CN111172592B - Doped silicon carbide single crystal, substrate, preparation method and used device - Google Patents
Doped silicon carbide single crystal, substrate, preparation method and used device Download PDFInfo
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- CN111172592B CN111172592B CN201911349956.1A CN201911349956A CN111172592B CN 111172592 B CN111172592 B CN 111172592B CN 201911349956 A CN201911349956 A CN 201911349956A CN 111172592 B CN111172592 B CN 111172592B
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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
- 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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- 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
Abstract
The application discloses a doped silicon carbide single crystal, a doped silicon carbide substrate, a preparation method and a used device, and belongs to the field of semiconductor material preparation. The preparation method comprises the following steps: loading raw materials into a raw material cavity formed by an interlayer on the side wall of a crucible, installing a seed crystal column in the crucible, and putting the seed crystal column into a crystal growth furnace after assembly; raising the temperature of the crystal growth furnace to ensure that the sublimated gas of the raw materials after sublimation passes through the inner side wall of the interlayer and is transmitted to the surface of the seed crystal column along the radial direction in a gas phase manner to grow crystals to obtain the doped silicon carbide single crystal; said comprises silicon carbide, and; the raw material also comprises a solid phase dopant and/or a gas phase dopant which is introduced into the crucible. The method can prepare doped silicon carbide single crystals with any volume, and particularly has the advantages of large volume, high thickness, high crystal growth efficiency and more cut substrates; the zero micropipe and the screw dislocation of the doped silicon carbide single crystal prepared by the method are less than 100cm‑2And edge dislocation density of less than 220cm‑2Defect density reaches even zero; the method lays a technical foundation for large-scale commercialization of the high-quality and low-cost doped silicon carbide substrate.
Description
Technical Field
The application relates to a doped silicon carbide single crystal, a doped silicon carbide substrate, a preparation method and a used device, and belongs to the field of semiconductor material preparation.
Background
The existing silicon carbide preparation technology is mainly based on a physical vapor transport (PVT for short). The PVT method is formed by sublimating and decomposing a silicon carbide raw material placed at the bottom and transmitting the silicon carbide raw material to a seed crystal along an axial temperature gradient for crystallization. The sheet seed crystal used by the PVT method in the prior art is arranged at the top of the crucible, and the silicon carbide single crystal grows vertically and downwards along a certain radial direction of the single crystal.
Since the growth of the silicon carbide single crystal is limited by the distance from the growth surface of the single crystal and the surface of the raw material when growing downward, the crystal growth thickness is usually in the range of 20 to 50mm, and the yield of the substrate made of the silicon carbide single crystal is low. In addition, defects such as micropipes and dislocations in the silicon carbide seed crystal penetrate the silicon carbide single crystal and the seed crystal prepared therefrom in the <0001> direction in many cases. These defects will continue to be inherited into the newly grown single crystal and continue to form through defects during the growth of the single crystal, so that the control of the defect density in the single crystal and the substrate is difficult, the cost is high, and the improvement of the substrate quality is difficult.
Nature reports a silicon carbide single crystal preparation method for avoiding inheritance of defects such as micropipes and dislocation through cross section growth of a crystal, but the method has the disadvantages of complicated preparation process, high cost and inapplicability to industrial production process, and can reduce the defect density.
Disclosure of Invention
In order to solve the problems, the application provides a doped silicon carbide single crystal, a substrate, a preparation method and a device used by the method. The doped silicon carbide single crystal can be in any size, particularly in any thickness, the production efficiency is high, and the density of zero micropipe, screw dislocation and edge dislocation can be reduced to zero; the substrate has high wafer yield and high quality; the preparation method can prepare the doped silicon carbide single crystal and the substrate with high efficiency and high quality; the doped silicon carbide single crystal and the substrate are stable and have high conductivity.
According to one aspect of the present application, there is provided a method for producing a large-sized doped silicon carbide single crystal, which can produce a doped silicon carbide single crystal of an arbitrary volume, particularly a large volume and a high thickness, with high crystal growth efficiency, and a large number of cut substrates; the zero micropipe and the screw dislocation of the doped silicon carbide single crystal prepared by the method are less than 100cm-2And edge dislocation density of less than 220cm-2The defect density can even reach zero; the method lays a technical foundation for large-scale commercialization of the silicon carbide substrate with high quality and low cost; the doped silicon carbide single crystal and the substrate are stable and have high conductivity.
The preparation method of the doped silicon carbide single crystal comprises the following steps:
1) providing a crucible and a seed crystal column;
2) loading raw materials into a raw material cavity formed by an interlayer on the side wall of a crucible, installing a seed crystal column in the crucible, and putting the seed crystal column into a crystal growth furnace after assembly;
3) raising the temperature of the crystal growth furnace to ensure that the sublimated gas of the raw material after sublimation passes through the inner side wall of the interlayer and is transmitted to the surface of the seed crystal column along the radial gas phase for crystal growth, thus obtaining the doped silicon carbide single crystal;
wherein the raw materials comprise a silicon carbide raw material and,
the raw material also comprises a doping agent, and the doping agent comprises a solid phase doping agent contained in the raw material cavity and/or a gas phase doping agent filled in the crucible.
Optionally, in the crystal growth process, the temperature difference between the inner surface of the inner side wall and the surface of the seed crystal is 50-300 ℃. Preferably, in the crystal growth process, the temperature difference between the inner surface of the inner side wall and the surface of the seed crystal is 100-200 ℃. The temperature is set in such a way that there is a sufficient temperature gradient between the inner surface and the seed crystal as a driving force to cause the sublimed gaseous components to be transported laterally toward the seed crystal in the center of the crucible.
