CN112374912A - Preparation method of graphite base with silicon carbide coating - Google Patents
Preparation method of graphite base with silicon carbide coating Download PDFInfo
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- CN112374912A CN112374912A CN202011267391.5A CN202011267391A CN112374912A CN 112374912 A CN112374912 A CN 112374912A CN 202011267391 A CN202011267391 A CN 202011267391A CN 112374912 A CN112374912 A CN 112374912A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 119
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 108
- 239000010439 graphite Substances 0.000 title claims abstract description 108
- 239000011248 coating agent Substances 0.000 title claims abstract description 48
- 238000000576 coating method Methods 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000011159 matrix material Substances 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 27
- 230000008021 deposition Effects 0.000 claims abstract description 26
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 20
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 15
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 15
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000004321 preservation Methods 0.000 claims abstract description 13
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 239000003085 diluting agent Substances 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 239000012159 carrier gas Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 239000012495 reaction gas Substances 0.000 abstract description 7
- 230000035939 shock Effects 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 58
- 238000000151 deposition Methods 0.000 description 28
- 238000005229 chemical vapour deposition Methods 0.000 description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
- C04B41/5059—Silicon carbide
Abstract
The invention discloses a preparation method of a graphite base with a silicon carbide coating, which comprises the following steps: pretreating the graphite base, and then placing the graphite base on a graphite shunt disk; performing CVR deposition: mixing high-purity Si powder and high-purity SiO2Mixing the powder, placing the powder in a vacuum furnace, carrying out vacuum-pumping treatment on the vacuum furnace, heating the vacuum furnace to 1850 and 2050 ℃ in an argon atmosphere, carrying out heat preservation reaction for 2-4h, and generating a SiC matrix layer on the surface of the graphite base; carrying out CVD deposition: reducing the furnace temperature of the vacuum furnace to 1050-3SiCl3‑H2An Ar reaction gas source system is adopted, the reaction is carried out for 10 to 30 hours in a heat preservation way, and an SiC outer layer is formed on the SiC matrix layer formed in the step S2; the silicon carbide coating obtained by the preparation method of the invention is tightly combined with the graphite base, and has no obvious layering, and the coating is high in purity and high in compactness, thereby improving the thermal shock resistance of the graphite base.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a preparation method of a silicon carbide coating graphite base.
Background
A Light Emitting Diode (LED) is a semiconductor Diode that converts electrical energy into Light energy. The LED light source has the characteristics of low energy consumption, strong applicability, strong stability, high reaction speed, environmental protection, no pollution and the like. With the continuous development of the current technology, LEDs have been widely applied in the fields of displays, tv lighting decoration, and illumination. One important process in the fabrication of LEDs is silicon epitaxy, in which a wafer is carried on a graphite susceptor. The performance and quality of the susceptor plays a crucial role in the quality of the epitaxial layers of the wafer. The silicon carbide coated graphite susceptor has unique advantages: high purity, compactness, uniformity and excellent thermal shock resistance and oxidation resistance, and improves the product quality and the process efficiency, thereby realizing the reduction of the whole operation cost. The preparation method of the silicon carbide coating graphite base is widely applied to Chemical Vapor Deposition (CVD) and Chemical Vapor Reaction (CVR).
The chemical vapor deposition method mainly adopts trichloromethylsilane (CH) at a certain deposition temperature3SiCl3MTS) as precursor, H2Ar is diluent gas and MTS is in gas form through oil temperature heating, and then carrier gas H is utilized through bubbling2The SiC outer layer is brought into a deposition furnace, is formed through a series of chemical reaction changes and is deposited on the surface of a graphite base, the deposition temperature is 1050-1200 ℃, the SiC outer layer prepared by the method is high in purity and good in density, the thickness of the coating is about 20 mu m, and the bonding strength of the generated SiC outer layer matrix is weak.
In the prior art, the published literature firstly utilizes silicon vapor and carbon on the surface of a graphite substrate to form an SiC outer layer, and then utilizes a CVD process to perform high-temperature cracking on the CVR silicon carbide coating to form the CVD silicon carbide coating, so that the bonding strength of the silicon carbide coating and the graphite substrate is improved. However, in the method, because the boiling point of silicon is high, the introduced silicon vapor is easy to condense into a silicon simple substance as reaction gas, so that certain impurities are doped in the generated coating to influence the performance of the coating, thereby influencing the use of the graphite base.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides the preparation method of the graphite base with the silicon carbide coating, the silicon carbide coating prepared by the method is tightly combined with the graphite base, obvious layering does not exist, and the coating is high in purity and high in compactness.
