CN116730744A - Graphite component for epitaxial growth of silicon carbide and preparation process of composite coating thereof - Google Patents
Graphite component for epitaxial growth of silicon carbide and preparation process of composite coating thereof Download PDFInfo
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- CN116730744A CN116730744A CN202310629660.5A CN202310629660A CN116730744A CN 116730744 A CN116730744 A CN 116730744A CN 202310629660 A CN202310629660 A CN 202310629660A CN 116730744 A CN116730744 A CN 116730744A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 238000000576 coating method Methods 0.000 title claims abstract description 111
- 239000011248 coating agent Substances 0.000 title claims abstract description 108
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 60
- 239000010439 graphite Substances 0.000 title claims abstract description 60
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 50
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 26
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 26
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 25
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000002491 polymer binding agent Substances 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 229920005596 polymer binder Polymers 0.000 claims abstract description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims description 20
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 229920000728 polyester Polymers 0.000 claims description 10
- 239000007767 bonding agent Substances 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000004642 Polyimide Substances 0.000 claims description 5
- 229920001721 polyimide Polymers 0.000 claims description 5
- 230000003746 surface roughness Effects 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 15
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- XUIMIQQOPSSXEZ-NJFSPNSNSA-N silicon-30 atom Chemical compound [30Si] XUIMIQQOPSSXEZ-NJFSPNSNSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- 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
- C04B41/5001—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 with carbon or carbonisable materials
-
- 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
- C04B41/80—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
-
- 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
- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/06—Reaction chambers; Boats for supporting the melt; Substrate holders
- C30B19/067—Boots or containers
Abstract
The invention relates to the technical field of epitaxial growth of silicon carbide, in particular to a graphite component for epitaxial growth of silicon carbide and a preparation process of a composite coating thereof, which comprises the following steps: firstly, preheating a graphite component in a high-purity nitrogen environment according to the mass ratio of 5% -10%; secondly, coating the graphite component subjected to preheating treatment with a coating raw material, wherein the coating raw material comprises 30-40% of carbon nanotubes, 20-30% of graphene, 10-20% of nano silicon carbide and 20-30% of high polymer binder in percentage by mass; and finally, carrying out heat treatment on the coated graphite part in a nitrogen environment to obtain the composite coating. The invention can realize the efficient combination of the graphite component and the composite coating, prolongs the service life of the graphite component, has simple operation and high efficiency, and is easy to realize industrial production.
Description
Technical Field
The invention relates to the technical field of epitaxial growth of silicon carbide, in particular to a graphite component for epitaxial growth of silicon carbide and a preparation process of a composite coating thereof.
Background
Silicon carbide (SiC) has been widely used in the fields of power electronics, optoelectronics, and microelectronics because of its excellent physicochemical properties such as high thermal conductivity, high electron mobility, large band gap, high thermal stability, chemical stability, etc., however, since SiC has a large difference in lattice and thermal expansion coefficient from other materials, it is difficult to grow SiC thin films on other materials by epitaxial growth methods, and thus new growth methods and growth apparatuses have been required to be developed.
In the conventional SiC epitaxial growth method, the growth is generally performed in a graphite crucible by Chemical Vapor Deposition (CVD) in a high-temperature environment, however, due to the high chemical activity of graphite, the graphite is easy to react with SiC in a high-temperature condition, so that the surface roughness and microstructure quality of the SiC film are difficult to ensure, and in order to solve the problem, some researchers try to coat a protective layer on the inner surface of the graphite crucible to prevent the reaction of graphite with SiC. However, this method has problems such as uneven thickness of the protective layer and easy falling off.
Therefore, a novel epitaxial growth method capable of effectively protecting a graphite crucible from reacting with SiC and improving the surface quality of a SiC film is needed to be developed, and the invention is provided under such a background, and the main purpose of the invention is to provide a novel graphite component for epitaxial growth of silicon carbide and a preparation process of a composite coating thereof, which can solve the problems.
Disclosure of Invention
Based on the above purpose, the invention provides a graphite component for epitaxial growth of silicon carbide and a preparation process of a composite coating thereof.
