CN212771047U - Preparation facilities of high quality major diameter SiC single crystal - Google Patents
Preparation facilities of high quality major diameter SiC single crystal Download PDFInfo
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- CN212771047U CN212771047U CN202021499230.4U CN202021499230U CN212771047U CN 212771047 U CN212771047 U CN 212771047U CN 202021499230 U CN202021499230 U CN 202021499230U CN 212771047 U CN212771047 U CN 212771047U
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Abstract
The utility model discloses a preparation device of high-quality large-diameter SiC single crystal, belonging to the field of SiC crystal growth, which comprises a crucible, a heat preservation layer, a heating device and a porous graphite barrel; wherein the crucible is positioned in the heat-insulating layer; the heating device is positioned on the outer side of the heat-insulating layer; the seed crystal and the porous graphite barrel are positioned in the crucible and are coaxial with the crucible; the SiC growth components of the utility model adopt a transportation mode from the raw material outside the crucible to the seed crystal inside, the process of crystal growth is a natural diameter expansion process, the diameter expansion of the crystal is not limited, meanwhile, the crystal grows along a nonpolar growth surface, and the threading dislocation density is greatly reduced compared with the growth along the C axis; c particles generated by the SiC raw material which is heated and carbonized along the crucible wall are effectively blocked by the SiC raw material and the porous graphite layer on the inner side, so that C inclusions in crystals are reduced, and the crystal quality is effectively improved.
Description
Technical Field
The utility model relates to a SiC crystal growth field especially relates to a preparation facilities of high quality major diameter SiC single crystal.
Background
In recent years, SiC has become an ideal material for manufacturing high-frequency, high-power, high-temperature resistant and radiation resistant devices, and the growth of high-quality SiC base materials has become a research hotspot. In the aspect of SiC single crystal growth technology, Physical Vapor Transport (PVT) is mainly adopted to grow SiC single crystals internationally. As shown in FIG. 1, the seed crystal is fixed at the top of the inside of the crucible, and the source material is at the bottom of the inside of the crucible. The induction coil surrounds the graphite crucible outside to heat the side wall of the graphite crucible, and the bottom raw material is gasified by heating and decomposed into Si and Si2C，SiC2And waiting for gas phase components, wherein the raw material is in a high temperature region, the seed crystal is in a relatively low temperature region, the related components of the gas phase SiC are conveyed to the surface of the seed crystal from the raw material under the drive of the axial temperature gradient, namely, the gaseous components are conveyed upwards under the drive of the axial temperature gradient, and the SiC crystal is driven to start to grow on the seed crystal due to the supersaturation caused by low temperature, so that the SiC crystal grows on the seed crystal again. In the thermal field heated by the induction coil, the coil surrounds the crucible at the side part, magnetic lines of force penetrate through the side wall of the crucible to generate heat, the seed crystal is arranged at the top of the inner side of the crucible, and the raw material is arranged at the bottom of the inner side of the crucible. The relative positions of the crucible and the coil are adjusted to enable the lower part of the crucible wall to generate the maximum heat, so that a temperature difference from the lower part to the upper part and from the crucible wall to the center of the crucible is formed in the crucible, SiC related gas components generated by heating raw materials are upwards transported to a seed crystal face to grow under the driving of a temperature gradient, and the structure determines the growth mode of the structure that the bottom raw materials are transported to the surface of a wafer-shaped seed crystal (the (0001) face of the SiC crystal), so that the thickness of the bottom raw materials is continuously increased to grow new crystals.
The limit of the diameter of the SiC crystal grown by the traditional PVT method is 8 inches at present, and the diameter difference with the diameter difference of the single crystal grown by CZ method such as Si and the like is large. The reason why the SiC crystal diameter cannot be made large is that the conventional PVT growth method cannot expand the diameter as fast as the czochralski method of Si single crystal. Due to the growth of the SiC crystal by the traditional PVT method, the crystal grows along the (0001) plane and is axially grown driven by an axial temperature gradient, and when the crystal needs to be expanded, a certain degree of transverse growth is needed. At this time, the temperature at the edge of the crystal is required to be lower, namely a certain radial temperature gradient, but just because the temperature at the edge of the crystal is lower, the sublimated SiC component is easy to nucleate at the position of dissimilar materials such as a graphite ring and the like next to the crystal, so that SiC polycrystal grows, and the diameter expansion failure is caused. The problem of expanding diameter has been a bottleneck hindering the growth of large diameter SiC crystals.