In order to achieve the above purpose, one of the purposes of the present invention is to provide a preparation method of a silicon carbide coating graphite base, which comprises the following specific scheme:
a preparation method of a silicon carbide coating graphite base comprises the following steps:
s1, pretreating the graphite base, and then placing the graphite base on a graphite shunt disk;
s2, performing CVR deposition: mixing Si powder and SiO2Mixing the powder, placing the powder in a vacuum furnace, carrying out vacuum-pumping treatment on the vacuum furnace, heating the vacuum furnace to 1850 and 2050 ℃ in an argon atmosphere, carrying out heat preservation reaction for 2-4h under micro-positive pressure, and generating a SiC substrate layer on the surface of the graphite base;
s3, carrying out CVD deposition: reducing the furnace temperature of the vacuum furnace to 1050-3SiCl3(MTS)-H2An Ar reaction gas source system, wherein MTS is carried and input by carrier gas hydrogen, the reaction is carried out for 10 to 30 hours under the condition of heat preservation, and an SiC outer layer is deposited on the SiC base body layer formed in the step S2; the SiC matrix layer is combined with the SiC outer layer to form a SiC coating; wherein the diluent gas is hydrogen or argon, H2The flow ratio of/MTS is 10; the hydrogen in the hydrogen to MTS flow ratio is the sum of the carrier hydrogen and the diluent hydrogen.
In some embodiments, in step S2, Si powder and SiO are mixed2The molar ratio of the powder is 1: 1; more preferably, in order to ensure SiO2The powder is completely reacted, and the mass ratio of Si powder is SiO2The mass of the powder is 5-10% more.
In some embodiments, the carrier gas hydrogen flow rate is 480ml/min and the dilution gas flow rate is 600 ml/min.
In some embodiments, in step S2, the temperature is raised to 1850-2050 ℃ at a rate of 10-15 ℃/min.
In some embodiments, the thickness of the SiC coating is ≧ 100 μm.
In some embodiments, in step S1, the step of pretreating the graphite susceptor is: and (3) polishing the surface of the graphite base, then placing the graphite base in alcohol, cleaning the graphite base for 20-40min by using ultrasonic waves, and finally drying the graphite base.
It is another object of the present invention to provide a silicon carbide coated graphite susceptor prepared by the method of any one of the above embodiments.
Compared with the prior art, the invention has the following beneficial effects:
the reaction principle of the invention is as follows: in step S2, Si powder and SiO2The powder reacts under the atmosphere of high temperature, micro positive pressure (300-; in addition, since the SiC base layer formed by the CVR reaction retains the porosity of the material, CH is introduced in step S33SiCl3-H2The SiC outer layer is formed on the formed SiC matrix layer through CVD deposition, in the CVD deposition process, the generated SiC can fill up the pores of the SiC matrix layer in the preparation of CVR reaction, and the defects of air holes, air bubbles and the like in the SiC matrix layer are almost not existed, so that on one hand, the structure of the SiC matrix layer can be more compact, and the SiC coating has high integral compactness and excellent performance; on the other hand, when the SiC outer layer is deposited, partial particles are filled in the pores of the SiC matrix layer, and a good bonding force is formed between the SiC matrix layer and the pores, so that the bonding force between the SiC coating and the graphite base is further enhanced.
Furthermore, by using the preparation method of the invention, the thickness of the SiC coating (comprising the SiC matrix layer and the SiC outer layer) can reach more than 100 μm, and the compactness is high, thereby further improving the thermal shock resistance of the coating.
Unlike the prior art which uses silicon vapor for deposition to prepare the coating, the invention uses Si powder and SiO powder under the atmosphere of high temperature, micro-positive pressure and argon gas2The powder is subjected to chemical reaction to generate SiO gas, the SiO gas is deposited on the surface of the graphite base and reacts with carbon to generate SiC and CO, and the SiC matrix layer generated on the surface of the graphite base has high component purity and cannot generate impurity Si when the SiC matrix layer is formed by deposition because CO is gas; and SiO reacts with carbon on the surface of the graphite base, so that the connection strength of the SiO and the carbon can be improved. In addition, when CVD deposition is carried out, the formed SiC partially fills the pores in the SiC matrix layer, so that the compactness of the SiC matrix layer is improved, and the SiC outer layer and the SiC matrix layer can have high bonding force.