A graphite component for epitaxial growth of silicon carbide and a preparation process of a composite coating thereof comprise the following steps:
step one: firstly, preheating a graphite component in a high-purity nitrogen environment according to the mass ratio of 5% -10%;
step two: coating a graphite component subjected to preheating treatment with a coating raw material, wherein the coating raw material comprises, by mass, 30% -40% of carbon nanotubes, 20% -30% of graphene, 10% -20% of nano silicon carbide and 20% -30% of a high-molecular bonding agent;
step three: and carrying out heat treatment on the coated graphite component in a nitrogen environment to obtain the composite coating.
Further, the temperature range of the preheating treatment is 200-500 ℃ and the duration time is 1-3 hours.
Further, the preparation method of the coating raw material comprises the following specific steps:
preparing materials: preparing a required carbon nano tube, graphene, nano silicon carbide and a high polymer binding agent, wherein the mass ratio of the raw materials is as follows: 30-40% of carbon nano tube, 20-30% of graphene, 10-20% of nano silicon carbide and 20-30% of high polymer binder.
Mixing materials: the raw materials are placed into a mixer for mixing, and the mixing time is required to ensure that all the raw materials can be uniformly distributed.
Ultrasonic treatment: and carrying out ultrasonic treatment on the mixed coating raw materials for 30-60 minutes, wherein the ultrasonic treatment can further promote the uniform mixing of the raw materials. And simultaneously, the adhesive property of the coating raw material is enhanced, so that the coating is more uniform and firmer.
The preparation of the coating raw materials is completed: after the ultrasonic treatment is completed, a coating raw material for coating the graphite member is obtained.
Further, the coating step includes a spraying method, the coating thickness ranges from 100 to 500 μm, the coating speed ranges from 5 to 10 mm/s, and the distance between the graphite member and the nozzle is maintained at 10 to 20 cm during the above-mentioned coating process.
Further, the temperature of the heat treatment is 800-1200 ℃ and the duration is 2-4 hours, and the rising and falling speed of the temperature is kept 2-5 ℃/min during the heat treatment.
Further, the graphite component comprises a graphite crucible, wherein the volume of the graphite crucible ranges from 500 cubic centimeters to 2000 cubic centimeters, and the surface roughness of the graphite crucible ranges from 0.2 micrometers to 0.5 micrometers.
Further, the high polymer binder comprises polyester, polyester ketone and polyimide, and the curing condition of the high polymer binder is that the temperature is 80-120 ℃ and the time is 1-2 hours.
Further, the nitrogen atmosphere is a high purity nitrogen atmosphere of 99.99% and the flow rate of nitrogen is in the range of 5-10 liters/min, and such nitrogen atmosphere is maintained during the whole coating and heat treatment process to avoid the influence of oxygen and water vapor.
Further, the carbon nanotubes, the graphene and the nano silicon carbide have the size ranges of 10-20 nanometers, 1-5 layers and 10-50 nanometers respectively, the length range of the carbon nanotubes is 0.5-2 micrometers, the lattice constant of the graphene is 0.142-0.146 nanometers, and the lattice constant of the nano silicon carbide is 0.43-0.44 nanometers.
The invention has the following beneficial effects:
1. according to the invention, through special raw material composition and fine process parameter adjustment, an effective method for preparing the composite coating of the graphite component for epitaxial growth of the silicon carbide is provided, the coating has excellent hardness, oxidation resistance, thermal stability and adhesion, the requirements of high-temperature stability and oxidation resistance in the epitaxial growth process of the silicon carbide are met, and the service life of the graphite component is further prolonged.
2. According to the invention, the quality proportion of the coating raw materials is adjusted, so that the performance of the coating can be optimized according to actual requirements, and the coating has high flexibility and wide applicability, for example, when a coating with higher hardness is required, the proportion of the carbon nano tube can be increased; when better oxidation resistance is desired, the ratio of nano silicon carbide can be increased.
3. The invention has the advantages of simple process flow and easy mass production by using commonly and easily available raw materials, and particularly has the advantages of simple operation, high efficiency and easy realization of industrial production by adopting a spraying method to coat a coating.
4. According to the invention, through a specific heat treatment process, the technical scheme further improves the heat stability of the coating, so that the coating can maintain good performance in a high-temperature environment, the requirements of high-temperature processes such as epitaxial growth of silicon carbide and the like are met, and the composite coating provided by the technical scheme can effectively protect graphite parts and prevent the graphite parts from reacting with the environment at high temperature, thereby improving the stability and service life of the graphite parts and reducing the use cost.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only of the invention and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a process flow for preparing a composite coating according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of a method for preparing a coating raw material according to an embodiment of the invention.