In the aspect of crystal quality, the thermal field for growing SiC single crystals by the traditional PVT method mostly adopts an induction coil to heat in a surrounding manner, the side wall of the crucible becomes a heat source, and SiC raw materials close to the wall of the graphite crucible can be carbonized very early, so that a large amount of free solid carbon is generated at the position, and the free carbon can not be effectively blocked, and can enter a crystal growth surface quickly under the action of axial temperature gradient and gas concentration difference to form a carbon wrap. Inclusions in SiC crystals induce other crystal defects such as micropipes, threading dislocations, and the like. With the gradual increase of the inclusions, the later grown crystals generate a large amount of dislocations and microtubule proliferation, and even polycrystallization occurs. Meanwhile, the conventional PVT method for growing SiC is to grow along a C-axis polar surface, and when SiC grows along a non-polar growth surface, compared with the growth along the C-axis polar surface, the SiC shows completely different growth dynamics and defect generation mechanisms, and the threading dislocation density is greatly reduced compared with the growth along the C-axis.
Therefore, there is a need to find a growing method and a corresponding thermal field structure, which can improve the quality and the quantity of the SiC single crystal at the same time, without limitation on the diameter expansion growth, with high relative crystallographic quality and few C inclusions.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a preparation facilities of high quality major diameter SiC single crystal to solve the problem that above-mentioned prior art exists, make the diameter of crystal very big that can be long, threading dislocation and C parcel in the crystal are less simultaneously, and the crystallography quality is higher.
For solving one of above-mentioned technical problem at least, the utility model discloses the technical scheme who takes is:
a production apparatus of a high-quality large-diameter SiC single crystal, comprising: the crucible, the insulating layer and the heating device also comprise a porous graphite barrel; wherein the content of the first and second substances,
the crucible is positioned in the heat insulation layer; the heating device is positioned on the outer side of the heat-insulating layer;
the porous graphite barrel is positioned in the crucible and is coaxial with the crucible, and a hollow interlayer is formed between the porous barrel body of the porous graphite barrel and the inner wall of the crucible.
Furthermore, seed crystals are fixedly arranged on the lower surface of the top cover of the crucible. Further preferably, a seed crystal is fixedly arranged between the lower surface of the top cover and the upper surface of the bottom of the crucible.
Furthermore, the seed crystal is in a round rod shape and is coaxial with the crucible.
Further, the heating device is an induction coil.
Further, the induction coil is a discrete multi-strand coil combination.
Further, the heat-insulating layer is a graphite hard felt or a graphite soft felt.
Further, the crucible is made of isostatic pressing graphite.
The utility model discloses at least, include following beneficial effect:
(1) the growth direction of the crystal in the utility model is vertical to the (0001) plane, the unique growth direction determines the diameter expanding direction of the crystal, namely the growth direction, and the growth direction are consistent, so the growth in the diameter direction of the crystal is not limited, and the diameter of the crystal can grow greatly; and the growth mode in the utility model grows along the nonpolar surface, when SiC grows along the nonpolar growth surface, the growth dynamics and defect generation mechanism which are completely different are displayed compared with the growth along the C-axis polar surface, and the threading dislocation density is greatly reduced compared with the growth along the C-axis, so the SiC crystal quality adopting the growth method of the utility model is higher;
(2) meanwhile, in the traditional PVT growth method, SiC growth components are conveyed upwards from a raw material position below a crucible so as to grow on seed crystals, the raw material close to the side wall of the crucible is preferentially carbonized due to the fact that a coil surrounds the crucible for heating, the upper part of the carbonized raw material is not effectively blocked, C particles are conveyed to the seed crystals too early to form C inclusions, a large number of defects are derived, and the single crystal structure is damaged; and the utility model provides a SiC growth component is from the raw materials in the crucible outside to the mode of transporting of inboard seed crystal, and the C granule that the SiC raw materials that is heated carbonization produced is effectively blockked by inboard SiC raw materials and porous graphite layer (staving) next to the crucible wall, and the free C granule that finally transports crystal surface has reduced to reduce the C parcel thing in the crystal, crystal quality has obtained effective improvement.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a device for preparing SiC crystals grown by a PVT method in the prior art.
