CN113622030A - Method for preparing silicon carbide single crystal - Google Patents
Method for preparing silicon carbide single crystal Download PDFInfo
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- CN113622030A CN113622030A CN202110947038.XA CN202110947038A CN113622030A CN 113622030 A CN113622030 A CN 113622030A CN 202110947038 A CN202110947038 A CN 202110947038A CN 113622030 A CN113622030 A CN 113622030A
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- silicon carbide
- single crystal
- carbide single
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- epitaxial layer
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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
- C30B23/02—Epitaxial-layer growth
- C30B23/025—Epitaxial-layer growth characterised by the substrate
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
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- Metallurgy (AREA)
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Abstract
The invention relates to the technical field of semiconductors, in particular to a preparation method of a silicon carbide single crystal; the preparation method of the silicon carbide single crystal comprises the steps of providing a silicon substrate, wherein the size of the silicon substrate is 8-12 inches; epitaxially growing a layer of silicon carbide on a silicon substrate; stripping the silicon substrate to obtain a silicon carbide epitaxial layer; and (3) carrying out silicon carbide single crystal growth on the silicon carbide epitaxial layer by using a physical vapor transport method. The method for producing a silicon carbide single crystal of the present invention facilitates the production of a silicon carbide single crystal having a size of 8 to 12 inches.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a preparation method of a silicon carbide single crystal.
Background
Silicon carbide semiconductor materials have achieved a great stride over a wide variety of applications over a long period of technological development. The silicon carbide material has the characteristics of large forbidden band width, high thermal conductivity, high carrier saturation mobility and the like, so that the silicon carbide material can be applied to the aspects of high temperature, high frequency, high power, microelectronic devices and the like. With the continuous improvement in diameter and quality of silicon carbide substrates, the range of application of silicon carbide single crystal substrates is also expanding. A commonly used method for growing a silicon carbide single crystal in the related art is a physical vapor transport method (PVT), which requires a silicon carbide seed crystal as a growth carrier, and the diameter of the seed crystal determines the diameter of the silicon carbide single crystal that can be finally obtained.
However, the method for producing a silicon carbide single crystal provided by the related art has difficulty in obtaining a silicon carbide single crystal having a size of 8 to 12 inches.
Disclosure of Invention
An object of the present invention is to provide a method for producing a silicon carbide single crystal which facilitates the production of a silicon carbide single crystal having a size of 8 to 12 inches.
Embodiments of the invention may be implemented as follows:
in a first aspect, the present invention provides a method for producing a silicon carbide single crystal, comprising:
providing a silicon substrate, wherein the size of the silicon substrate is 8-12 inches;
epitaxially growing a layer of silicon carbide on a silicon substrate;
stripping the silicon substrate to obtain a silicon carbide epitaxial layer;
and (3) carrying out silicon carbide single crystal growth on the silicon carbide epitaxial layer by using a physical vapor transport method.
In an alternative embodiment, a layer of silicon carbide is epitaxially grown on a silicon substrate using a chemical vapor transport process using methane and silane as the gas sources.
In an alternative embodiment, the silicon carbide epitaxial layer has a thickness greater than or equal to 100 μm, for example, between 100 μm and 1000 μm.
In an alternative embodiment, the method of peeling the silicon substrate includes a laser lift-off method.
In an alternative embodiment, the silicon carbide epitaxial layer is subjected to silicon carbide single crystal growth by a physical vapor transport method in a high-temperature thermal field with the temperature of 2000-2300 ℃.
In an alternative embodiment, the physical vapor transport process is carried out in a graphite crucible.
In an optional embodiment, the graphite crucible comprises a graphite crucible cover, a graphite crucible barrel and a guide cylinder arranged between the graphite crucible barrel and the graphite crucible cover, the guide cylinder is communicated with the graphite crucible barrel, and the graphite crucible cover covers the guide cylinder; the physical vapor phase transmission method by using the graphite crucible comprises the step of arranging a silicon carbide epitaxial layer on a graphite crucible cover, wherein the silicon carbide epitaxial layer is provided with a first surface which is in contact with a silicon substrate and is stripped from the silicon substrate and a second surface which is deviated from the first surface, and the second surface of the silicon carbide epitaxial layer faces to an inner cavity of the guide cylinder.
In an alternative embodiment, the guide cylinder is a constant diameter graphite cylinder.
In an alternative embodiment, the silicon substrate is 8 inches in size.