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
It is to be noted that unless otherwise defined, technical or scientific terms used herein should be taken in a general sense as understood by one of ordinary skill in the art to which the present invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
As shown in fig. 1-2, a graphite component for epitaxial growth of silicon carbide and a preparation process of a composite coating thereof comprise the following steps: firstly, preheating a graphite component in a high-purity nitrogen environment according to the mass ratio of 5% -10%; secondly, coating the graphite component subjected to preheating treatment with a coating raw material, wherein the coating raw material comprises 30-40% of carbon nanotubes, 20-30% of graphene, 10-20% of nano silicon carbide and 20-30% of high polymer binder in percentage by mass; and finally, carrying out heat treatment on the coated graphite part in a nitrogen environment to obtain the composite coating.
The temperature range of the preheating treatment is 200-500 ℃ and the duration time is 1-3 hours.
The preparation method of the coating raw material comprises the following specific steps:
preparing materials: preparing a required carbon nano tube, graphene, nano silicon carbide and a high polymer binding agent, wherein the mass ratio of the raw materials is as follows: 30-40% of carbon nano tube, 20-30% of graphene, 10-20% of nano silicon carbide and 20-30% of high polymer binder.
Mixing materials: the raw materials are placed into a mixer for mixing, and the mixing time is required to ensure that all the raw materials can be uniformly distributed.
Ultrasonic treatment: and carrying out ultrasonic treatment on the mixed coating raw materials for 30-60 minutes, wherein the ultrasonic treatment can further promote the uniform mixing of the raw materials. And simultaneously, the adhesive property of the coating raw material is enhanced, so that the coating is more uniform and firmer.
The preparation of the coating raw materials is completed: after the ultrasonic treatment is completed, a coating raw material for coating the graphite member is obtained.
The coating step includes a spraying method, a coating thickness ranging from 100 to 500 μm, a coating speed ranging from 5 to 10 mm/s, and a distance between the graphite member and the nozzle during the above coating process being maintained at 10 to 20 cm.
The heat treatment is carried out at 800-1200deg.C for 2-4 hr, and the temperature rise and fall rate is maintained at 2-5deg.C/min during the heat treatment.
The graphite component comprises a graphite crucible, wherein the volume of the graphite crucible ranges from 500 cubic centimeters to 2000 cubic centimeters, and the surface roughness of the graphite crucible ranges from 0.2 micrometers to 0.5 micrometers.
The polymer binder comprises polyester, polyester ketone and polyimide, and the curing condition of the polymer binder is that the temperature is 80-120 ℃ and the time is 1-2 hours.
The nitrogen atmosphere is 99.99% high purity nitrogen atmosphere, and the nitrogen flow is in the range of 5-10 liters/min, and such nitrogen atmosphere is maintained during the whole coating and heat treatment process to avoid the influence of oxygen and water vapor.
The size ranges of the carbon nano tube, the graphene and the nano silicon carbide are respectively 10-20 nanometers, 1-5 layers and 10-50 nanometers, the length range of the carbon nano tube is 0.5-2 micrometers, the lattice constant of the graphene is 0.142-0.146 nanometers, and the lattice constant of the nano silicon carbide is 0.43-0.44 nanometers.
The following describes the embodiments of the present invention in further detail with reference to specific examples, but is not intended to limit the scope of the present invention:
example 1:
firstly, preparing required carbon nano tube, graphene, nano silicon carbide and polyester ketone bonding agent, wherein the mass ratio is as follows: 35% of carbon nano tube, 25% of graphene, 15% of nano silicon carbide and 25% of polyester ketone bonding agent. Putting the raw materials into a mixer for mixing for 30 minutes, and then performing ultrasonic treatment for 45 minutes to prepare a uniform composite coating raw material;
then, the coating raw material was coated on the graphite member using a spray coating method with a coating thickness of 300 μm and a coating speed of 7 mm/sec, and the distance between the graphite member and the nozzle was maintained at 15 cm;
finally, the coated graphite parts were heat treated in a 99.99% high purity nitrogen atmosphere at a temperature of 1000 ℃ for 3 hours maintaining the rate of temperature rise and fall at 3 ℃/min.