Preferably, the crystal growth temperature is 2000-2300 ℃, and the crystal growth pressure is 5-50 mbar.
Optionally, the solid-phase dopant is selected from at least one of elemental phosphorus, elemental germanium, elemental tin, elemental arsenic, a phosphorus compound, a germanium compound, a tin compound and an arsenic compound, and/or the gas-phase dopant is nitrogen.
Preferably, the solid-phase dopant comprises low-resistance silicon single crystal powder.
Preferably, inert gas and gas phase dopant are introduced into the crucible. Preferably, the inert gas is nitrogen or helium, and the gas phase dopant is nitrogen. The gas phase dopant is nitrogen gas, so that the conductive N-type doped silicon carbide single crystal can be prepared, and the amount of the nitrogen gas is determined according to the resistivity of the doped silicon carbide single crystal prepared according to the requirement. Of course, the gas phase dopant can also be any gas that is desired to be incorporated into the doped silicon carbide single crystal.
Optionally, the side wall of the crucible comprises an interlayer comprising an inner side wall and an outer side wall, the inner side wall having a higher porosity than the outer side wall, the interlayer forming a feedstock chamber;
the seed crystal column and the extension direction of the central axis of the crucible are approximately same, and a long crystal cavity is formed between the seed crystal column and the inner surface of the inner side wall.
Optionally, the seed crystal column is obtained by cutting and polishing a single crystal column, and the surface of the seed crystal column is a smooth crystalline surface.
Optionally, the interlayer is arranged corresponding to the height of the seed crystal column, and the seed crystal column and the crucible share a central axis.
Preferably, the distance D1 between the inner side wall and the outer side wall is 50-300 mm.
Preferably, the distance D2 between the inner surface of the inner side wall and the surface opposite to the seed crystal column is 100-300 mm.
Further, the range of D1 values has a lower limit selected from 70mm, 100mm, 120mm, 140mm, 160mm, 180mm, 200mm, 220mm, 240mm, 260mm, or 280mm and an upper limit selected from 70mm, 100mm, 120mm, 140mm, 160mm, 180mm, 200mm, 220mm, 240mm, 260mm, or 280 mm. Further, the D1 is 120mm-200mm, and the D1 is preferably 140mm-180 mm.
Further, the range of D2 values has a lower limit selected from 120mm, 140mm, 160mm, 180mm, 200mm, 220mm, 240mm, 260mm or 280mm and an upper limit selected from 120mm, 140mm, 150mm, 160mm, 170mm, 180mm, 200mm, 220mm, 240mm, 260mm or 280 mm. Further, the D1 is 150mm-240mm, preferably 170mm-220mm at the D1 position.
Optionally, the interlayer extends upward from the bottom of the crucible, and the seed column extends upward from the bottom of the crucible. Preferably, the interlayer extends from the bottom of the crucible to the top of the crucible, and the seed column extends from the bottom of the crucible to the top of the crucible.
Optionally, the bottom and/or the top of the crucible are distributed with slots for installing the seed crystal columns. Preferably, the clamping groove is in an equilateral hexagon corresponding to the seed crystal column.
Optionally, the silicon carbide seed crystal is arranged as a hexagonal system seed crystal, the doped silicon carbide single crystal is a hexagonal system single crystal, and the seed crystal column is arranged as a hexagonal prism including six equivalent crystal planes.
Preferably, the width of the equivalent crystal plane is 5 to 20 mm. Preferably, the width of the equivalent crystal plane is 7 to 15 mm.
Preferably, if the crystal face indexes of the long crystal faces are the same, the prepared single crystal is in the same shape as the crystal form of the seed crystal column.
Preferably, the six equivalent crystal planes of the seed column are <1120> <11-20> < -1120> <1-120> <1-1-20> respectively; or the six equivalent crystal planes of the seed column are <10-10> <01-10> < 1100> < 1010> <0-110> <1-100> respectively.
Preferably, the seed crystal column is integrated or spliced along the axial direction of the seed crystal column, the axial length of the seed crystal column is not less than 100mm, and the axial length of the single crystal is not less than 100 mm.
Optionally, the crucible is a graphite crucible. Preferably, the side wall of the crucible is a porous graphite plate, the porosity of the inner side wall is 40% -60%, and the pore diameter of the inner side wall is not higher than 1 μm. The porosity of the outer side wall is not more than 10%, and the pore diameter of the outer side wall is not more than 1 μm.
Optionally, the seed crystal column is integrally arranged or spliced along the axial direction of the seed crystal column. The seed crystal columns can be directly stacked or bonded. Due to the limitation of seed crystal preparation, a plurality of seed crystal columns can be spliced axially to lengthen the length of the seed crystal columns, so that the thickness of the prepared doped silicon carbide single crystal is improved. The prepared single crystal is cut into a flaky single crystal substrate along the radial direction, so that the defects of the single crystal grown at the splicing part can be cut off; in order to improve the single crystal utilization rate, the cut defective single crystal may be used as a raw material for preparing the single crystal.
Optionally, the axial length of the seed crystal column is not less than 100mm, and the axial length of the single crystal is not less than 100 mm. Preferably, the axial length of the seed crystal column is not less than 120mm, and the axial length of the single crystal is not less than 120 mm. More preferably, the axial length of the seed column is not less than 150mm, and the axial length of the single crystal is not less than 150 mm.
According to another aspect of the present application, there is provided a crucible comprising a crucible for use in any one of the above-described preparation methods.
According to another aspect of the present application, there is provided a silicon carbide seed column including the seed column used in any one of the above-described production methods.
