CN111074342B - Method for preparing carrier disc coating by utilizing silicon carbide epitaxial growth equipment - Google Patents
Method for preparing carrier disc coating by utilizing silicon carbide epitaxial growth equipment Download PDFInfo
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- CN111074342B CN111074342B CN201911379924.6A CN201911379924A CN111074342B CN 111074342 B CN111074342 B CN 111074342B CN 201911379924 A CN201911379924 A CN 201911379924A CN 111074342 B CN111074342 B CN 111074342B
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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
- C30B25/12—Substrate holders or susceptors
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
- C23C16/325—Silicon carbide
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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
Abstract
The invention provides a method for preparing a carrier disc coating by utilizing silicon carbide epitaxial growth equipment, which comprises the following steps: A. placing the graphite carrying disc into an epitaxial growth chamber of silicon carbide epitaxial growth equipment; B. heating the graphite carrying disc to a first preset temperature, keeping the pressure of the epitaxial growth chamber at the first preset pressure, and introducing a silicon source and a carbon source by taking hydrogen as a carrier gas to perform a chemical combination reaction on the graphite carrying disc and deposit to form a SiC coating; the first preset temperature is 1550-1750 ℃, and the first preset pressure is 150-250 torr; C. keeping introducing hydrogen and closing the silicon source and the carbon source, and reducing the temperature to a second preset temperature, wherein the second preset temperature is 600-800 ℃; D. repeat the step B, C a preset number of times; E. when the temperature is reduced to be lower than a second preset temperature, closing the hydrogen, and continuously reducing the temperature to be room temperature; F. and taking out the graphite carrying disc. The method can reduce the preparation cost of the coating and prolong the service life of the graphite carrying disc.
Description
Technical Field
The invention relates to the technical field of coating preparation, in particular to a method for preparing a carrier disc coating by utilizing silicon carbide epitaxial growth equipment.
Background
The silicon carbide epitaxial growth refers to that a single crystal layer which has certain requirements and is the same as the substrate crystal orientation is grown on a silicon carbide substrate as if the original crystal extends outwards by a section. There are various methods for growing epitaxial layers, and the most common method is a vapor phase epitaxy process, in which a substrate is placed in a reaction chamber and heated, and a silicon-containing reaction gas is introduced to perform a high temperature reaction, so that the silicon-containing reaction gas is reduced or thermally decomposed, and the generated silicon atoms are epitaxially grown on the surface of the substrate.
In a general silicon carbide epitaxial growth device, during the epitaxial growth process of SiC, a substrate slice is usually placed on a graphite carrying disc, and in order to improve the cleanliness of an epitaxial growth environment and avoid impurity elements from being separated out from the graphite carrying disc in a high-temperature environment, the graphite carrying disc needs to be covered by a coating.
The existing graphite carrying disc is generally coated with a TaC coating, although the existing graphite carrying disc has the advantages of high temperature resistance and stability, special coating preparation equipment is required to be used, and raw materials are expensive, so the preparation cost is high; in addition, the TaC coating and the graphite carrier plate are not firmly combined, and are easy to fall off in thermal cycle.
Therefore, if the SiC coating is used for replacing a TaC coating to be used as a surface coating on the graphite carrying disc, the SiC is also stable at high temperature and can be firmly combined with the graphite material, so that the SiC carrying disc can bear more thermal cycle times without cracking or falling off, and the service life of the graphite carrying disc can be prolonged; and the price of the raw materials for preparing the SiC coating is lower, so that the preparation cost can be reduced, and if the SiC coating can be prepared by using the existing silicon carbide epitaxial growth equipment, the cost can be further reduced.
Disclosure of Invention
In view of the shortcomings of the prior art, the invention aims to provide a method for preparing a carrier disc coating by using silicon carbide epitaxial growth equipment.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a carrier disk coating by utilizing silicon carbide epitaxial growth equipment comprises the following steps:
A. placing the graphite carrying disc into an epitaxial growth chamber of silicon carbide epitaxial growth equipment;
B. heating the graphite carrying disc to a first preset temperature, keeping the pressure of the epitaxial growth chamber at the first preset pressure, and introducing a silicon source and a carbon source by taking hydrogen as a carrier gas to perform a chemical combination reaction on the graphite carrying disc and deposit to form a SiC coating; the first preset temperature is 1550-1750 ℃, and the first preset pressure is 150-250 torr;
C. keeping introducing hydrogen and closing the silicon source and the carbon source, and reducing the temperature to a second preset temperature, wherein the second preset temperature is 600-800 ℃;
D. repeat the step B, C a preset number of times;
E. when the temperature is reduced to be lower than a second preset temperature, closing the hydrogen, and continuously reducing the temperature to be room temperature;
F. and taking out the graphite carrying disc.
In the method for preparing the coating of the carrier disc by using the silicon carbide epitaxial growth equipment, before the step A, the method further comprises the following steps:
A1. the upper surface of the graphite carrying disc is provided with a positioning groove for placing the substrate slice.
