiding component is used for guiding the silicon carbide raw material powder for the first time after sublimation, the flow guiding effect is important, and in the angle range, the gas phase substances can be better guided to be conveyed to the subsequent flow guiding space.
Preferably, the rotating member is located directly above the second diversion space.
Alternatively, the connections between the first, second and third flow directing members and the crucible member may be detachable connections or non-detachable connections.
Alternatively, the connection between the porous graphite member and the third flow directing member may be a detachable connection or a non-detachable connection.
Preferably, the outer surface of the porous graphite member is provided with a high temperature resistant coating.
Preferably, the porous graphite member has an application range of 10% -90% of porosity.
Preferably, the porous graphite member has a pore diameter in the range of 2 to 10 μm.
Compared with the prior art, the invention has obvious beneficial effects as follows:
the seed crystal is arranged at the bottom of the crucible, so that the restriction of the action of gravity and the like on the crystal size can be effectively reduced, meanwhile, the internal thermal stress in the crystal can be effectively reduced, and the crystal growth quality is improved.
The rotating part is arranged to uniformly mix the gas phase to a certain extent, thereby being beneficial to increasing the uniformity of gas phase substances and improving the crystal growth quality.
The porous graphite component is arranged above the seed crystal, so that the generation of carbon wrappage in the crystal can be effectively reduced, and the growth quality of the crystal can be improved.
The heat sources are arranged in the second accommodating space and the third accommodating space, so that the problem of uneven radial temperature distribution in the crystal growth space can be effectively solved, and the growth quality of crystals can be improved.
In the axial direction, the temperature difference is properly increased, so that the temperature close to the seed crystal region is lower, the gas phase substance can flow towards the direction of the seed crystal region, and the growth efficiency of the crystal is improved.
In general, the crucible device provided by the invention reduces the generation of thermal stress in the crystal growth process, reduces the generation probability of carbon wrappage in the crystal growth process, can maintain the uniformity of radial temperature distribution in the inner cavity of the crucible, and can effectively reduce the internal thermal stress of the grown crystal, thereby reducing the dislocation density in the crystal and being beneficial to improving the crystal quality. In particular, the crucible apparatus of the present invention can be used for other crystalline materials grown using physical vapor transport.
Drawings
Fig. 1 is a schematic structural view of a crucible device according to an embodiment of the present invention.
Fig. 2 is a schematic structural view of a crucible device according to another embodiment of the present invention.
Fig. 3 is a schematic structural view of a crucible device according to another embodiment of the present invention.
Fig. 4 is a thermal stress diagram of crucible apparatus according to the present invention and comparative example, wherein a corresponds to example 1, b corresponds to example 2, c corresponds to example 3, d corresponds to example 4, and e corresponds to comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in connection with examples of the present invention. It is expressly intended that the described embodiments be some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The invention will be further illustrated, but is not limited, by the following examples.
Example 1
As shown in fig. 1, a crucible apparatus for growing a silicon carbide single crystal by a sublimation method is provided in an embodiment of the present invention, which is applied to the growth of a silicon carbide single crystal. The device comprises a crucible component, a rotating component, a diversion component and a porous graphite component.
The crucible component is made of materials and has an external structure consistent with that of the existing crucible, and comprises a crucible side wall 102 and a crucible bottom wall 103, a crucible inner cavity is formed by surrounding, and a crucible top wall 101 is arranged at the top.
The embodiment is further provided with a crucible inner wall 104 in the inner cavity of the crucible, the crucible inner wall 104 and the crucible side wall 102 are of an integrated structure, the crucible inner wall 104 also comprises a bottom and a side, a first containing space 401 is formed between the bottom and the side and the crucible side wall 102 in a surrounding mode, the first containing space 401 is used for containing the silicon carbide raw material powder source 100, the first containing space 401 is located in a high temperature area in the crucible device, and sublimation of the silicon carbide raw material powder source 100 is guaranteed. The temperature of the high temperature region is controlled by the heat source, and the type of the heat source is not limited in the present invention, and the heating is performed by adopting a mode of heating by an induction magnetic field in the present embodiment.
In the inner cavity of the crucible, besides the inner wall 104 of the crucible, a first diversion component 201, a second diversion component 202 and a third diversion component 203 are additionally arranged, and a gas phase substance conveying diversion conveying channel is formed by matching with the first storage space 401.
The first diversion component 201 is located on the upper portion of the inner cavity of the crucible and the first storage space 401, the first diversion component 201 and the side wall 102 of the crucible are also of an integrated structure, the whole first diversion component 201 is in a ring shape with a narrow upper part and a wide lower part, the first diversion component 201 is blocked above the outlet of the first storage space 401, a space between the first diversion component 201 and the inner wall 104 of the crucible is a first diversion space 301, and the first diversion space 301 is communicated with the first storage space 401.