According to another aspect of the present application, there is provided a doped silicon carbide single crystal produced by the method described in any one of the above, having an axial length of not less than 100mm and a defect density of less than 50cm-2。
Preferably, the doped silicon carbide single crystal has a resistivity of 10 to 20m Ω. More preferably, the doped silicon carbide single crystal has a resistivity of 10 to 15m Ω.
Preferably, the concentration of nitrogen in the doped silicon carbide single crystal is 1018cm-3-1020cm-3And, the concentration of phosphorus in the doped silicon carbide single crystal is 1017cm-3％-1019cm-3(ii) a Or
The concentration of nitrogen in the doped silicon carbide single crystal is 1019cm-3-1020cm-3。
More preferably, the concentration of nitrogen in the doped silicon carbide single crystal is 1019cm-3-1020cm-3And, the concentration of phosphorus in the doped silicon carbide single crystal is 1018cm-3％-1019cm-3(ii) a Or
The nitrogen concentration in the doped silicon carbide single crystal is 1019cm-3-1020cm-3。
Preferably, the screw dislocation of the doped silicon carbide single crystal is less than 90cm-2(ii) a More preferably, the doped silicon carbide single crystal screw dislocations are less than 70cm-2。
Optionally, the edge dislocation of the doped silicon carbide single crystal is less than 220cm-2. Preferably, the doped silicon carbide single crystal screw dislocation is less than 180cm-2. More preferably, the doped silicon carbide single crystal screw dislocations are less than 130cm-2。
According to another aspect of the present application, there is provided a doped silicon carbide single crystal substrate made of any one of the doped silicon carbide single crystals described aboveCrystal cutting and polishing, the doped silicon carbide single crystal of the doped silicon carbide single crystal substrate has a screw dislocation defect density of less than 50cm-2. Preferably, the doped silicon carbide single crystal substrate has a resistivity of 10-20m Ω;
preferably, the concentration of nitrogen in the doped silicon carbide single crystal substrate is 1018cm-3-1020cm-3And the concentration of phosphorus in the doped silicon carbide single crystal substrate is 1017cm-3-1019cm-3(ii) a Or
The concentration of nitrogen in the doped silicon carbide single crystal substrate was 1019cm-3-1020cm-3。
More preferably, the doped silicon carbide single crystal substrate has a resistivity of 10 to 15m Ω.
More preferably, the concentration of nitrogen in the doped silicon carbide single crystal substrate is 1019cm-3-1020cm-3And the concentration of phosphorus in the doped silicon carbide single crystal substrate is 1018cm-3-1019cm-3(ii) a Or
The mass percentage of nitrogen in the doped silicon carbide single crystal substrate is 1019cm-3-1020cm-3。
Preferably, the screw dislocation of the doped silicon carbide single crystal substrate is less than 90cm-2(ii) a More preferably, the threading dislocation of the doped silicon carbide single crystal substrate is less than 70cm-2。
Optionally, the edge dislocation of the doped silicon carbide single crystal substrate is less than 220cm-2. Preferably, the screw dislocation of the doped silicon carbide single crystal substrate is less than 180cm-2. More preferably, the threading dislocation of the doped silicon carbide single crystal substrate is less than 130cm-2。
According to an aspect of the present application, there is provided a crucible assembly for PVT method for manufacturing single crystal, which is capable of manufacturing single crystal having a large thickness when manufacturing single crystal by PVT method, so that a yield of a substrate manufactured from single crystal is high; when the method is used for preparing the doped silicon carbide single crystal, the efficiency is high, the defect density of the prepared doped silicon carbide single crystal is low, and the technical foundation is laid for large-scale commercialization of the doped silicon carbide single crystal substrate.
The crucible assembly for preparing the single crystal by the PVT method comprises a crucible and a seed crystal column arranged in the crucible; the side wall of the crucible comprises an interlayer, the interlayer comprises an inner side wall and an outer side wall, the inner side wall has higher porosity than the outer side wall, and the interlayer forms a raw material cavity; the seed crystal column and the extension direction of the central axis of the crucible are approximately same, and a long crystal cavity is formed between the seed crystal column and the inner surface of the inner side wall.
Optionally, the seed crystal column is obtained by cutting and polishing a single crystal column, and the surface of the seed crystal column is a smooth crystalline surface.
Optionally, the interlayer is disposed corresponding to the height of the seed crystal column, and the seed crystal column has the crucible common axis.
Optionally, the distance D1 between the inner side wall and the outer side wall is 50-300mm, and the distance D2 between the inner surface of the inner side wall and the surface opposite to the seed crystal column is 100-300 mm.
Optionally, the interlayer extends upward from the bottom of the crucible, and the seed column extends upward from the bottom of the crucible. Preferably, the interlayer extends from the bottom of the crucible to the top of the crucible, and the seed column extends from the bottom of the crucible to the top of the crucible.
Optionally, the bottom and/or the top of the crucible are distributed with slots for installing the seed crystal columns. Preferably, the clamping groove is in an equilateral hexagon corresponding to the seed crystal column.
Optionally, the seed crystal is a hexagonal seed crystal, and the single crystal is a hexagonal single crystal.
Alternatively, the seed column is configured as a hexagonal prism comprising six equivalent crystal planes.
Alternatively, the equivalent crystal plane has a width of 5 to 20 mm. Preferably, the width of the equivalent crystal plane is 7 to 15 mm.
Preferably, if the crystal face indexes of the long crystal faces are the same, the prepared single crystal is in the same shape as the crystal form of the seed crystal column.