In the method for preparing the coating of the carrier disc by using the silicon carbide epitaxial growth equipment, the first preset temperature is 1650 ℃.
In the method for preparing the coating of the carrier disc by using the silicon carbide epitaxial growth equipment, the first preset pressure is 200 torr.
In the method for preparing the coating of the carrier disc by using the silicon carbide epitaxial growth equipment, the second preset temperature is 700 ℃.
In the method for preparing the carrier disc coating by using the silicon carbide epitaxial growth equipment, in the step D, the preset times are 2-3 times.
In the method for preparing the coating of the carrier disc by using the silicon carbide epitaxial growth equipment, the method further comprises the following steps before the step F:
F1. and D, turning the graphite carrying disc by 180 degrees, and repeating the steps B to E.
In the method for preparing the coating of the carrying disc by utilizing the silicon carbide epitaxial growth equipment, the graphite carrying disc 1 is rotated by 180 degrees around the central shaft after the graphite carrying disc is turned by 180 degrees and before the steps B to E are repeated
In the method for preparing the coating of the carrier disc by using the silicon carbide epitaxial growth equipment, the method further comprises the following steps after the step F:
G. raising the temperature of the epitaxial growth chamber to a third preset temperature again, keeping the pressure of the epitaxial growth chamber at a second preset pressure, introducing a cleaning gas by taking hydrogen as a carrier gas, and cleaning the growth chamber; the third preset temperature is 1550-1750 ℃, and the second preset pressure is 150-250 torr.
In the method for preparing the carrier plate coating by using the silicon carbide epitaxial growth equipment, the third preset temperature is 1650 ℃, the second preset pressure is 200 torr, and the cleaning gas comprises HCl gas.
Has the advantages that:
the method for preparing the coating of the carrier disc by using the silicon carbide epitaxial growth equipment has the following advantages:
1. the SiC coating is prepared on the graphite carrying disc to replace an expensive TaC coating, so that the preparation cost is reduced;
2. the existing silicon carbide epitaxial growth equipment is adopted to prepare the SiC coating on the graphite carrying disc, and special coating preparation equipment is not required to be additionally configured, so that the cost can be further reduced;
3. through multiple cycles of heating, covering and cooling, the firmness of the combination of the SiC coating and the graphite carrying disc can be greatly improved, and the service life of the graphite carrying disc is greatly prolonged.
Drawings
FIG. 1 is a flow chart of a method for preparing a carrier disk coating by using a silicon carbide epitaxial growth device provided by the invention.
FIG. 2 is a graph showing the temperature change of a graphite boat in the method for preparing a boat coating by using silicon carbide epitaxial growth equipment according to the present invention.
Fig. 3 is a schematic structural view of the silicon carbide epitaxial growth apparatus.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention. 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, features defined as "first", "second", may explicitly or implicitly include one or more of the described features. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The following disclosure provides embodiments or examples for implementing different configurations of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples, such repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or uses of other materials.
Referring to fig. 1-3, the present invention provides a method for preparing a boat coating using a silicon carbide epitaxial growth apparatus, comprising the steps of:
A. and putting the graphite carrying disc into an epitaxial growth chamber of silicon carbide epitaxial growth equipment.
As shown in FIG. 3, the silicon carbide epitaxial growth apparatus comprises an epitaxial growth chamber 2, a heat retaining plate 3, a heating plate 4, a reaction gas inlet means 5, and an exhaust gas discharge means 6. When preparing the SiC coating, the graphite carrier disc 1 is placed on a heating plate 4 of an epitaxial growth chamber, so that the heating plate heats the graphite carrier disc 1.
B. Heating the graphite carrying disc to a first preset temperature, keeping the pressure of the epitaxial growth chamber at the first preset pressure, and introducing a silicon source and a carbon source by taking hydrogen as a carrier gas to perform a chemical combination reaction on the graphite carrying disc and deposit to form a SiC coating; the first preset temperature is 1550-1750 ℃, and the first preset pressure is 150-250 torr.
Wherein, the silicon source is a silicon-containing gas which can be but not limited to silane, dichlorosilane, trichlorosilane, tetrachlorohydrogensilicon and the like; the carbon source is a carbon-containing gas, and may be, but is not limited to, methane, ethylene, acetylene, propane, and the like.
