CN115838963A - Be applied to crucible device of sublimation method growth carborundum single crystal - Google Patents
Be applied to crucible device of sublimation method growth carborundum single crystal Download PDFInfo
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- CN115838963A CN115838963A CN202211716479.XA CN202211716479A CN115838963A CN 115838963 A CN115838963 A CN 115838963A CN 202211716479 A CN202211716479 A CN 202211716479A CN 115838963 A CN115838963 A CN 115838963A
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- 239000013078 crystal Substances 0.000 title claims abstract description 97
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 46
- 238000005092 sublimation method Methods 0.000 title claims abstract description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
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- 239000010439 graphite Substances 0.000 claims description 13
- 238000000859 sublimation Methods 0.000 claims description 13
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- 238000009826 distribution Methods 0.000 description 6
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Abstract
The invention relates to the technical field of single crystal preparation, and particularly discloses a crucible device applied to growing silicon carbide single crystals by a sublimation method. The crucible part comprises a crucible top wall, a crucible side wall, a crucible bottom wall and a crucible inner wall. A space between the inner wall of the crucible and the side wall of the crucible is a first accommodating space, and a silicon carbide raw material powder source is accommodated in the first accommodating space; a second flow guide part is arranged below the inner wall of the crucible, and a flaring space is formed between the outer walls of the second flow guide part; a third flow guide part is arranged below the second flow guide part, a flow guide space is formed between the outer walls of the third flow guide part, a porous graphite part is arranged at the top of the flow guide space, and seed crystals are arranged at the bottom of the flow guide space. The crucible device can reduce the influence of factors such as gravity on the growth of the single crystal, reduce carbon inclusions in the growth process of the crystal and is beneficial to improving the quality of the crystal.
Description
Technical Field
The invention relates to the technical field of single crystal preparation, in particular to a crucible device applied to growing silicon carbide single crystals by a sublimation method.
Background
Silicon carbide (SiC) has attracted attention as an environment-resistant semiconductor material because of its physical and chemical properties such as excellent heat resistance and mechanical strength and high resistance to radiation.
The growth of silicon carbide single crystal, which uses physical vapor deposition (PVT) as the main growth mode, has been proven to be the most mature method for growing SiC crystal. The method for preparing the silicon carbide crystal by the sublimation method comprises the following steps: and (3) putting the silicon carbide solid raw material into the crucible body, subliming the silicon carbide solid raw material in an internal heating environment of the growth furnace, and crystallizing the silicon carbide solid raw material on seed crystals adhered to the bottom of a top cover of the crucible to finish the growth of the crystals.
In the long run, the growth of silicon carbide crystals based on sublimation will dominate the future growth of large size, high quality silicon carbide crystals. With the development of the semiconductor industry, the requirements on the quality of silicon carbide crystals are higher and higher. Optimizing the crystal growth thermal environment is important for improving the crystal quality.
In-process that traditional PVT method was prepared carborundum single crystal, carborundum raw materials powder source is accomodate in the crucible bottom, the seed crystal is installed in crucible top cap bottom, the in-process that leads to crystal growth receives factors such as gravity to influence great, all have certain restriction to crystal growth size and growth quality, in addition, carbon particles are mingled with easily in the gaseous phase structure of carborundum raw materials powder source sublimed in-process for reserve carbon inclusion in the crystal of growth, seriously influence crystal growth quality.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the crucible device applied to the sublimation method for growing the silicon carbide single crystal, so that the silicon carbide single crystal starts 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 inclusions 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 applied to the growth of silicon carbide single crystal by a sublimation method, which comprises: a crucible member, a rotating member, a guide member and a porous graphite member;
the crucible component comprises a crucible outer wall and a crucible inner wall, 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 containing space is formed between the side wall of the crucible and the inner wall of the crucible and is used for containing a silicon carbide raw material powder source;
the flow guide parts comprise a first flow guide part, a second flow guide part and a third flow guide part which are arranged close to the inner side of the side wall of the crucible;
the first flow guide component is arranged above an outlet of a first containing space formed by the inner wall of the crucible, the second flow guide component is arranged below the inner wall of the crucible, and the third flow guide component is arranged below the second flow guide component;
the space between the first flow guide part and the upper surface of the inner wall of the crucible is a first flow guide space, a second flow guide 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 guide part, the inner diameter of the flaring space is gradually increased from top to bottom, and a third flow guide space is formed between the outer side walls of the third flow guide part;
the first accommodating space is communicated with the first flow guide space, and the first flow guide space, the second flow guide space, the flaring space and the third flow guide space are sequentially communicated;
the bottom of the third flow guide space comprises a seed crystal accommodating space for accommodating a silicon carbide seed crystal, the top of the third flow guide space comprises a porous graphite part accommodating space for accommodating a porous graphite part, and the space between the porous graphite part and the seed crystal is used for conveying gas-phase substances and accommodating a growing single crystal;
the rotating component is arranged on the top wall of the crucible.