Preferably, the six equivalent crystal planes of the seed column are <1120> <11-20> < -1120> <1-120> <1-1-20> respectively; or the six equivalent crystal planes of the seed column are <10-10> <01-10> < 1100> < 1010> <0-110> <1-100> respectively.
Optionally, the seed crystal column is a silicon carbide seed crystal column, and the single crystal is a doped silicon carbide single crystal. Preferably, the doped silicon carbide single crystal is an α silicon carbide single crystal, which has a hexagonal crystal structure.
Optionally, the crucible is a graphite crucible. Preferably, the side wall of the crucible is a porous graphite plate, the porosity of the inner side wall is 40% -60%, and the pore diameter of the inner side wall is not higher than 1 μm. The porosity of the outer side wall is not more than 10%, and the pore diameter of the outer side wall is not more than 1 μm.
Optionally, the seed crystal column is integrally arranged or spliced along the axial direction of the seed crystal column. The seed crystal columns can be directly stacked or bonded. Due to the limitation of seed crystal preparation, a plurality of seed crystal columns can be spliced axially to lengthen the length of the seed crystal columns, so that the thickness of the prepared doped silicon carbide single crystal is improved. The prepared single crystal is cut into a flaky single crystal substrate along the radial direction, so that the defects of the single crystal grown at the splicing part can be cut off; in order to improve the single crystal utilization rate, the cut defective single crystal may be used as a raw material for preparing the single crystal.
Optionally, the axial length of the seed crystal column is not less than 100mm, and the axial length of the single crystal is not less than 100 mm. Preferably, the axial length of the seed crystal column is not less than 120mm, and the axial length of the single crystal is not less than 120 mm. More preferably, the axial length of the seed column is not less than 150mm, and the axial length of the single crystal is not less than 150 mm.
Optionally, the crucible assembly is suitable for use in any one of the above methods for producing a doped silicon carbide single crystal for use in producing any one of the above doped silicon carbide single crystal and a substrate.
Optionally, the crucible in the crucible assembly is suitable for any one of the crucibles described above, and the seed crystal column in the crucible assembly is suitable for any one of the seed crystal columns described above.
According to one aspect of the application, a crystal growth furnace comprising any one of the crucible assemblies is provided, and the crystal growth furnace is heated in a mode that the side wall of the crucible generates heat, so that raw materials in the interlayer are heated to be sublimated to the seed crystal column for crystal growth, the thickness of the prepared single crystal is large, and the number of substrates prepared from the single crystal is large; when the method is used for preparing the doped silicon carbide single crystal, the efficiency is high, the defect density of the prepared doped silicon carbide single crystal is low, and the technical foundation is laid for large-scale commercialization of the doped silicon carbide single crystal substrate.
This contain long brilliant stove of any above-mentioned crucible subassembly, still include heating coil and insulation construction, insulation construction is established to the crucible overcoat, heating coil centers on insulation construction's lateral wall sets up. The induction coil is a medium-frequency induction coil.
Optionally, the crystal growth furnace comprises a furnace body, the furnace body is a quartz furnace, the crucible assembly is arranged outside the heat insulation structure and then placed in the furnace body, and the outer side wall of the furnace body is surrounded by the induction coil.
Benefits that can be produced by the present application include, but are not limited to:
1. according to the preparation method of the doped silicon carbide single crystal, the prepared doped silicon carbide single crystal can be any size, particularly has large thickness which can be larger than 100mm, so that the substrate prepared from the doped silicon carbide single crystal is high in wafer yield, and a technical foundation is laid for large-scale commercialization of the doped silicon carbide single crystal substrate.
2. The preparation method of the large-size doped silicon carbide single crystal has high efficiency, the prepared doped silicon carbide single crystal has low defect density, and zero micropipe and screw dislocation lower than 100cm are prepared-2And edge dislocation density of less than 220cm-2The defect density of the high-quality doped silicon carbide single crystal can be reduced to zero.
3. According to the preparation method of the large-size doped silicon carbide single crystal, the low resistance is realized by doping the gas-phase dopant and the solid-phase dopant together; besides the dopant, the low-resistance silicon single crystal material doped with phosphorus and the like can be selected and mixed with the conventional SiC powder, so that the codoping of silicon, phosphorus and the like is realized, the doping is improved, and simultaneously, the reaction substance is supplemented through the reaction of silicon and redundant carbon, and the crystal quality is improved.
4. The large-size doped silicon carbide single crystal provided by the application can be any size, particularly any thickness, and has zero micropipe and screw dislocation lower than 100cm-2And edge dislocation density of less than 220cm-2And may approach zero.
5. The large-size doped silicon carbide single crystal provided by the application has high substrate quality, and zero micropipe and screw dislocation are lower than 100cm-2And edge dislocation density of less than 220cm-2And may approach zero.
6. The large-size doped silicon carbide single crystal and the substrate have high substrate quality and good conductivity.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a schematic view of a crucible assembly according to an embodiment of the present application.
Detailed Description
In order to more clearly explain the overall concept of the present application, the following detailed description is given by way of example in conjunction with the accompanying drawings.
So that the manner in which the above recited objects, features and advantages of the present application can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to the embodiments thereof which are illustrated in the appended drawings. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, however, the present application may be practiced in other ways than those described herein, and therefore the scope of the present application is not limited by the specific embodiments disclosed below.
In addition, in the description of the present application, it is to be understood that the terms "center", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", "radial", "circumferential", and the like, indicate orientations and positional relationships based on those shown in the drawings, are only for convenience of description and simplicity of description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present application.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.