In some preferred embodiments, the first predetermined temperature is 1650 ℃ and the first predetermined pressure is 200 torr, which produces the best quality and longest service life of the SiC coating.
C. Keeping introducing hydrogen and closing the silicon source and the carbon source, and reducing the temperature to a second preset temperature, wherein the second preset temperature is 600-800 ℃.
D. The step B, C is repeated a preset number of times.
In the process, the temperature change of the graphite carrying disc 1 is shown in fig. 2, and the graphite carrying disc undergoes the processes of cyclic heating, high-temperature heat preservation and cooling; wherein the high-temperature heat preservation process is a process of depositing a single-layer SiC layer, the temperature is a first preset temperature T1, the duration time is T1, and hydrogen, a silicon source and a carbon source are continuously introduced in the process. t1 is preferably 90 min-110 min, the thickness of the formed single-layer SiC layer is moderate, and the quality of the obtained SiC coating is good.
Preferably, between the high temperature soak sections, when the temperature is decreased to the second predetermined temperature T2, the temperature is not immediately increased, but is maintained at the second predetermined temperature T2 for a duration T2, and the hydrogen gas is continuously introduced and the silicon source and the carbon source are turned off. After the monolayer deposition is finished, the graphite carrying disc 1 is shaped in the environment of the second preset temperature T2, and the bonding force between the coating and the graphite carrying disc 1 can be improved. t2 is preferably 90min to 110 min.
Generally, the predetermined number of times is 2 to 3 times.
In the process of circularly heating and cooling the graphite carrying disc 1, the SiC layer formed in advance can generate some fine cracks, and the cracks can be penetrated in the process of settling the next SiC layer, so that mutually penetrated parts are arranged among the SiC layers, and the firmness of the combination between the whole SiC coating and the graphite carrying disc can be greatly improved.
Preferably, the second preset temperature is 700 ℃, so that the formed fine cracks are enough, the width of the cracks is not too large, and the formed SiC coating is bonded with the graphite carrier disc most firmly.
E. And when the temperature is reduced to be lower than a second preset temperature, closing the hydrogen, and continuously reducing the temperature to the room temperature.
And after the deposition of the last SiC layer is finished, the silicon source and the carbon source are not heated and introduced, the hydrogen is closed when the temperature of the graphite carrying disc 1 is reduced to be lower than a second preset temperature, and then the temperature is continuously reduced until the temperature is reduced to the room temperature.
F. And taking out the graphite carrying disc.
In some embodiments, step a is preceded by the step of: A1. the upper surface of the graphite carrying disc 1 is provided with a positioning groove 1.1 for placing a substrate slice.
In fact, some silicon carbide epitaxial growth apparatuses are capable of holding only one graphite boat 1 with its bottom directly on the heating plate during operation (when silicon carbide is epitaxially grown on the substrate plate), as shown in fig. 3, and the bottom surface of the graphite boat 1 used in such silicon carbide epitaxial growth apparatuses is not coated with a SiC coating and does not affect the quality of the epitaxial layer on the substrate plate.
Still some silicon carbide epitaxial growth equipment can place multilayer graphite carrying disks 1 when working, the graphite carrying disks 1 are arranged at intervals in the height direction, and the bottom of the graphite carrying disk 1 is also contacted with reaction gas, so that the preparation of a SiC coating needs to be carried out on the bottom of the graphite carrying disk 1; for such a graphite boat 1, step F further comprises, before step F, the steps of: F1. and D, turning the graphite carrying disc by 180 degrees, and repeating the steps B to E. And C, turning the graphite carrying disc 1 to enable the bottom surface of the graphite carrying disc to face upwards, and repeating the steps B to E to form the SiC coating on the bottom surface of the graphite carrying disc 1.
Preferably, after the graphite carrying disc 1 is turned by 180 degrees and before the steps B to E are repeated, the graphite carrying disc 1 is rotated by 180 degrees around the central shaft, namely the front and back directions of the graphite carrying disc 1 are turned, so that the side which is positioned in the leeward direction before is turned to the windward direction; because the peripheral surface of the graphite carrying disc 1 is also required to be covered with the SiC coating, the SiC coating formed on the peripheral surface on the leeward side is thinner than that formed on the windward side, the front and back directions of the graphite carrying disc 1 are turned after the graphite carrying disc 1 is turned over, the original thinner coating can be effectively thickened, and the coating thickness on the peripheral surface is uniform.