The graphite base with the silicon carbide coating prepared by the preparation method has high coating purity and good compactness, the coating thickness can reach more than 100 mu m, and the coating and the graphite base are tightly combined without obvious layering.
Furthermore, the continuous high-temperature deposition furnace reaction equipment is adopted, and CVR reaction and CVD deposition do not need to be carried out in two equipment, so that the surface pollution of products is reduced, the production cost and time are saved, and the production efficiency is improved.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is an SEM image of a cross-section of a graphite susceptor with a silicon carbide coating formed in example 1 of the present invention;
FIG. 3 is an SEM image of the surface of a SiC coating layer formed in example 1 of the present invention.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Si powder and SiO powder used in the following examples2Powders of high purity Si and SiO, respectively2The purity of the powder is more than 99.99 percent.
Example 1
As shown in fig. 1, the present embodiment provides a method for preparing a graphite susceptor with a silicon carbide coating, which specifically includes the following steps:
s1, pretreatment of the graphite base: polishing the surface of a graphite base, then placing the graphite base in alcohol, cleaning the graphite base for 20-40min by using ultrasonic waves, and finally drying the graphite base in an oven at the temperature of 100 ℃ for 30 min; after the pretreatment is finished, placing the graphite base above a graphite gas distribution plate in a vacuum furnace;
s2, performing CVR deposition: mixing Si powder and SiO2Mixing the powders at a molar ratio of 1:1, placing at the bottom of a graphite crucible, and placing the graphite crucible in a vacuum furnace to prevent SiO2Residual powder, the mass of Si powder is 6% more; vacuumizing the vacuum furnace, introducing argon, heating to 1850 ℃ at the speed of 10-15 ℃/min in the argon atmosphere, then carrying out heat preservation reaction for 4 hours under micro-positive pressure, and depositing on the surface of the graphite base to form a SiC matrix layer;
s3, carrying out CVD deposition: reducing the temperature of a vacuum furnace to 1050 ℃, introducing a CH3SiCl3-H2-Ar reaction gas source system, carrying out heat preservation reaction for 20 hours, depositing a SiC matrix layer on the surface of the graphite base to generate a SiC outer layer, and combining the SiC matrix layer with the SiC outer layer to form a SiC coating; after the reaction is finished, cooling to room temperature in an argon atmosphere, and taking out a product; wherein H2The flow ratio of/MTS is 10, the flow rate of carrier gas hydrogen is 480ml/min, the flow rate of diluent gas is 600ml/min, and the flow rate of diluent gas is argon.
SEM analysis of the cross section of the resultant product (silicon carbide coated graphite susceptor) and SEM analysis of the surface of the resultant SiC outer layer, the results of the analyses being shown in fig. 2 and 3; in fig. 2, the dark portion is the graphite susceptor and the light portion is the SiC coating formed.
As shown in FIG. 2, the SiC coating formed by the method of the invention has high purity and good compactness, no delamination exists between the SiC base layer and the SiC outer layer formed by CVR and CVD deposition, and the combination between the SiC coating and the graphite base is good.
As can be seen from fig. 3, the SiC coating formed had a smooth and dense surface.
Compared with the prior art that the silicon steam is formed by adopting the simple substance of silicon under the conditions of low pressure and high temperature and reacts with the graphite base to generate the SiC coating, the invention does not need the condition of low pressure, and only needs to lead the Si powder and the SiO powder to react under the conditions of high temperature and slight positive pressure2The powder reacts to generate SiC gas, the SiC gas reacts with carbon on the surface of the graphite base to generate SiC and CO, and Si powder and SiO2The powder is firstly reacted, so that the generated SiC matrix layer can not be doped with Si impurities, the purity is high, the mechanical property is good, and the formed silicon carbide coating graphite base can not crack due to impurity doping when in use; in addition, the SiC matrix layer generated based on the CVR reaction retains the porosity of the material, so that the SiC part formed during CVD deposition fills the pores of the SiC matrix layer, on one hand, the tightness of the SiC matrix layer is higher, on the other hand, the binding force between the SiC outer layer and the SiC matrix layer is high, and the SiC coating formed by combining the SiC outer layer and the SiC matrix layer has a compact structure, high mechanical strength and good thermal shock resistance.