In this application, unless expressly stated or limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can include, for example, fixed connections, removable connections, or integral parts; the connection can be mechanical connection, electrical connection or communication; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
In this application, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through intervening media. In the description herein, reference to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Referring to fig. 1, an embodiment of the present application discloses a crucible assembly for preparing a single crystal by a PVT process, which includes a crucible and a seed crystal column 6 disposed in the crucible; the side wall of the crucible comprises an interlayer, the interlayer comprises an inner side wall 8 and an outer side wall 2, the inner side wall 8 has higher porosity than the outer side wall 2, and the interlayer forms a raw material cavity 4; the axial direction of the seed crystal column 6 extends along the side wall of the crucible, and a long crystal cavity is formed between the seed crystal column 6 and the inner surface of the inner side wall 8. The crucible assembly can produce a single crystal having a large thickness when the single crystal is produced by the PVT method, so that the number of substrates produced from the single crystal is large; the method has high efficiency when being used for preparing the doped silicon carbide single crystal, and the prepared doped silicon carbide single crystal has low defect density, thereby laying a technical foundation for large-scale commercialization of the doped silicon carbide single crystal substrate.
Alternatively, part or all of the height area of the sidewall is provided as an interlayer, and when part of the height area of the sidewall is provided as an interlayer, the interlayer may be provided at any height position of the sidewall.
In order to improve the crystal growth efficiency and make the shape of the single crystal uniform, the interlayer is arranged at a height corresponding to that of the seed crystal column 6, and the seed crystal column 6 has a crucible common axis, so that the side walls of the seed crystal column 6 are simultaneously subjected to crystal growth.
In an embodiment not shown, the interlayer extends upwards from the bottom of the crucible, i.e. the inner and outer side walls 8, 2 extend upwards from the bottom of the crucible and are connected to the remainder of the crucible side walls. Preferably, referring to fig. 1, the interlayer extends from the bottom of the crucible to the top of the crucible, and the seed crystal column 6 extends from the bottom of the crucible to the top of the crucible, the seed crystal column 6 being disposed corresponding to the interlayer. The interlayer arrangement mode can efficiently prepare large-volume single crystals, and the fixing mode of the seed crystal column 6 is simple.
In one embodiment, the sandwich of inner and outer walls 8, 2 forms a feedstock chamber 4, the feedstock chamber 4 being used to hold feedstock, such as silicon carbide powder used in the preparation of doped silicon carbide single crystals. Preferably, the distance D1 between inside wall 8 and the lateral wall 2 is 50-300mm, and D1's setting mode makes the crucible lateral wall generate heat when, can guarantee that the heat from lateral wall 2 to the high-efficient transmission of seed crystal post 6 direction, guarantees simultaneously that raw materials sublimation temperature and the long brilliant face's of seed crystal post 6 temperature is in the long brilliant temperature range of needs, low-power consumption, low cost.
As an implementation mode, a long crystal cavity is formed between the seed crystal column 6 and the inner surface of the inner side wall 8, and the distance D2 between the inner surface of the inner side wall 8 and the surface opposite to the seed crystal column 6 is 100-300 mm. The arrangement mode of the D2 can ensure the crystal growth quality, the crystal growth volume and the crystal growth efficiency of crystal growth. Preferably, the crucible is of a roughly cylindrical structure, the interlayer is of a cylindrical ring structure, and the combination of D1 and D2 can efficiently prepare large-volume high-quality single crystals.
In order to fix the seed crystal column 6 in the crucible, clamping grooves are distributed at the positions where the seed crystal column 6 needs to be fixed, such as the bottom and/or the top of the crucible, so that the seed crystal column 6 is inserted into the clamping grooves to be fixedly installed, and the shape of the clamping grooves is matched with the shape of the cross section of the seed crystal column 6. In one embodiment, when the seed column 6 has a hexagonal prism shape, the chucking groove is provided in an equilateral hexagon corresponding to the seed column 6. The clamping groove can be arranged in an upward protruding or concave structure relative to the inner side of the bottom wall of the crucible.
The seed crystal can be in any crystal form, the species and the crystal form of the seed crystal and the single crystal are the same, and the shape of the seed crystal column 6 can be in any columnar structure, such as a square prism, a cylinder or a hexagonal prism. Preferably, the seed crystal is a hexagonal system seed crystal, and the single crystal is a hexagonal system single crystal; more preferably, the seed column 6 is provided as a hexagonal prism including six equivalent crystal planes which are symmetrical, and the shape of the seed column 6 is set so that the single crystal produced grows uniformly to the periphery. Alternatively, the width of the equivalent crystal plane is 5 to 20 mm. Preferably, the width of the equivalent crystal plane is 7 to 15 mm. The width of the equivalent crystal face is set to ensure that the crystal can equally grow transversely at a uniform speed in a uniform thermal field taking the crucible axis as the symmetry center, thereby keeping the same axial position of the crystal, namely the consistency and uniformity of the quality in the wafer of the substrate finished by subsequent processing. The equivalent crystal face is used as a seed crystal growth face for growth, so that the inheritance of threading defects such as dislocation, micropipes and the like during the traditional growth along <000-1> can be avoided, and the dislocation density is effectively reduced; meanwhile, the thickness of the crystal during transverse growth is determined by the height of the seed crystal column, so that the preparation efficiency of the crystal is greatly improved.
In order to enable the doped silicon carbide single crystal to uniformly grow around the seed column 6, when the seed column 6 is prepared, the crystal plane indexes of six equivalent planes of the seed column 6 are <1120> <11-20> <1120> <1-120> <1-1-20> respectively; or the six equivalent crystal planes of the seed crystal column 6 are <10-10> <01-10> < 1100> < 1010> <0-110> <1-100 respectively, but the crystal is not limited to the six equivalent crystal planes, and other hexagonal symmetric crystal planes can be used as long as the crystal growth conditions are met.