Since the ready-made silicon carbide epitaxial growth equipment is adopted to prepare the SiC coating of the graphite carrying disc 1, the silicon carbide epitaxial growth equipment is required to be used for normal production and processing (namely, used for carrying out epitaxial growth on a substrate), and therefore an epitaxial growth chamber is required to be cleaned;
specifically, the method further comprises the following steps:
G. raising the temperature of the epitaxial growth chamber to a third preset temperature again, keeping the pressure of the epitaxial growth chamber at a second preset pressure, introducing a cleaning gas by taking hydrogen as a carrier gas, and cleaning the growth chamber; the third preset temperature is 1550-1750 ℃, and the second preset pressure is 150-250 torr.
In some preferred embodiments, the third predetermined temperature is 1650 ℃, the second predetermined pressure is 200 torr, and the purge gas comprises HCl gas.
From the above, the method for preparing the carrier disc coating by using the silicon carbide epitaxial growth equipment has the following advantages:
1. the SiC coating is prepared on the graphite carrying disc to replace an expensive TaC coating, so that the preparation cost is reduced;
2. the existing silicon carbide epitaxial growth equipment is adopted to prepare the SiC coating on the graphite carrying disc, and special coating preparation equipment is not required to be additionally configured, so that the cost can be further reduced;
3. through multiple cycles of heating, covering and cooling, the firmness of the combination of the SiC coating and the graphite carrying disc can be greatly improved, and the service life of the graphite carrying disc is greatly prolonged.
In summary, although the present invention has been described with reference to the preferred embodiments, the above-described preferred embodiments are not intended to limit the present invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention, which are substantially the same as the present invention.
Claims (8)
1. A method for preparing a carrier disc coating by utilizing silicon carbide epitaxial growth equipment is characterized by comprising the following steps:
A. placing the graphite carrying disc into an epitaxial growth chamber of silicon carbide epitaxial growth equipment;
B. heating the graphite carrying disc to a first preset temperature, keeping the temperature for 90-110 min, keeping the pressure of the epitaxial growth chamber at the first preset pressure, and introducing a silicon source and a carbon source by taking hydrogen as a carrier gas to perform a chemical combination reaction on the graphite carrying disc and deposit to form a SiC coating; the first preset temperature is 1650 ℃, and the first preset pressure is 150 to 250 torr;
C. keeping introducing hydrogen and closing the silicon source and the carbon source, reducing the temperature to a second preset temperature, and keeping the temperature for 90-110 min, wherein the second preset temperature is 600-800 ℃;
D. repeat the step B, C a preset number of times; the preset times are 2-3 times;
E. after the deposition of the last SiC layer is finished, a silicon source and a carbon source are not heated and introduced, hydrogen is closed when the temperature of the graphite carrying disc is reduced to be lower than a second preset temperature, and then the temperature is continuously reduced until the temperature is reduced to room temperature;
F. and taking out the graphite carrying disc.
2. The method for preparing a coating for a carrier disk by using an epitaxial growth apparatus for silicon carbide according to claim 1, further comprising, before step a, the steps of:
A1. the upper surface of the graphite carrying disc is provided with a positioning groove for placing the substrate slice.
3. The method for preparing a boat coating using silicon carbide epitaxial growth equipment as claimed in claim 1, wherein the first preset pressure is 200 torr.
4. The method for preparing a boat coating using a silicon carbide epitaxial growth apparatus as claimed in claim 1, wherein the second predetermined temperature is 700 ℃.
5. The method for preparing a coating for a carrier disk by using an apparatus for epitaxial growth of silicon carbide according to claim 1, further comprising the step of, before step F:
F1. and D, turning the graphite carrying disc by 180 degrees, and repeating the steps B to E.
6. A method for preparing a coating on a carrier disc using silicon carbide epitaxial growth apparatus as claimed in claim 5, wherein the graphite carrier disc is rotated 180 ° about the central axis after being turned 180 ° and before repeating steps B to E.
7. The method for preparing a coating for a carrier disk by using an apparatus for epitaxial growth of silicon carbide according to claim 1, further comprising the step of, after step F:
G. raising the temperature of the epitaxial growth chamber to a third preset temperature again, keeping the pressure of the epitaxial growth chamber at a second preset pressure, introducing a cleaning gas by taking hydrogen as a carrier gas, and cleaning the growth chamber; the third preset temperature is 1550-1750 ℃, and the second preset pressure is 150-250 torr.
8. The method for preparing a boat coating using silicon carbide epitaxial growth equipment as claimed in claim 7, wherein the third predetermined temperature is 1650 ℃, the second predetermined pressure is 200 torr, and the purge gas comprises HCl gas.
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| JPS56140021A (en) * | 1980-03-31 | 1981-11-02 | Mitsubishi Electric Corp | Manufacture of silicon carbide thin film |
| JPS6114726A (en) * | 1984-06-29 | 1986-01-22 | Fujitsu Ltd | Treatment of semiconductor substrate |
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