In the process of growing the silicon carbide single crystal, the space above the flaring space in the crucible device is a high-temperature space, the high-temperature space provides heat to promote the silicon carbide raw material powder source to sublimate and transmit, 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 spaces, and a temperature environment for promoting the gas phase substances in the crucible to condense and grow crystals on the surface of the seed crystals can be provided.
The invention is not limited in particular to the way of acting the heat source in the high-temperature space, for example, the heat source can be from a resistance heater at the periphery of the crucible, or the heat source can be from heat generated by the action of the induction magnetic field on the crucible, or the heat source generated by other ways.
In the in-process of carborundum single crystal growth, the carbofrax raw materials powder source is heated to decompose and sublimate in first storage space, and gaseous phase substance after the sublimation transmits to first water conservancy diversion space, and rotary part's rotation makes the gaseous phase substance intensive mixing in the first water conservancy diversion space later directional transmission to second water conservancy diversion space simultaneously to get into flaring space and third water conservancy diversion space, the radial distribution scope of gaseous phase substance has been increased in the flaring space, be favorable to ordering about gaseous phase substance and carry towards third water conservancy diversion space. The top device of the third diversion space is provided with a porous graphite part, and the porous graphite material can absorb carbon inclusions in gas-phase substances, so that the generation of the carbon inclusions in the crystal growth process can be reduced.
Preferably, the second air guide member includes a second housing space therein, and the third air guide member includes a third housing space therein. A first heat source is arranged in the second containing space, and a second heat source is arranged in the third containing space. Due to the existence of the second flow guide part and the third flow guide part, the radial temperature distribution uniformity of the inner cavity of the crucible, particularly the lower part of the inner cavity of the crucible, is poor, so that the endogenous thermal stress in the crystal growth process is increased, and the gas phase components near the long crystal boundary surface are not uniformly distributed, so that the defects and the dislocation are increased, and the preparation of the high-quality silicon carbide crystal is not facilitated. In this preferred embodiment, the heat sources are provided in the second storage space and the third storage space, so that the problem of uneven temperature distribution in the crystal growth space can be effectively solved.
The second receiving space and the third receiving space may be in communication with each other, and may be separated from each other and not in communication with each other.
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 of the area close to the seed crystal is lower, and the gas phase substance flows towards the direction of the seed crystal area.
Optionally, the first receiving space may be a plurality of first receiving spaces distributed along the inner side of the crucible side wall, or may be a circle around the inner side of the crucible side wall, and more preferably, the first receiving space is of a circle structure, so that the generation of the gas phase is more uniform, and the temperature distribution in the first receiving space and the second guiding space after being heated is more uniform.
Preferably, the outer wall of the first flow guide part is obliquely arranged, and the included angle between the outer wall of the first flow guide part and the plane where the top of the inner wall of the crucible is located is 30-60 degrees. The first diversion component is the first diversion encountered after the silicon carbide raw material powder source sublimes, the diversion effect is of great importance, and the gas phase substances can be better guided to be conveyed to the subsequent diversion space within the angle range.
Preferably, the rotating member is located directly above the second guide space.
Alternatively, the connections between the first, second and third flow guide 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 guide 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 porosity of the porous graphite component is applied within a range of 10% to 90%.
Preferably, the pore diameter of the porous graphite member is 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 limitation of the action of gravity and the like on the size of the crystal can be effectively reduced, the endogenous thermal stress in the crystal can be effectively reduced, and the growth quality of the crystal is improved.
Set up rotary part, carry out certain degree homogeneous mixing to the gaseous phase, be favorable to increasing gaseous phase material's homogeneity, improve crystal growth quality.
The porous graphite component is arranged above the seed crystal, so that the generation of carbon inclusions in the crystal can be effectively reduced, and the growth quality of the crystal is improved.
The heat sources are arranged in the second containing space and the third containing 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 is improved.
In the axial direction, the temperature difference is properly increased, so that the temperature of the area close to the seed crystal is lower, the gas-phase substance can flow towards the direction of the seed crystal area, and the growth efficiency of the crystal is improved.
Generally, the crucible device provided by the invention reduces the generation of thermal stress in the crystal growth process, reduces the generation probability of carbon inclusions 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 crystal materials grown by physical vapor transport.
Drawings
Fig. 1 is a schematic structural diagram of a crucible apparatus according to an embodiment of the present invention.
Fig. 2 is a schematic structural view of a crucible apparatus according to another embodiment of the present invention.