In one embodiment, the seed column 6 is a silicon carbide seed column, and the single crystal is a doped silicon carbide single crystal. Preferably, the doped silicon carbide single crystal is an α silicon carbide single crystal, which has a hexagonal crystal structure. A hexagonal crystal column is used as a seed crystal column 6 for crystal growth, and the surfaces of the seed crystal column 6 are six equivalent crystal planes <1120> <11-20> <1120> <1-120> <1-1-20> respectively. The silicon carbide single crystal block is polished to prepare a smooth crystal surface suitable for the gas phase growth of the silicon carbide single crystal, and the six crystal faces are used for replacing the flaky wafer seed crystal in the conventional PVT method. The seed crystal column 6 can be processed by a silicon carbide crystal bar, the side length of the seed crystal column 6 is 5-20mm, and the length is determined by the initial silicon carbide crystal bar.
In one embodiment, the crucible is a graphite crucible, the inner sidewall 8 is a porous graphite plate, the porosity of the inner sidewall 8 is 40% -60%, the pore diameter of the inner sidewall 8 is not higher than 1 μm, the porosity of the outer sidewall 2 is not higher than 10%, and the pore diameter of the outer sidewall 2 is not higher than 1 μm. The inner side wall 8 has a porosity greater than that of the outer side wall 2, so that the inner side wall 8 serves as a gas phase transmission passage after decomposition and sublimation of the raw material.
In one embodiment, the seed column 6 is formed by cutting and polishing a single crystal column, for example, the seed column 6 is formed by processing a silicon carbide crystal bar, the width of the side edge of the seed column 6 is 5-20mm, and the length is determined by the original silicon carbide crystal bar.
In order to arrange the seed crystal column 6 with any length, the seed crystal column 6 is arranged to be integrated or spliced along the axial direction of the seed crystal column 6. The splicing mode comprises the following steps: the seed crystal columns 6 can be directly stacked or the seed crystal columns 6 can be bonded.
In order to prepare a high-length silicon carbide seed crystal column, a plurality of seed crystal columns 6 can be spliced axially to lengthen the length of the seed crystal column 6, so that the thickness of the prepared doped silicon carbide single crystal is increased. For example, a plurality of identical silicon carbide seed columns 6 can be spliced together up and down, the spliced seed columns 6 are respectively connected and fixed with the hexagonal graphite hole clamping grooves in the center of the graphite cover body in the crucible through two ends of the uppermost and lowermost seed columns, and the height of the connected seed columns is the thickness of the silicon carbide crystal which can grow.
When the substrate is prepared by the single crystal, the substrate can be cut into a sheet-shaped single crystal substrate along the radial direction of the single crystal, and then the defect single crystal grown at the splicing part can be cut off; in order to improve the single crystal utilization rate, the cut defective single crystal may be used as a raw material for preparing the single crystal.
The length of the seed crystal column 6 in the crucible assembly determines the length of the prepared single crystal, and the seed crystal column 6 can be spliced in multiple sections, so that the thickness obtained by one-time growth is not less than 100mm, 120mm and 150mm, the axial length of the single crystal is not less than 100mm, 120mm and 150mm, and the length of the prepared single crystal is far greater than the length of the single crystal prepared by the traditional disc seed crystal fixed on the top of the crucible, namely 20-50 mm. The length of the single crystal produced by the crucible assembly is large, so that the number of substrates produced from the single crystal is large.
As an implementation mode, the crystal growth furnace comprises any one of the crucible assemblies, and further comprises a heating coil, a furnace body and a heat preservation structure; after the crucible assembly is sleeved with the heat insulation structure, the crucible assembly is placed in the furnace body, and the outer side wall 2 of the furnace body is surrounded by the induction coil. Preferably, the furnace body is a quartz furnace, and the induction coil is a medium-frequency induction coil. The crystal growth furnace heats the side wall of the crucible through a heating coil, and then heats sublimation gas A after sublimation of the raw material in the raw material cavity 4 to flow to each surface of the seed crystal column 6 to carry out crystal growth after passing through the inner side wall 8; preferably, the long crystal planes have the same plane index. The thickness of the single crystal prepared by the crystal growth furnace is large, and the number of substrates prepared by the single crystal is large. When the crystal growth furnace is used for preparing the doped silicon carbide single crystal, the preparation efficiency is high, the defect density of the prepared doped silicon carbide single crystal is low, and the technical foundation is laid for large-scale commercialization of the doped silicon carbide single crystal substrate.
When the doped silicon carbide single crystal is prepared, the outer side wall 2 of the graphite is inductively heated by the intermediate frequency coil, heat is transmitted to the raw material of the silicon carbide powder in the interlayer, and the heat further flows to the inner side wall 8 of the porous graphite and the seed crystal column 6. Because the outer side wall 2 of the crucible generates heat, a certain temperature gradient exists along the radial direction of the crucible, the growth rate of the doped silicon carbide single crystal is determined by the inner side wall 8, the seed crystal column 6 and the outer growth surface of the grown single crystal, and the initial radial temperature gradient, namely the temperature difference between the inner side wall 8 of the crucible and the surface of the seed crystal column 6, is controlled between 50 ℃ and 300 ℃. Due to the existence of the radial temperature gradient, the powder in the raw material cavity 4 is transmitted to the crystal face of the seed crystal column 6 along the radial temperature gradient for recrystallization after decomposition and sublimation, and the surface of the single crystal expands towards the inner side wall 8 along the radial temperature gradient, so that the doped silicon carbide single crystal with the required size is grown.