Example 2:
firstly, preparing required carbon nano tubes, graphene, nano silicon carbide and polyester bonding agents, wherein the mass ratio is as follows: 30% of carbon nano tube, 30% of graphene, 20% of nano silicon carbide and 20% of polyester bonding agent. Putting the raw materials into a mixer for mixing for 40 minutes, and then performing ultrasonic treatment for 50 minutes to prepare a uniform composite coating raw material;
then, the coating raw material was coated on the graphite member using a spray coating method with a coating thickness of 400 μm and a coating speed of 8 mm/sec, and the distance between the graphite member and the nozzle was maintained at 12 cm;
finally, the coated graphite parts were heat treated in a 99.99% high purity nitrogen atmosphere at 1100 ℃ for 2.5 hours maintaining the rate of temperature rise and fall at 4 ℃/min.
Example 3:
firstly, preparing required carbon nano tubes, graphene, nano silicon carbide and polyimide bonding agents, wherein the mass ratio is as follows: 40% of carbon nano tube, 20% of graphene, 10% of nano silicon carbide and 30% of polyimide bonding agent. Putting the raw materials into a mixer for mixing for 35 minutes, and then performing ultrasonic treatment for 60 minutes to prepare a uniform composite coating raw material;
next, a coating raw material was coated on the graphite member using a spray coating method, the coating thickness was 200 μm, the coating speed was 6 mm/sec, and the distance between the graphite member and the nozzle was maintained at 18 cm;
finally, the coated graphite parts were heat treated in a 99.99% high purity nitrogen atmosphere at 900 ℃ for 4 hours maintaining the rate of temperature rise and fall at 2 ℃/min.
All of the examples described above, which are based on different parameters and different material ratios, are intended to aid in understanding the invention and are not intended to limit the invention, as long as the coating process and steps are correct, and the desired composite coated graphite article can be obtained regardless of the ratio of coating materials and the specific parameters of the heat treatment, and many variations and modifications are possible without departing from the spirit and scope of the invention.
The following are experimental data obtained according to example 1, example 2 and example 3.
Table 1: mass ratio of composite coating raw material and ultrasonic treatment time
| Examples | Carbon nanotubes | Graphene | Nano silicon carbide | Binding agent | Ultrasonic treatment time |
| Example 1 | 35％ | 25％ | 15％ | 25％ | 45 minutes |
| Example 2 | 30％ | 30％ | 20％ | 20％ | 50 minutes |
| Example 3 | 40％ | 20％ | 10％ | 30％ | 60 minutes |
As can be seen from table 1, as the ratio of carbon nanotubes increases and the ratio of graphene decreases, the ultrasonic treatment time increases because the dispersibility of carbon nanotubes is inferior to that of graphene, and longer ultrasonic treatment is required to ensure uniform dispersion.
Table 2: spraying parameters and heat treatment parameters
| Examples | Coating thickness | Coating speed | Heat treatment temperature | Heat treatment time | Ultrasonic treatment time |
| Example 1 | 300 micrometers | 7 mm/s | 1000℃ | 3 hours | 45 minutes |
| Example 2 | 400 micrometers | 8 mm/s | 1100℃ | 2.5 hours | 50 minutes |
| Example 3 | 200 micrometers | 6 mm/s | 900℃ | 4 hours | 60 minutes |
As can be seen from table 2, the coating thickness, coating speed and heat treatment temperature, time all varied in three examples, reflecting that different coating and heat treatment parameters are critical to achieving the desired coating quality and performance.
Table 3: coating performance parameters
In Table 3, the hardness of the coating is expressed as Vickers Hardness Value (HV), the oxidation resistance is expressed as the number of hours maintained at 1000℃and the thermal stability is also expressed as the number of hours maintained at 1000℃and the adhesion of the coating is expressed as the force value (N) obtained by the standard adhesion test, it can be seen that the hardness, oxidation resistance, thermal stability, adhesion of the coating and other performance parameters of example 2 are the best but the adhesion of the coating of example 3 is slightly weaker depending on the examples, and these data indicate that the performance parameters of the coating can be adjusted to meet different application requirements by adjusting the mass ratio of the coating raw materials and the parameters of the coating preparation process.