FIG. 3 is a schematic view of a crucible apparatus according to another embodiment of the present invention.
FIG. 4 is a graph showing thermal stress in the crucible apparatus according to the examples and comparative examples of the present invention, wherein a corresponds to example 1,b to example 2,c to example 3,d to example 4,e to comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the examples of the present invention. It is specifically intended that the embodiments described are a subset of the embodiments of the invention and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Example 1
As shown in fig. 1, the embodiment of the present invention provides a crucible apparatus for growing a silicon carbide single crystal by sublimation, which is applied to the growth of a silicon carbide single crystal. The apparatus includes a crucible member, a rotating member, a flow guide member, and a porous graphite member.
The crucible component is made of the same material and has the same external structure as that of the existing crucible, and comprises a crucible side wall 102 and a crucible bottom wall 103 which enclose a crucible inner cavity, and a crucible top wall 101 is arranged at the top.
In the embodiment, a crucible inner wall 104 is additionally arranged in the crucible inner cavity, the crucible inner wall 104 and the crucible side wall 102 are of an integral structure, the crucible inner wall 104 also comprises a bottom part and a side part, a first accommodating space 401 is defined between the bottom part and the side part and the crucible side wall 102, the first accommodating space 401 is used for accommodating the silicon carbide raw material powder source 100, and the first accommodating space 401 is located in a high-temperature area of the crucible device, so that sublimation of the silicon carbide raw material powder source 100 is ensured. The temperature of the high temperature region is controlled by a heat source, the type of the heat source is not limited in the present invention, and the heating is performed by an induction magnetic field heating method in this embodiment.
In addition to the crucible inner wall 104, a first diversion member 201, a second diversion member 202 and a third diversion member 203 are additionally arranged in the crucible inner cavity, and a conveying diversion conveying channel for gas phase substances is formed by matching with the first receiving space 401.
The first flow guide component 201 is located on the upper portion of the inner cavity of the crucible and the first containing space 401, the first flow guide component 201 and the crucible side wall 102 are of an integral structure, the first flow guide component 201 is integrally in a ring shape with a narrow top and a wide bottom, the first flow guide component 201 is blocked above an outlet of the first containing space 401, a space between the first flow guide component 201 and the inner wall 104 of the crucible is a first flow guide space 301, and the first flow guide space 301 is communicated with the first containing space 401.
A second diversion space 302 is arranged between the outer side walls of the crucible inner walls 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 rotating member 105 is rotated to make the gas phase substance in the first guiding space 301 fully mixed and directionally transferred to the second guiding space 302. The head structure of the rotating part 105 positioned in the crucible cavity is not suitable for being too large and too long, preferably in a short sheet shape or a spherical shape, and the rotating speed is not too fast and is slow to rotate, so that the uniformity of gas phase substances is facilitated, and the head structure is usually rotated at the speed of 0.1 to 10 rpm.
The second flow guiding component 202 of the crucible device is located below the crucible inner wall 104, the top of the second flow guiding component is tightly attached to the crucible inner wall 104, the side of the second flow guiding component is tightly attached to the crucible side wall, and the second flow guiding component and the crucible side wall can also be designed into an integral structure. The second flow guide part 202 is a solid structure, a flaring space 303 is formed between the outer side walls of the second flow guide part 202, the flaring space 303 is communicated with the second flow guide space 302, and the inner diameter of the flaring space 303 is gradually increased from top to bottom.
The third flow guide part 203 of the crucible device is arranged below the second flow guide part 202, the top of the third flow guide part 203 is tightly attached to the bottom of the second flow guide part 202, a third flow guide space 304 is formed between the outer side walls of the third accommodating part 203, the third flow guide space 304 comprises a seed crystal 205 accommodating space, a porous graphite part 204 accommodating space and a gas phase substance transmission and crystal growth space, the third flow guide space 304 is communicated with a flaring space 303 through a gas phase substance transmission channel contained in the porous graphite part 204, and the outer surface of the third flow guide space is provided with a high temperature resistant coating; the application range of the porosity of the porous graphite component is 10% -90%, and the pore diameter range of the pores is 2-10 mu m. The porous graphite component 204 in the crucible device is arranged in the top space of the third diversion space 304, the porous graphite component 204 contains channels for conveying gas phase substances, and the main function of the porous graphite component 204 is to filter carbon particulate substances included in the gas phase substances, thereby reducing the formation of carbon inclusions in the crystal growth process of the silicon carbide single crystal and improving the crystal quality; in the crucible device, the seed crystal 205 is arranged on the upper surface of the bottom wall 103 of the crucible, so that the generation of internal stress in the crystal can be effectively reduced, the growth size of the crystal can be increased, and the quality of the crystal can be improved.