A second diversion space 302 is arranged between the outer side walls of the inner crucible wall 104 in the crucible device, and the second diversion space 302 is communicated with the first diversion space 301.
The middle part of the top wall 101 of the crucible in the crucible device is provided with a rotating part 105, and the rotating part 105 is driven by a motor outside the crucible device to rotate and is positioned right above the inlet of the second diversion space 302. The rotation member 105 is rotated such that the gas phase substances in the first diversion space 301 are sufficiently mixed and directionally transferred to the second diversion space 302. The head structure of the rotating member 105 inside the inner cavity of the crucible is not suitable for being too large and too long, preferably in the shape of a short piece or a sphere, and the rotating speed is not suitable for being too fast and slowly rotated, so that the uniformity of the gas phase material is facilitated, and the rotating speed is usually 0.1-10 rpm.
The second flow guiding component 202 of the crucible device is positioned below the inner wall 104 of the crucible, the top of the second flow guiding component is tightly attached to the inner wall 104 of the crucible, and the side of the second flow guiding component is tightly attached to the side wall of the crucible, or the second flow guiding component and the side wall of the crucible device can be integrally designed. The second flow guiding component 202 is of a solid structure, a flaring space 303 is formed between the outer side walls of the second flow guiding component 202, the flaring space 303 is communicated with the second flow guiding space 302, and the inner diameter of the flaring space 303 gradually increases from top to bottom.
The third diversion component 203 of the crucible device is arranged below the second diversion component 202, the top of the third diversion component 203 is tightly attached to the bottom of the second diversion component 202, a third diversion space 304 is formed between the outer side walls of the third storage component 203, the third diversion space 304 comprises a placement space of the seed crystal 205, a placement space of the porous graphite component 204 and a space for gas phase substance transmission and crystal growth, the third diversion space 304 is communicated with the flaring space 303 through a gas phase substance transmission channel in the porous graphite component 204, and a high-temperature resistant coating is arranged on the outer surface of the third diversion space 304; the application range of the porosity of the porous graphite component is 10% -90%, and the pore diameter range is 2-10 mu m. The porous graphite part 204 in the crucible device is arranged at the top space of the third diversion space 304, the porous graphite part 204 contains channels for transporting gas phase substances, and the porous graphite part 204 has the main function of filtering carbon particle substances mixed in the gas phase substances, thereby reducing the formation of carbon wrappers in the process of growing silicon carbide single crystals and improving the crystal quality; seed crystal 205 is arranged on the upper surface of crucible bottom wall 103 in the crucible device, which can effectively reduce the generation of internal stress in the crystal, and is beneficial to increasing the growth size of the crystal and improving the quality of the crystal.
Example 2
Unlike embodiment 1, as shown in fig. 2, the second diversion member 202 includes a second accommodation space 402, the third diversion member 203 includes a third accommodation space 403, and the second accommodation space 402 and the third accommodation space 403 are filled with the heat insulating material 200.
Example 3
Unlike the embodiment 1, as shown in fig. 3, the second diversion member 202 includes a second accommodating space 402, the third diversion member 203 includes a third accommodating space 403, and the heat sources 300 are disposed in the second accommodating space 402 and the third accommodating space 403, and the power is the same.
Example 4
Unlike embodiment 1, the second diversion member 202 includes a second accommodation space 402, the third diversion member 203 includes a third accommodation space 403, the first heat source is disposed in the second accommodation space 402, and the second heat source is disposed in the third accommodation space 403. The first heat source power is greater than the second heat source power. The first heat source temperature is 2390K and the second heat source temperature is 2350K.
Comparative example 1
A crucible apparatus for growing crystals by sublimation is different from embodiment 1 in that the second flow guide member and the third flow guide member are not provided.
The results of the test statistics of thermal stress on the crystal surface at the start of crystallization when silicon carbide crystal growth was performed using the crucible apparatuses of the respective examples and comparative examples are shown in fig. 4. As can be seen from fig. 4, in comparative example 1, in which the second flow guide member and the third flow guide member are not provided, the thermal stress of the crystal surface is maximum, which is most disadvantageous for the formation of high quality crystals. Next is example 1. In embodiment 2, the heat insulating material is disposed in the receiving spaces of the second flow guiding member and the third flow guiding member, which is advantageous in reducing the generation of thermal stress on the crystal surface. In the embodiment 3 and the embodiment 4, the heat source is arranged in the accommodating space of the second diversion component and the third diversion component, which is more favorable for maintaining low thermal stress than the heat insulation material, and the temperature near the seed crystal is slightly lower, so that the effect is better.