Controlling the growth temperature of the doped silicon carbide single crystal at 2000-23000 ℃, controlling the pressure at 5-50mbar, and introducing inert gas such as argon or helium as protective gas into the growth chamber; if a conductive N-type doped silicon carbide single crystal is prepared, nitrogen can be introduced into the inert gas in an amount determined according to the actual required resistivity as a gas phase dopant.
When the doped silicon carbide single crystal is produced, low resistance can be achieved by doping with at least one of a gas-phase dopant and a solid-phase dopant. As an embodiment, the doping is carried out simultaneously with the solid phase dopant phosphorus, a phosphorus compound or a mixture of phosphorus and a low resistivity silicon single crystal material and, the gas phase dopant nitrogen; by adjusting the nitrogen flow, doping in the crystal growth process after the nitrogen flow is introduced into a growth cavity in the crucible; the solid dopant is placed directly in the feedstock cavity, preferably mixed with the feedstock. The phosphorus-doped low-resistance silicon single crystal material is mixed with conventional SiC powder, so that the co-doping of silicon and phosphorus is realized, the doping is improved, and simultaneously, reaction substances are supplemented through the reaction of silicon and redundant carbon, and the quality of the doped silicon carbide single crystal is improved.
Due to doping silicon carbide single crystalOr micropipes, threading dislocation and other defects in the silicon carbide seed crystal column 6 [0001 ]]The direction, therefore, the transverse growth can avoid the inheritance of defects such as micropipes, dislocation and the like, thereby obtaining the silicon carbide crystal ingot with extremely low defect density; preferably, zero micropipes and screw dislocations below 100cm can be obtained-2And edge dislocation density of less than 220cm-2The defect density of the doped silicon carbide single crystal and the substrate is even close to zero.
Example 1
As a preparation method for preparing the doped silicon carbide single crystal by any one of the crucibles and the seed crystal column, the method comprises the following steps:
1) providing a crucible and a silicon carbide seed crystal column;
2) silicon carbide powder is filled into a raw material cavity formed by an interlayer on the side wall of the crucible, a silicon carbide seed crystal column is arranged in the crucible, and the silicon carbide seed crystal column is put into a crystal growth furnace after being assembled;
3) raising the temperature of the crystal growth furnace to 2000-2300 ℃, so that the sublimed gas after the raw material is sublimated passes through the inner side wall of the interlayer and is transmitted to the surface of the seed crystal column along the radial gas phase, and the temperature difference T between the inner surface of the inner side wall and the surface of the seed crystal is 50-300 ℃ for crystal growth, namely preparing the doped silicon carbide single crystal;
wherein the D1 position is 50-100mm, the D2 is 100-300mm, the seed crystal column is a hexagonal prism comprising six symmetrical equivalent planes, the width D3 of the equivalent crystal plane is 5-20mm, and the axial length of the seed crystal column is not less than 100 mm;
the raw materials are silicon carbide powder, dopant gas phase dopant nitrogen and solid phase dopant phosphorus P.
Example 2
The preparation method is described by taking the length of the seed column as an example of 150mm, and the doped silicon carbide single crystal # 1 to # 7 and the comparative doped silicon carbide single crystal # D1 to # D5 are prepared according to the method of example 1, except for the difference from the method of example 1 in Table 1.
TABLE 1
| Sample (I) | Temperature difference T/. degree.C | D1/mm | D2/mm | D3/mm |
| Doped silicon carbide single crystal 1# | 50 | 180 | 170 | 15 |
| Doped silicon carbide |
150 | 180 | 170 | 15 |
| Doped silicon carbide single crystal 3# | 300 | 180 | 170 | 15 |
| Doped silicon carbide |
150 | 160 | 170 | 15 |
| Doped silicon carbide single crystal 5# | 150 | 180 | 190 | 15 |
| Doped silicon carbide |
150 | 180 | 170 | 7 |
| Doped silicon carbide single crystal 7# | 150 | 180 | 220 | 15 |
| Contrast doped silicon carbide single crystal D1# | 150 | 320 | 170 | 15 |
| Contrast doped silicon carbide single crystal D2# | 150 | 180 | 280 | 15 |
| Contrast doped silicon carbide single crystal D3# | 150 | 180 | 170 | 15 |
| Contrast doped silicon carbide single crystal D4# | 150 | 180 | 170 | 3 |
| Contrast doped silicon carbide single crystal D5# | 330 | 180 | 170 | 15 |
The prepared doped silicon carbide single crystal 1# -7#, the comparative doped silicon carbide single crystal D1# -D5# micropipe of 6 inches was zero, screw dislocation (TSD) density, edge dislocation (TED) density and XRD characterization crystal quality and resistivity were tested, and the test results are shown in Table 2.
TABLE 2
From the above, when the radial temperature gradient, namely the lateral driving force, of the silicon carbide crystal growing laterally is large, the D1, namely the loading amount, is large, the D2, namely the transmission distance, is moderate, and the equivalent crystal plane of the seed crystal is long, the high-quality silicon carbide crystal with excellent crystallization quality and low dislocation density is easy to obtain. This is because the sufficient amount of material, the large lateral growth driving force and the appropriate transport distance help to maintain the C/Si ratio balance at the crystal growth interface, while the large size of the equivalent crystal plane avoids dislocations induced when the step flows of atoms of the polycrystalline planes are merged, thereby improving the crystal quality. The resistivity of the crystal is determined by the electroactive impurities introduced into the crystal and intrinsic defects in the crystal, and the higher flow of doping atmosphere and more solid-phase doping reactants introduced into the lattice position can obviously reduce the resistivity of the crystal and improve the conductivity of the crystal until the dissolution degree of the electroactive impurities in the crystal is reached. .