Example 2
The difference from embodiment 1 is that, as shown in fig. 2, the second air guide member 202 includes a second housing space 402, the third air guide member 203 includes a third housing space 403, and the heat insulating material 200 is filled in both the second housing space 402 and the third housing space 403.
Example 3
The difference from embodiment 1 is that, as shown in fig. 3, the second air guide member 202 includes a second housing space 402, the third air guide member 203 includes a third housing space 403, and the heat sources 300 are provided in both the second housing space 402 and the third housing space 403, and the power is the same.
Example 4
The difference from embodiment 1 is that the second guide member 202 includes a second housing space 402, the third guide member 203 includes a third housing space 403, a first heat source is provided in the second housing space 402, and a second heat source is provided in the third housing 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 a crystal by sublimation is different from embodiment 1 in that a second flow guide member and a third flow guide member are not provided.
The results of the measurement statistics of the thermal stress on the crystal surface at the start of crystallization when a silicon carbide crystal was grown using the crucible devices of each of the 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 were not provided, the thermal stress of the crystal surface was the largest, most disadvantageous to the formation of high quality crystals. Next is example 1. In embodiment 2, the heat insulating material is provided in the storage spaces of the second and third flow guide members, which is advantageous for reducing the generation of thermal stress on the crystal surface. In the embodiments 3 and 4, the heat source is arranged in the accommodating space of the second flow guide member and the third flow guide member, which is more favorable for maintaining low thermal stress than the heat insulating material, and the temperature near the seed crystal is slightly lower, so that the effect is better.
It should be noted that the above-mentioned embodiment is only one of the examples provided by the present invention, and does not limit the implementation and protection scope of the present invention, and it should be appreciated by those skilled in the art that the equivalent alternatives and obvious variations made from the description of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A crucible apparatus for growing a silicon carbide single crystal by a sublimation method, comprising: a crucible part, a flow guide part and a porous graphite part;
the crucible component comprises a crucible outer wall and a crucible inner wall, 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 guide parts comprise a first flow guide part, a second flow guide part and a third flow guide part which are arranged close to the inner side of the side wall of the crucible;
the first flow guide component is arranged above an outlet of a first containing space formed by the inner wall of the crucible, the second flow guide component is arranged below the inner wall of the crucible, and the third flow guide component is arranged below the second flow guide component;
the space between the first flow guide part and the upper surface of the inner wall of the crucible is a first flow guide space, a second flow guide 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 guide part, the inner diameter of the flaring space is gradually increased from top to bottom, and a third flow guide space is formed between the outer side walls of the third flow guide part;
the first accommodating space is communicated with the first flow guide space, and the first flow guide space, the second flow guide space, the flaring space and the third flow guide space are sequentially communicated;
the bottom of the third flow guide space is provided with a silicon carbide seed crystal, the top of the third flow guide space is provided with a porous graphite part, and the space between the porous graphite part and the seed crystal is used for gas phase substance transmission and accommodating a growing single crystal.
2. A crucible apparatus for use in growing a silicon carbide single crystal by sublimation according to claim 1, wherein: the second diversion part is internally provided with a second containing space, the third diversion part is internally provided with a third containing space, a first heat source is arranged in the second containing space, and a second heat source is arranged in the third containing space.
3. The crucible device for growing a silicon carbide single crystal by the sublimation method 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 use in growing a silicon carbide single crystal by sublimation according to claim 1, wherein: also included is a rotating member.
5. A crucible apparatus for use in growing silicon carbide single crystals by sublimation according to claim 4, wherein: the rotating component is arranged on the top wall of the crucible and is positioned right above the inlet of the second diversion space.
6. A crucible apparatus for use in growing a silicon carbide single crystal by sublimation according to claim 1, wherein: the first receiving space is a circle surrounding the inner side of the side wall of the crucible.
7. A crucible apparatus for use in growing a silicon carbide single crystal by sublimation according to claim 1, wherein: the outer wall of the first flow guide part is obliquely arranged, and an included angle formed by the outer wall of the first flow guide part and a plane where the top of the inner wall of the crucible is located is 30-60 degrees.
8. A crucible apparatus for use in growing a silicon carbide single crystal by sublimation according to claim 1, wherein: and the outer surface of the porous graphite part is provided with a high-temperature resistant coating.
9. A crucible apparatus for use in growing a silicon carbide single crystal by sublimation according to claim 8, wherein: the porosity of the porous graphite component is 10% -90%.
10. A crucible apparatus for use in growing a silicon carbide single crystal by sublimation according to claim 8, wherein: the pore diameter range of the porous graphite component is 2 to 10 mu m.
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