It should be noted that the above embodiment is only one of the examples provided for reference of the present invention, and is not intended to limit the embodiments and the protection scope of the present invention, and those skilled in the art should appreciate that all equivalent substitutions and obvious modifications made by applying the content of the present invention are included in the protection scope of the present invention.
Claims (7)
1. A crucible apparatus for growing a silicon carbide single crystal by sublimation, comprising: crucible component, diversion component and porous graphite component and rotating component;
the crucible component comprises a crucible outer wall and a crucible inner wall, wherein the crucible outer wall comprises a crucible top wall, a crucible side wall and a crucible bottom wall, and the crucible outer wall encloses a crucible inner cavity; a first accommodating space is formed between the side wall of the crucible and the inner wall of the crucible and is used for accommodating a silicon carbide raw material powder source;
the flow guiding component comprises a first flow guiding component, a second flow guiding component and a third flow guiding component, which are all arranged close to the inner side of the side wall of the crucible;
the first flow guiding component is arranged above a first storage space outlet formed on the inner wall of the crucible, the second flow guiding component is arranged below the inner wall of the crucible, and the third flow guiding component is arranged below the second flow guiding component;
the space between the first flow guiding component and the upper surface of the inner wall of the crucible is a first flow guiding space, a second flow guiding space is formed between the outer side walls of the inner wall of the crucible, a flaring space is formed between the outer side walls of the second flow guiding component, the inner diameter of the flaring space gradually increases from top to bottom, and a third flow guiding space is formed between the outer side walls of the third flow guiding component;
the first storage space is communicated with the first diversion space, and the first diversion space, the second diversion space, the flaring space and the third diversion space are communicated in sequence;
the silicon carbide seed crystal is arranged at the bottom of the third diversion space, the porous graphite component is arranged at the top of the third diversion space, and the space between the porous graphite component and the seed crystal is used for gas phase substance transmission and accommodating grown single crystals;
the rotating component is arranged on the top wall of the crucible and is positioned right above the inlet of the second diversion space;
the outer wall of the first flow guiding component is obliquely arranged, and an included angle between the outer wall and a plane where the top of the inner wall of the crucible is located is 30-60 degrees.
2. A crucible apparatus for growing a silicon carbide single crystal by sublimation according to claim 1, wherein: the second flow guide part comprises a second storage space, the third flow guide part comprises a third storage space, a first heat source is arranged in the second storage space, and a second heat source is arranged in the third storage space.
3. A crucible apparatus for growing a silicon carbide single crystal by sublimation according to claim 2, wherein: the power of the second heat source is greater than the power of the third heat source.
4. A crucible apparatus for growing a silicon carbide single crystal by sublimation according to claim 1, wherein: the first receiving space is a circle around the inner side of the side wall of the crucible.
5. A crucible apparatus for growing a silicon carbide single crystal by sublimation according to claim 1, wherein: the outer surface of the porous graphite component is provided with a high-temperature resistant coating.
6. A crucible apparatus for growing a silicon carbide single crystal by a sublimation method according to claim 5, wherein: the porosity of the porous graphite component is 10% -90%.
7. A crucible apparatus for growing a silicon carbide single crystal by a sublimation method according to claim 5, wherein: the pore diameter range of the porous graphite component is 2-10 mu m.
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| JP2010100447A (en) * | 2008-10-21 | 2010-05-06 | Bridgestone Corp | Apparatus and method for producing silicon carbide single crystal |
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| CN105442037A (en) * | 2015-12-08 | 2016-03-30 | 西安交通大学 | High-speed single crystal growth device |
| CN113106546B (en) * | 2021-03-25 | 2022-05-17 | 徐州鑫晶半导体科技有限公司 | Guide cylinder for single crystal furnace, single crystal furnace and machining method of guide cylinder |
| CN113151897B (en) * | 2021-04-26 | 2022-08-26 | 福建北电新材料科技有限公司 | Crucible structure |
| CN114059154A (en) * | 2021-11-17 | 2022-02-18 | 宁波合盛新材料有限公司 | Silicon carbide single crystal growth device and method |
| CN115216842A (en) * | 2022-06-24 | 2022-10-21 | 厦门大学 | Crucible structure for growing high-quality silicon carbide single crystal and growing method |
| CN114990690B (en) * | 2022-06-30 | 2024-02-27 | 武汉大学 | Crucible device for preparing silicon carbide monocrystal by gas phase sublimation method |
| CN115491759A (en) * | 2022-11-16 | 2022-12-20 | 浙江晶越半导体有限公司 | Additional powder source container and crucible device for preparing silicon carbide single crystal |
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