In an alternative embodiment, the silicon substrate is 12 inches in size.
The embodiment of the invention has the beneficial effects that:
the preparation method of the silicon carbide single crystal provided by the embodiment of the invention comprises the following steps: providing a silicon substrate, wherein the size of the silicon substrate is 8-12 inches; epitaxially growing a layer of silicon carbide on a silicon substrate; stripping the silicon substrate to obtain a silicon carbide epitaxial layer; and (3) carrying out silicon carbide single crystal growth on the silicon carbide epitaxial layer by using a physical vapor transport method. Thus, the silicon carbide epitaxial layer after the silicon substrate is stripped is used as a silicon carbide seed crystal, and the silicon carbide single crystal is grown by a physical vapor transport method to prepare the silicon carbide single crystal, the size of the prepared silicon carbide epitaxial layer is 8-12 inches because the size of the silicon substrate for preparing the silicon carbide epitaxial layer is 8-12 inches, and the silicon carbide single crystal with the size of 8-12 inches is correspondingly grown by the physical vapor transport method to prepare the silicon carbide single crystal with the size of 8-12 inches.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic structural view of an expanding device according to the related art;
fig. 2 is a schematic structural view of another expanding device provided in the related art;
FIG. 3 is a process flow chart of the method for producing a silicon carbide single crystal of the present invention.
Icon: 1-a graphite crucible cover; 2-silicon carbide seed crystal; 3-a graphite crucible barrel; 4-silicon carbide powder; 5-continuously expanding the guide shell; 6-expanding the guide shell in the early stage; 10-a graphite crucible; 11-a guide shell; 12-a silicon substrate; 13-epitaxial layer of silicon carbide.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that if the terms "inside", "outside", etc. indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings or the orientation or positional relationship which is usually placed when the product of the present invention is used, the description is merely for convenience of describing the present invention and simplifying the description, but the indication or suggestion that the referred device or element must have a specific orientation, be constructed in a specific orientation and operation, and thus, cannot be understood as the limitation of the present invention.
It should be noted that the features of the embodiments of the present invention may be combined with each other without conflict.
The Physical Vapor Transport (PVT) method provided by the related art generally obtains 8-12 inches of silicon carbide single crystals by a method of iteratively enlarging the diameter. The specific method is that firstly, a commercially available 6-inch silicon carbide single crystal substrate is used as a seed crystal, and then the silicon carbide single crystal with large diameter is obtained through expanding growth; the silicon carbide single crystal after diameter expansion can be used as a new seed crystal, diameter expansion growth is continuously carried out on the basis of the diameter of the seed crystal, and the diameter size of the silicon carbide single crystal can be expanded step by repeating the cycle iteration until the silicon carbide single crystal of 8 inches or 12 inches is obtained. The related art provides an expanding device as shown in fig. 1, which comprises a graphite crucible cover 1, a silicon carbide seed crystal 2 adhered to the crucible cover, a graphite crucible barrel 3, a silicon carbide powder 4 and a continuous expanding guide cylinder 5, or as shown in fig. 2, which comprises a graphite crucible cover 1, a silicon carbide seed crystal 2 adhered to the crucible cover, a graphite crucible barrel 3, a silicon carbide powder 4 and an early expanding guide cylinder 6. Two sets of expanding devices shown in fig. 1 and 2 have main expanding parts of a continuous expanding guide cylinder 5 and an early expanding guide cylinder 6 respectively; however, the inner diameter of the guide cylinder 5 is gradually increased, but the expansion angle is not necessarily too large in order to ensure good crystal quality, and an expansion angle of 10 ° or less is generally selected. The diameter expansion angle of the earlier diameter expansion guide cylinder 6 can be larger than that of the continuous diameter expansion guide cylinder 5, generally, the diameter expansion angle within 45 degrees is selected, the earlier diameter expansion guide cylinder 6 can quickly expand in the early growth stage, and then the equal-diameter growth is maintained. The two iterative expanding modes can expand the diameter by 5-6 mm every time of single crystal growth, if the diameter is expanded from 6 inches to 8 inches, at least 10 heats of single crystal growth are needed, the size of the guide shell needs to be changed continuously in the period, at least 5-6 guide shells with different initial inner diameters are needed, and the whole expanding time course is expected to require 5 months to half a year. However, if the diameter of the silicon carbide single crystal is expanded from 6 inches to 12 inches, the time is longer, and more guide cylinders with different inner diameters are replaced, so that the preparation of the silicon carbide single crystal of 8 to 12 inches is difficult, and the preparation period is too long.