FIG. 2 is a schematic structural view of a high-quality large-diameter SiC single crystal manufacturing apparatus of the present invention.
Fig. 3 is a high-resolution X-ray rocking curve test result of the high-quality large-diameter SiC single crystal wafer prepared in embodiment 1 of the present invention, wherein a is a wafer test point distribution diagram, b is a wafer test point characteristic spectrum peak diagram, and an abscissa ω in the diagram b represents a peak position and an ordinate represents intensity.
FIG. 4 is a comparison of visual inclusions between a high quality SiC wafer produced according to example 1 of the present invention and a SiC wafer produced by a conventional PVT process, wherein A is a SiC wafer grown by a conventional PVT process and B is an enlarged view of a microscope at a local E position of A; c is a high-quality SiC wafer grown in example 1 of the present invention, and D is an enlarged view of a microscope at a local F position of C.
Fig. 5 is a view showing dislocation corrosion observation of the SiC wafer produced in the prior art and in example 1 of the present invention, showing comparison of the penetration dislocation conditions between the two, where M is a view showing dislocation corrosion of the SiC wafer grown in the prior art, and N is a view showing dislocation corrosion of the SiC wafer grown in example 1 of the present invention.
The method comprises the following steps of 1-seed crystal, 2-porous graphite barrel, 3-crucible, 4-insulating layer, 5-heating device, 6-SiC raw material, 7-C wrap and 8-penetration dislocation.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
FIG. 1 is a schematic structural diagram of a prior art preparation device for growing SiC crystals by a PVT method, and as shown in FIG. 1, the outermost layer is a heating coil, the middle layer is an insulating layer, and the innermost layer is a crucible. The upper part in the crucible is fixed with a wafer-shaped seed crystal, the lower part is filled with SiC raw material, and the growth mode of the crucible is determined by the structure that the bottom raw material is conveyed to the surface of the wafer-shaped seed crystal (the (0001) surface of the SiC crystal), so that the thickness of the seed crystal is continuously increased to grow new crystals. The existing PVT method is used for growing SiC crystals according to the principle that: the raw material is arranged below the seed crystal and is heated, sublimated and decomposed into Si under certain pressure by heating the solid raw material2C，SiC2And (3) the gas phase components. At the moment, the raw material is in a high-temperature region, the seed crystal is in a relatively low-temperature region, the SiC related components in the gas phase are conveyed to the surface of the seed crystal from the raw material under the drive of the axial temperature gradient, and SiC crystals are driven to start to grow on the seed crystal in an arrangement mode due to the supersaturation brought by the low temperature. The disadvantages of the prior art are described in the background, and are not described herein.
For solving the technical problem of the prior art, the utility model discloses the utility model concept of taking mainly does: by discrete polyThe strand induction coil uniformly heats the side wall of the crucible to form a radial temperature difference with high outside and low inside (high outside raw material and low temperature at the middle seed crystal), and the heated outside SiC raw material is heated to sublimate and decompose into Si and Si2C，SiC2Gas phase components are transported to the seed crystal in the middle through the pores on the barrel body of the porous graphite barrel, and SiC crystals are driven to start to grow on the seed crystal due to supersaturation caused by low temperature, so that SiC grows along a nonpolar growth surface, completely different growth dynamics and defect generation mechanisms are displayed compared with growth along a C-axis polar surface, and the threading dislocation density is greatly reduced compared with growth along the C-axis; the porous graphite bucket staving can also be in the middle of not influencing the SiC gaseous phase component and carry out the effectual solid-state C granule that wraps up in the middle of screening off under the condition that transports, the C granule that the SiC raw materials that is heated and carbonized promptly next to the crucible wall produced is effectively blockked by inboard SiC raw materials and porous graphite layer (staving), and the free C granule that finally transports crystal surface has reduced to reduce the C parcel thing in the crystal, the crystal quality has also obtained effective improvement.
In order to make the above objects, features and advantages of the present invention more comprehensible, the present invention is described in detail with reference to the accompanying drawings and the detailed description.