The present invention is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the scope of the present invention.
Claims (9)
1. The preparation process of the graphite component for epitaxial growth of the silicon carbide and the composite coating thereof is characterized by comprising the following steps:
step one: firstly, preheating a graphite component in a high-purity nitrogen environment according to the mass ratio of 5% -10%;
step two: coating a graphite component subjected to preheating treatment with a coating raw material, wherein the coating raw material comprises, by mass, 30% -40% of carbon nanotubes, 20% -30% of graphene, 10% -20% of nano silicon carbide and 20% -30% of a high-molecular bonding agent;
step three: and carrying out heat treatment on the coated graphite component in a nitrogen environment to obtain the composite coating.
2. The graphite component for epitaxial growth of silicon carbide and process for preparing composite coating thereof according to claim 1, wherein the preheating treatment is carried out at a temperature ranging from 200 to 500 ℃ for a duration ranging from 1 to 3 hours.
3. The graphite component for epitaxial growth of silicon carbide and the preparation process of the composite coating thereof according to claim 1, wherein the specific steps of the preparation method of the coating raw material are as follows:
preparing materials: preparing a required carbon nano tube, graphene, nano silicon carbide and a high polymer binding agent, wherein the mass ratio of the raw materials is as follows: 30-40% of carbon nano tube, 20-30% of graphene, 10-20% of nano silicon carbide and 20-30% of high polymer binder.
Mixing materials: the raw materials are placed into a mixer for mixing, and the mixing time is required to ensure that all the raw materials can be uniformly distributed.
Ultrasonic treatment: and carrying out ultrasonic treatment on the mixed coating raw materials for 30-60 minutes, wherein the ultrasonic treatment can further promote the uniform mixing of the raw materials. And simultaneously, the adhesive property of the coating raw material is enhanced, so that the coating is more uniform and firmer.
The preparation of the coating raw materials is completed: after the ultrasonic treatment is completed, a coating raw material for coating the graphite member is obtained.
4. The graphite component for epitaxial growth of silicon carbide and process for preparing a composite coating thereof according to claim 1, wherein the coating step comprises a spray coating method, the coating thickness is in the range of 100 to 500 μm, the coating speed is 5 to 10 mm/s, and the distance between the graphite component and the nozzle is maintained at 10 to 20 cm during the above coating.
5. The graphite component for epitaxial growth of silicon carbide and process for preparing a composite coating thereof according to claim 1, wherein the heat treatment is carried out at a temperature ranging from 800 to 1200 ℃ for a duration ranging from 2 to 4 hours, and the rate of temperature rise and fall is maintained at 2 to 5 ℃/min during the heat treatment.
6. The graphite component for epitaxial growth of silicon carbide and the process for preparing the composite coating thereof according to claim 1, wherein the graphite component comprises a graphite crucible having a volume ranging from 500 to 2000 cubic centimeters and a surface roughness Ra of 0.2 to 0.5 μm.
7. The graphite component for epitaxial growth of silicon carbide and the preparation process of the composite coating thereof according to claim 1, wherein the polymer binder comprises polyester, polyester ketone and polyimide, and the curing condition of the polymer binder is that the temperature is 80-120 ℃ and the time is 1-2 hours.
8. The graphite component for epitaxial growth of silicon carbide and process for preparing composite coating thereof according to claim 1, wherein the nitrogen atmosphere is 99.99% high purity nitrogen atmosphere, and the flow rate of nitrogen is in the range of 5-10 liters/min, and such nitrogen atmosphere is maintained during the whole coating and heat treatment.
9. The preparation process of the graphite component for epitaxial growth of silicon carbide and the composite coating thereof according to claim 1, wherein the carbon nanotubes, the graphene and the nano silicon carbide have the size ranges of 10-20 nanometers, 1-5 layers and 10-50 nanometers respectively, the length of the carbon nanotubes is 0.5-2 micrometers, the lattice constant of the graphene is 0.142-0.146 nanometers, and the lattice constant of the nano silicon carbide is 0.43-0.44 nanometers.
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| CN115992383A (en) * | 2021-10-20 | 2023-04-21 | 昊石新材料科技南通有限公司 | Preparation method of coating for silicon carbide epitaxial growth equipment carrier disc |
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