The invention provides a method for preparing a silicon carbide single crystal, which is convenient for preparing the silicon carbide single crystal with the size of 8-12 inches.
Referring to fig. 3, the method for producing a silicon carbide single crystal of the present invention includes: providing a silicon substrate, wherein the size of the silicon substrate is 8-12 inches; epitaxially growing a layer of silicon carbide on a silicon substrate; stripping the silicon substrate to obtain a silicon carbide epitaxial layer; and (3) carrying out silicon carbide single crystal growth on the silicon carbide epitaxial layer by using a physical vapor transport method.
Since the silicon substrate 12 for preparing the silicon carbide epitaxial layer 13 has a size of 8-12 inches, the prepared silicon carbide epitaxial layer 13 has a size of 8-12 inches, and accordingly, the silicon carbide single crystal with a size of 8-12 inches can be conveniently prepared by growing the silicon carbide single crystal on the silicon carbide epitaxial layer 13 with a physical vapor transport method, wherein the silicon carbide single crystal with a size of 8-12 inches is prepared.
The method directly prepares the silicon carbide epitaxial layer 13 of 8-12 inches as the silicon carbide seed crystal, and further can directly prepare the silicon carbide seed crystal of 8-12 inches into the silicon carbide single crystal of 8-12 inches by a physical vapor transport method, does not need iterative expanding any more, effectively shortens the time for preparing the silicon carbide single crystal, also reduces the procedure of replacing guide cylinders with different inner diameters, and has the advantages of simple preparation method, easy operation, time saving and labor saving.
It should be noted that the silicon substrate 12 having a size of 8 to 12 inches is readily available and has good operability for growing the silicon carbide epitaxial layer 13.
In the present invention, a layer of silicon carbide is epitaxially grown on a silicon substrate 12 by a chemical vapor transport method, and the gas source is methane and silane.
Further, the thickness of the silicon carbide epitaxial layer 13 is 100 μm or more, for example, 100 μm to 1000 μm.
The lift-off method of the silicon substrate 12 includes, but is not limited to, a laser lift-off method. The silicon carbide epitaxial layer 13 left after the silicon substrate 12 is peeled off can be used as a silicon carbide seed crystal.
And (3) carrying out physical vapor transport on the prepared silicon carbide epitaxial layer 13 serving as the silicon carbide seed crystal in a graphite crucible to prepare the silicon carbide single crystal.
When the silicon carbide single crystal growth is carried out by using a physical vapor transport method, a silicon carbide epitaxial layer 13 as a silicon carbide seed crystal is arranged on the graphite crucible cover 1, and specifically, the silicon carbide epitaxial layer 13 is pasted on the graphite crucible cover 1; arranging the graphite crucible cover 1 at one end of the guide cylinder 11 far away from the graphite crucible barrel 3, and enabling the silicon carbide epitaxial layer 13 to face the inner cavity of the guide cylinder 11; the graphite crucible barrel 3 is filled with silicon carbide powder.
Further, the silicon carbide epitaxial layer has a first face and a second face that deviates from the first face after contacting with the silicon substrate and peeling off the silicon substrate, and the second face of silicon carbide epitaxial layer is towards the inner chamber of draft tube 11.
Further, the silicon carbide epitaxial layer 13 is subjected to silicon carbide single crystal growth by a physical vapor transport method in a high-temperature thermal field at a temperature of 2000-.
The method for producing a silicon carbide single crystal of the present invention will be described in detail below with reference to specific examples.
Example 1
A layer of silicon carbide is epitaxially grown on an 8-inch silicon substrate by chemical vapor transport using methane and silane as gas sources, and the thickness of the epitaxial layer is 100 μm.
And completely stripping the silicon substrate from the silicon carbide epitaxial layer by using a laser stripping technology. The silicon carbide epitaxial layer remaining after the stripping was an 8 inch silicon carbide seed.
One surface of the 8-inch silicon carbide seed crystal after being stripped from the silicon substrate is bonded with a graphite crucible cover, and the graphite crucible cover bonded with the silicon carbide seed crystal is arranged on the guide cylinder, so that the silicon carbide seed crystal is opposite to the silicon carbide powder in the graphite crucible barrel; the silicon carbide single crystal was grown in a high-temperature thermal field at a temperature of 2000 c to produce a silicon carbide single crystal having a size of 8 inches.