According to the embodiment of the utility model, fig. 2 is the utility model discloses high quality major diameter SiC single crystal's preparation facilities schematic structure, it is shown with reference to fig. 2, the utility model discloses high quality major diameter SiC single crystal's preparation facilities mainly includes: the device comprises a crucible, a heat insulation layer, a heating device and a porous graphite barrel; the crucible is positioned in the heat insulation layer, the heating device is positioned on the outer side of the heat insulation layer, the heat insulation layer is made of heat insulation materials with high temperature resistance and low heat conductivity, the crucible is wrapped, heat loss can be prevented, radial temperature difference with high outside and low inside is formed, and the SiC raw material which is heated and sublimated is conveyed to the seed crystal in the middle to start growing; the porous graphite barrel is positioned in the crucible and is coaxial with the crucible, and the porous graphite barrel is of a porous structure and can prevent the transportation of C particles under the condition that the effective transportation of SiC powder is not influenced.
The seed crystal is arranged between the lower surface of the top cover of the crucible and the upper surface of the bottom of the crucible, is of a round rod-shaped structure, is fixed in the middle of the crucible and is coaxial with the crucible, a layer of component growth cavity surrounds the outside of the seed crystal, a hollow interlayer of porous graphite and the crucible wall is arranged outside the seed crystal, and SiC raw materials are filled in the middle of the seed crystal.
According to some embodiments of the utility model, the seed crystal is still high with crucible inside height, and seed crystal upper end contact crucible top cap, seed crystal lower extreme contact crucible bottom inner wall promptly.
Heating device can be induction coil, and the induction coil number is unrestricted, sets up according to concrete growth needs, according to the utility model discloses a some embodiment, induction coil set up to the combination of discrete stranded coil.
The heat preservation layer is made of hard graphite felt or soft graphite felt, and the crucible is made of isostatic pressing graphite.
The method for preparing the high-quality large-diameter SiC single crystal by using the preparation device comprises the following steps:
(1) fixing a seed crystal between the lower surface of the top cover of the crucible and the upper surface of the bottom of the crucible;
(2) filling a SiC raw material into a hollow interlayer between the crucible and the porous graphite barrel;
(3) vacuumizing to make the vacuum degree in the crucible less than or equal to 10-4Pa, introducing inert gas to the pressure of 100 Kpa;
(4) starting a heating device, taking a contact point of the seed crystal and a crucible top cover as a temperature measuring point, heating and raising the temperature to the temperature of 1800 plus 2200 ℃ and reducing the pressure to 500 plus 2000Pa so as to sublimate the SiC raw material between the porous graphite barrel and the crucible, conveying the sublimated Si and C components to the surface of the SiC seed crystal in the middle through the pores on the porous barrel body of the porous graphite barrel under the driving of radial temperature gradient from outside to inside, and starting crystal growth under a certain supersaturation degree;
(5) after the crystal grows for 100-150h, introducing inert gas to increase the pressure to 100KPa, stopping the growth of the crystal, cooling to room temperature, and taking out the crystal which finishes the growth.
Example 1
1. A crucible of isostatic graphite is used as a heat source for induction heating;
2. a round bar-shaped SiC seed crystal is fixed in the middle of the crucible, and the SiC seed crystal is formed by cutting a crystal grown by a traditional PVT method according to the (0001) direction;
3. the porous graphite barrel is positioned in the crucible and is coaxial with the crucible; filling a SiC raw material into a hollow interlayer between the crucible and the porous graphite barrel;
4. the graphite soft felt is used as a heat insulation layer to surround the crucible to prevent heat loss and form radial temperature difference with high outside and low inside;
5. the outermost periphery is a Cu induction coil which is used for generating an electromagnetic field to heat the crucible, and in order to ensure that different positions of the side wall of the crucible generate heat uniformly, the induction coil is a combination of discrete multi-strand coils;
6. vacuumizing until the vacuum degree in the crucible is less than or equal to 10-4Pa, introducing Ar gas until the pressure in the crucible is 100kpa, heating to raise the temperature to 2000 ℃ by taking the contact point of the seed crystal and the crucible top cover as a temperature measuring point, reducing the pressure to 1000Pa to sublimate the SiC raw material between the porous graphite and the crucible, conveying the sublimated Si and C components to the surface of the middle SiC seed crystal under the driving of the radial temperature gradient from outside to inside, and starting crystal growth under a certain supersaturation degree; and after 130h, raising the pressure to 100kpa to stop the growth of the crystal, and then cooling to room temperature and taking out the crystal.