Example 2
As shown in fig. 1, the present embodiment provides a method for preparing a graphite susceptor with a silicon carbide coating, which specifically includes the following steps:
s1, pretreatment of the graphite base: polishing the surface of a graphite base, then placing the graphite base in alcohol, cleaning the graphite base for 20-40min by using ultrasonic waves, and finally drying the graphite base in an oven at the temperature of 100 ℃ for 30 min; after the pretreatment is finished, placing the graphite base above a graphite gas distribution plate in a vacuum furnace;
s2, performing CVR deposition: mixing Si powder and SiO2Mixing the powders at a molar ratio of 1:1, placing at the bottom of a graphite crucible, and placing the graphite crucible in a vacuum furnace to prevent SiO2Residual powder, the mass of Si powder is 5% more; pumping the vacuum furnaceIntroducing argon after vacuum treatment, heating to 1950 ℃ at the speed of 10-15 ℃/min in the argon atmosphere, then carrying out heat preservation reaction for 4 hours under slight positive pressure, and depositing on the surface of the graphite base to form a SiC matrix layer;
s3, carrying out CVD deposition: the temperature of the vacuum furnace is reduced to 1100 ℃, CH is introduced3SiCl3(MTS)-H2an-Ar reaction gas source system is subjected to heat preservation reaction for 20 hours, a SiC outer layer is generated on the SiC base layer on the surface of the graphite base in a deposition mode, and the SiC base layer and the SiC outer layer are combined to form a SiC coating; after the reaction is finished, cooling to room temperature in an argon atmosphere, and taking out a product; wherein H2The flow ratio of/MTS is 10, the flow rate of carrier gas hydrogen is 480ml/min, the flow rate of diluent gas is 600ml/min, and the flow rate of diluent gas is argon.
Example 3
As shown in fig. 1, the present embodiment provides a method for preparing a graphite susceptor with a silicon carbide coating, which specifically includes the following steps:
s1, pretreatment of the graphite base: polishing the surface of a graphite base, then placing the graphite base in alcohol, cleaning the graphite base for 20-40min by using ultrasonic waves, and finally drying the graphite base in an oven at the temperature of 100 ℃ for 30 min; after the pretreatment is finished, placing the graphite base above a graphite gas distribution plate in a vacuum furnace;
s2, performing CVR deposition: mixing Si powder and SiO2Mixing the powders at a molar ratio of 1:1, placing at the bottom of a graphite crucible, and placing the graphite crucible in a vacuum furnace to prevent SiO2Residual powder, the mass of Si powder is 10% more; vacuumizing the vacuum furnace, introducing argon, heating to 2050 ℃ at the speed of 10-15 ℃/min in the argon atmosphere, then carrying out heat preservation reaction for 2 hours under micro positive pressure, and depositing on the surface of the graphite base to form a SiC matrix layer;
s3, carrying out CVD deposition: the temperature of the vacuum furnace is reduced to 1200 ℃, CH is introduced3SiCl3-H2an-Ar reaction gas source system is subjected to heat preservation reaction for 15h, a SiC outer layer is deposited on the SiC base body layer on the surface of the graphite base, and the SiC base body layer and the SiC outer layer are combined to form a SiC coating; after the reaction is complete, CH is turned off3SiCl3Inputting gas and hydrogen, cooling to room temperature in argon atmosphere,taking out the product; wherein H2The flow ratio of/MTS is 10, the flow rate of carrier gas hydrogen is 480ml/min, the flow rate of diluent gas is 600ml/min, and the flow rate of diluent gas is argon.