Example 2
A layer of silicon carbide was epitaxially grown by chemical vapor transport on a 12 inch silicon substrate from methane and silane as gas sources and the thickness of the epitaxial layer was 120 μm.
And completely stripping the silicon substrate from the silicon carbide epitaxial layer by using a laser stripping technology. The silicon carbide epitaxial layer remaining after the stripping was a 12 inch silicon carbide seed.
One surface of the 12-inch silicon carbide seed crystal after being stripped from the silicon substrate is bonded with a graphite crucible cover, and the graphite crucible cover bonded with the silicon carbide seed crystal is arranged on the guide cylinder, so that the silicon carbide seed crystal is opposite to the silicon carbide powder in the graphite crucible barrel; the silicon carbide single crystal was grown in a high-temperature thermal field at a temperature of 2300 c to produce a silicon carbide single crystal having a size of 12 inches.
Example 3
A layer of silicon carbide was epitaxially grown by chemical vapor transport on a 9 inch silicon substrate from methane and silane as gas sources and the thickness of the epitaxial layer was 110 μm.
And completely stripping the silicon substrate from the silicon carbide epitaxial layer. The silicon carbide epitaxial layer remaining after the lift-off was a 9 inch silicon carbide seed.
Bonding one surface of the 9-inch silicon carbide seed crystal stripped from the silicon substrate with a graphite crucible cover, and arranging the graphite crucible cover bonded with the silicon carbide seed crystal on a guide cylinder so that the silicon carbide seed crystal is opposite to the silicon carbide powder in the graphite crucible barrel; the silicon carbide single crystal was grown in a high-temperature thermal field at a temperature of 2200 c to produce a silicon carbide single crystal having a size of 9 inches.
In conclusion, the method for preparing the silicon carbide single crystal of the present invention facilitates the preparation of silicon carbide single crystals having a size of 8 to 12 inches.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for producing a silicon carbide single crystal, comprising:
providing a silicon substrate, wherein the size of the silicon substrate is 8-12 inches;
epitaxially growing a layer of silicon carbide on the silicon substrate;
stripping the silicon substrate to obtain a silicon carbide epitaxial layer;
and carrying out silicon carbide single crystal growth on the silicon carbide epitaxial layer by using a physical vapor transport method.
2. A method for producing a silicon carbide single crystal according to claim 1, wherein a layer of the silicon carbide is epitaxially grown on the silicon substrate by a chemical vapor transport method using a gas source of methane and silane.
3. A method for producing a silicon carbide single crystal according to claim 1, wherein the thickness of the silicon carbide epitaxial layer is 100 to 1000 μm.
4. A method for producing a silicon carbide single crystal according to claim 1, characterized in that the method of peeling the silicon substrate is a laser peeling method.
5. A method for producing a silicon carbide single crystal as defined in claim 1, wherein the silicon carbide single crystal growth is carried out on the silicon carbide epitaxial layer by the physical vapor transport method in a high-temperature thermal field at a temperature of 2000-2300 ℃.
6. A method for producing a silicon carbide single crystal according to claim 1, characterized in that the physical vapor transport method is performed in a graphite crucible.
7. The method for producing a silicon carbide single crystal according to claim 6, wherein the graphite crucible comprises a graphite crucible cover, a graphite crucible barrel, and a draft tube provided between the graphite crucible barrel and the graphite crucible cover, the draft tube being in communication with the graphite crucible barrel, the graphite crucible cover being fitted over the draft tube; the step of carrying out the physical vapor transport method by using the graphite crucible comprises the step of arranging the silicon carbide epitaxial layer on the graphite crucible cover, wherein the silicon carbide epitaxial layer is provided with a first surface which is in contact with the silicon substrate and is stripped from the silicon substrate and a second surface which is deviated from the first surface, and the second surface of the silicon carbide epitaxial layer faces the inner cavity of the guide shell.
8. A method for producing a silicon carbide single crystal according to claim 7, wherein the guide cylinder is a constant diameter graphite cylinder.
9. A method for producing a silicon carbide single crystal according to claim 1, wherein the silicon substrate has a size of 8 inches.
10. A method for producing a silicon carbide single crystal according to claim 1, wherein the silicon substrate has a size of 12 inches.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115595671A (en) * | 2022-12-12 | 2023-01-13 | 青禾晶元（天津）半导体材料有限公司（Cn） | Preparation method of composite substrate |
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| CN113622030B (en) | 2022-08-26 |
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