Carrying out a high-resolution X-ray rocking curve test on the high-quality large-diameter SiC single crystal wafer prepared in example 1; the results are shown in a and b in fig. 3, and show that the full width at half maximum of all data points of 9 sample regions distributed at different positions is less than 20 arc seconds, which proves that the crystal has good crystallization quality and few related defects. It is understood that the calculation of the full width at half maximum is conventional in the art and will not be described herein.
To prior art and the utility model discloses the SiC single crystal piece of embodiment 1 preparation carries out dislocation corrosion and observes with the microscope with melting KOH respectively, and the result shows to compare in prior art, the utility model discloses penetration dislocation (hexagon etch pit) density greatly reduced in the SiC single crystal piece of embodiment 1 preparation, and the crystal quality is higher, as shown in fig. 5.
Moreover, the diameter of the high-quality large-diameter SiC monocrystal prepared in the embodiment 1 is measured, and can reach or even exceed 8 inches, which greatly exceeds the level of 4-6 inches of the diameter of the monocrystal prepared by the traditional PVT method; visual and microscopic comparative observation is carried out on the SiC single crystal wafer prepared by the traditional PVT method and the high-quality large-diameter SiC single crystal wafer prepared in the example 1, as shown in figure 4, the obvious aggregation of the wrappage C of the lens grown by the traditional method is shown, as shown in the local E of the figure A, the density of the wrappage C is high, the distribution quantity of black points in the figure B is shown, and the figure C shows that the aggregation of the wrappage C is not observed obviously on the SiC single crystal wafer prepared in the example 1 of the utility model, the quantity of the black points in the figure D is extremely small, the density of the wrappage C is greatly reduced, and the condition of the wrappage C is effectively improved.
Therefore, through the practical test prove, use the utility model discloses the crystal diameter that grows out is great, and crystal quality is higher, defect density greatly reduced such as C parcel.
The above-mentioned embodiments are only intended to describe the preferred embodiments of the present invention, but not to limit the scope of the present invention, and those skilled in the art should also be able to make various modifications and improvements to the technical solution of the present invention without departing from the spirit of the present invention, and all such modifications and improvements are intended to fall within the scope of the present invention as defined in the appended claims.
Claims (7)
1. A production apparatus of a high-quality large-diameter SiC single crystal, comprising: the crucible, the insulating layer and the heating device are characterized by also comprising a porous graphite barrel; wherein the content of the first and second substances,
the crucible is positioned in the heat insulation layer; the heating device is positioned on the outer side of the heat-insulating layer;
the porous graphite barrel is positioned in the crucible and is coaxial with the crucible, and a hollow interlayer is formed between the porous barrel body of the porous graphite barrel and the inner wall of the crucible.
2. The preparation device as claimed in claim 1, wherein a seed crystal is fixedly arranged on the lower surface of the top cover of the crucible.
3. A production apparatus according to claim 2, wherein said seed crystal is in the form of a round rod, coaxial with said crucible.
4. The manufacturing apparatus of claim 1, wherein the heating device is an induction coil.
5. The manufacturing apparatus of claim 4, wherein the induction coil is a discrete multi-strand coil assembly.
6. The manufacturing device of claim 1, wherein the heat insulating layer is a graphite hard felt or a graphite soft felt.
7. A production apparatus according to any one of claims 1 to 3, wherein the crucible is of an isostatically pressed graphite material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113584571A (en) * | 2021-06-17 | 2021-11-02 | 山东大学 | Low-cost and high-yield SiC single crystal growth method |
| CN115142132A (en) * | 2022-06-02 | 2022-10-04 | 江苏集芯半导体硅材料研究院有限公司 | Silicon carbide crystal growth device and large-size silicon carbide crystal growth method |
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2020
- 2020-07-27 CN CN202021499230.4U patent/CN212771047U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113584571A (en) * | 2021-06-17 | 2021-11-02 | 山东大学 | Low-cost and high-yield SiC single crystal growth method |
| CN113584571B (en) * | 2021-06-17 | 2023-03-10 | 山东大学 | Low-cost and high-yield SiC single crystal growth method |
| CN115142132A (en) * | 2022-06-02 | 2022-10-04 | 江苏集芯半导体硅材料研究院有限公司 | Silicon carbide crystal growth device and large-size silicon carbide crystal growth method |
| CN115142132B (en) * | 2022-06-02 | 2024-03-19 | 江苏集芯先进材料有限公司 | Silicon carbide crystal growth device and growth method of large-size silicon carbide crystal |
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