Example 4
As shown in fig. 1, the present embodiment provides a method for preparing a graphite susceptor with a silicon carbide coating, which specifically includes the following steps:
s1, pretreatment of the graphite base: polishing the surface of a graphite base, then placing the graphite base in alcohol, cleaning the graphite base for 20-40min by using ultrasonic waves, and finally drying the graphite base in an oven at the temperature of 100 ℃ for 30 min; after the pretreatment is finished, placing the graphite base above a graphite gas distribution plate in a vacuum furnace;
s2, performing CVR deposition: mixing Si powder and SiO2Mixing the powders at a molar ratio of 1:1, placing at the bottom of a graphite crucible, and placing the graphite crucible in a vacuum furnace to prevent SiO2Residual powder, the mass of Si powder is 6% more; vacuumizing the vacuum furnace, introducing argon, heating to 1850 ℃ at the speed of 10-15 ℃/min in the argon atmosphere, then carrying out heat preservation reaction for 4 hours under micro-positive pressure, and depositing on the surface of the graphite base to form a SiC matrix layer;
s3, carrying out CVD deposition: reducing the temperature of the vacuum furnace to 1850 ℃, introducing a CH3SiCl3-H2-Ar reaction gas source system, carrying out heat preservation reaction for 25 hours, depositing a SiC matrix layer on the surface of the graphite base to generate a SiC outer layer, and combining the SiC matrix layer and the SiC outer layer to form a SiC coating; after the reaction is complete, CH is turned off3SiCl3Inputting gas and hydrogen, cooling to room temperature in an argon atmosphere, and taking out a product; wherein H2The flow ratio of/MTS is 10, the flow rate of carrier gas hydrogen is 480ml/min, the flow rate of diluent gas is 600ml/min, and the flow rate of diluent gas is argon.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. A preparation method of a silicon carbide coating graphite base is characterized by comprising the following steps:
s1, pretreating the graphite base, and then placing the graphite base on a graphite shunt disk;
s2, performing CVR deposition: mixing Si powder and SiO2Mixing the powder, placing the powder in a vacuum furnace, carrying out vacuum-pumping treatment on the vacuum furnace, heating the vacuum furnace to 1850 and 2050 ℃ in an argon atmosphere, carrying out heat preservation reaction for 2-4h under micro-positive pressure, and generating a SiC substrate layer on the surface of the graphite base;
s3, carrying out CVD deposition: reducing the furnace temperature of the vacuum furnace to 1050-2Ar, wherein MTS is carried and input by carrier gas hydrogen, and is subjected to reaction for 10 to 30 hours at the constant temperature, and a SiC outer layer is deposited on the SiC base layer formed in the step S2; the SiC matrix layer is combined with the SiC outer layer to form a SiC coating; wherein H2The flow ratio of/MTS is 10; the diluent gas is hydrogen and argon.
2. The method for preparing the silicon carbide coated graphite susceptor as claimed in claim 1, wherein in the step S2, Si powder and SiO are mixed2The molar ratio of the powders was 1: 1.
3. The method of preparing the silicon carbide coated graphite susceptor as set forth in claim 2, wherein the Si powder is SiO in mass ratio2The mass is 5-10% more.
4. The method of preparing a silicon carbide coated graphite susceptor as claimed in claim 1, wherein the carrier gas hydrogen flow rate is 480ml/min and the dilution gas flow rate is 600 ml/min.
5. The method as set forth in claim 1, wherein the temperature in step S2 is raised to 1850-2050 ℃ at a rate of 10-15 ℃/min.
6. The method for preparing the silicon carbide coated graphite susceptor as claimed in claim 1, wherein the thickness of the SiC coating is not less than 100 μm.
7. The method of preparing the silicon carbide coated graphite susceptor as claimed in claim 1, wherein the step of pretreating the graphite susceptor in the step S1 is: and (3) polishing the surface of the graphite base, then placing the graphite base in alcohol, cleaning the graphite base for 20-40min by using ultrasonic waves, and finally drying the graphite base.
8. A silicon carbide coated graphite susceptor prepared by the method of any one of claims 1 to 7.
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Cited By (4)
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| CN114368982A (en) * | 2022-01-21 | 2022-04-19 | 巩义市泛锐熠辉复合材料有限公司 | Silicon carbide coating graphite base and preparation method thereof |
| CN114525495A (en) * | 2022-01-05 | 2022-05-24 | 湖南德智新材料有限公司 | Preparation method and application of graphite tray with SiC coating on surface |
| CN115417678A (en) * | 2022-11-07 | 2022-12-02 | 湖南联合半导体科技有限公司 | Method for preparing SiC coating by low-temperature chemical vapor reaction method |
| CN115959669A (en) * | 2023-01-30 | 2023-04-14 | 武汉理工大学 | Preparation method of SiC nano powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114525495A (en) * | 2022-01-05 | 2022-05-24 | 湖南德智新材料有限公司 | Preparation method and application of graphite tray with SiC coating on surface |
| CN114525495B (en) * | 2022-01-05 | 2024-03-15 | 湖南德智新材料有限公司 | Preparation method and application of graphite tray with surface SiC coating |
| CN114368982A (en) * | 2022-01-21 | 2022-04-19 | 巩义市泛锐熠辉复合材料有限公司 | Silicon carbide coating graphite base and preparation method thereof |
| CN115417678A (en) * | 2022-11-07 | 2022-12-02 | 湖南联合半导体科技有限公司 | Method for preparing SiC coating by low-temperature chemical vapor reaction method |
| CN115959669A (en) * | 2023-01-30 | 2023-04-14 | 武汉理工大学 | Preparation method of SiC nano powder |
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