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (17)
1. A method for producing a doped silicon carbide single crystal, characterized by comprising the steps of:
1) providing a crucible and a seed crystal column;
2) putting a crystal growth raw material into a raw material cavity formed by an interlayer on the side wall of a crucible, installing a seed crystal column in the crucible, wherein the extension direction of the seed crystal column is approximately the same as the extension direction of the central axis of the crucible, forming a crystal growth cavity between the seed crystal column and the inner surface of the inner side wall of the interlayer, and putting the crystal growth cavity into a crystal growth furnace after assembling;
3) raising the temperature of the crystal growth furnace to ensure that the sublimated gas of the raw material after sublimation passes through the inner side wall of the interlayer and is transmitted to the surface of the seed crystal column along the radial gas phase for crystal growth, thus obtaining the doped silicon carbide single crystal;
wherein the raw materials comprise a silicon carbide raw material and,
the raw material also comprises a doping agent, and the doping agent comprises a solid phase doping agent contained in the raw material cavity and/or a gas phase doping agent filled into the crucible;
the silicon carbide seed crystal is arranged as a hexagonal system seed crystal, the doped silicon carbide single crystal is a hexagonal system single crystal, and the seed crystal column is arranged as a hexagonal prism comprising six equivalent crystal faces; the width of the equivalent crystal face is 5-20 mm; the seed crystal column is integrated or formed by splicing along the axial direction of the seed crystal column, the axial length of the seed crystal column is not less than 100mm, and the axial length of the single crystal is not less than 100 mm;
the six equivalent crystal planes of the seed column are <1120> <11-20> <1120> <1-120> <1-1-20> respectively, or the six equivalent crystal planes of the seed column are <10-10> <01-10> < 1100> <0-110> <1-100> respectively.
2. The preparation method according to claim 1, wherein the temperature difference between the inner surface of the inner side wall and the surface of the seed crystal column during the crystal growth is 50-300 ℃.
3. The method as claimed in claim 2, wherein the crystallization temperature is 2000-2300 ℃, and the crystallization pressure is 5-50 mbar.
4. The preparation method according to claim 1, wherein the solid phase dopant is at least one selected from the group consisting of elemental phosphorus, elemental germanium, elemental tin, elemental arsenic, phosphorus compounds, germanium compounds, tin compounds, and arsenic compounds, and/or the gas phase dopant is nitrogen.
5. The preparation method according to claim 4, wherein the solid phase dopant comprises low-resistance silicon single crystal powder.
6. The method of claim 1, wherein the crucible side wall comprises a sandwich layer comprising an inner side wall and an outer side wall, the inner side wall having a higher porosity than the outer side wall, the sandwich layer forming a feedstock cavity.
7. The method according to claim 6, wherein the interlayer is disposed at a height corresponding to that of the seed column, and the seed column and the crucible share a common central axis.
8. The method of claim 7, wherein the distance D1 between the inner and outer side walls is 50-300 mm.
9. The method as set forth in claim 7, wherein the distance D2 between the inner surface of the inner sidewall and the surface of the seed crystal column is 100-300 mm.
10. A crucible assembly characterized by comprising a crucible used in the production method according to any one of claims 1 to 9 and a seed column disposed in the crucible.
11. A silicon carbide seed column, comprising the seed column used in the production method according to any one of claims 1 to 9.
12. A doped silicon carbide single crystal produced by the method according to any one of claims 1 to 9, having an axial length of not less than 100mm and a density of threading dislocation defects of less than 100cm-2。
13. The doped silicon carbide single crystal of claim 12, wherein the doped silicon carbide single crystal has a resistivity of 10-20 Ω -m.
14. The doped silicon carbide single crystal of claim 12, wherein the concentration of nitrogen in the doped silicon carbide single crystal is 1018cm-3-1020cm-3The concentration of phosphorus in the doped silicon carbide single crystal is 1017cm-3％-1019cm-3(ii) a Or
The mass percentage of nitrogen in the doped silicon carbide single crystal is 1019cm-3-1020cm-3。
15. A doped silicon carbide single crystal substrate produced by cutting and polishing the doped silicon carbide single crystal according to claim 12, wherein the doped silicon carbide single crystal substrate is a silicon carbide single crystalThe density of threading dislocation defects of the substrate is less than 100cm-2。
16. The single crystal substrate according to claim 15, wherein the doped silicon carbide single crystal substrate has a resistivity of 10 to 20 Ω -m.
17. The single crystal substrate according to claim 15, wherein the concentration of nitrogen in the doped silicon carbide single crystal substrate is 1018cm-3-1020cm-3And the mass percentage of phosphorus in the doped silicon carbide single crystal substrate is 1017cm-3％-1019cm-3(ii) a Or
The mass percentage of nitrogen in the doped silicon carbide single crystal substrate is 1019cm-3-1020cm-3。
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| CN113186601B (en) * | 2021-04-30 | 2022-09-30 | 北京天科合达半导体股份有限公司 | High-quality silicon carbide seed crystal, silicon carbide substrate and preparation method thereof |
| EP4170073A4 (en) * | 2021-04-30 | 2024-04-17 | Tankeblue Semiconductor Co Ltd | High quality silicon carbide seed crystal, silicon carbide crystal, silicon carbide substrate, and preparation method therefor |
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