CN116768653B - Carbon-carbon thermal field crucible containing composite ceramic coating and preparation method thereof - Google Patents
Carbon-carbon thermal field crucible containing composite ceramic coating and preparation method thereof Download PDFInfo
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- CN116768653B CN116768653B CN202310710968.2A CN202310710968A CN116768653B CN 116768653 B CN116768653 B CN 116768653B CN 202310710968 A CN202310710968 A CN 202310710968A CN 116768653 B CN116768653 B CN 116768653B
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- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000011203 carbon fibre reinforced carbon Substances 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000005524 ceramic coating Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 31
- 239000010703 silicon Substances 0.000 claims abstract description 31
- 238000005507 spraying Methods 0.000 claims abstract description 31
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 20
- 229910052582 BN Inorganic materials 0.000 claims abstract description 19
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 19
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 239000011247 coating layer Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 20
- 239000007921 spray Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
- 238000005229 chemical vapour deposition Methods 0.000 claims description 7
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000005011 phenolic resin Substances 0.000 claims description 6
- 229920001568 phenolic resin Polymers 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 239000003345 natural gas Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 66
- 238000000576 coating method Methods 0.000 abstract description 66
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 19
- 239000010453 quartz Substances 0.000 abstract description 15
- 238000005336 cracking Methods 0.000 abstract description 9
- 238000005260 corrosion Methods 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 7
- 229920005989 resin Polymers 0.000 abstract description 5
- 239000011347 resin Substances 0.000 abstract description 5
- 238000007740 vapor deposition Methods 0.000 abstract description 5
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000011863 silicon-based powder Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000000746 purification Methods 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
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
-
- 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
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a carbon-carbon thermal field crucible containing a composite ceramic coating and a preparation method thereof, wherein the carbon-carbon thermal field crucible is prepared by spraying resin solution to mix silicon carbide whisker and silicon slurry on the surface of a carbon crucible substrate, placing the carbon crucible substrate into an oven for curing, continuously spraying resin solution to mix boron nitride and silicon slurry, placing the carbon crucible substrate into the oven for curing to obtain a composite coating blank, and then enabling the carbonized spray coating to be firmly and compactly adsorbed by vapor deposition; finally, silicon in the coating is reacted through high-temperature heat treatment, and corresponding impurities are removed and purified to prepare the product; the silicon carbide whisker of the inner coating has certain toughness, and can slow down the cracking phenomenon of the coating, thereby greatly prolonging the service life of the coating and further greatly prolonging the service life of the carbon-carbon crucible; the boron nitride of the outer coating has poor wettability to silicon, silicon oxide and the like, and is favorable for disassembling the quartz crucible after being used; silicon and carbon in the coating can react to generate silicon carbide, so that the silicon corrosion resistance of the product and the adsorption capacity of the coating are improved.
Description
Technical Field
The invention is applied to the technical field of single crystal/polycrystal thermal field tools/components, and particularly relates to a carbon-carbon thermal field crucible containing a composite ceramic coating and a preparation method thereof.
Background
At present, the main stream of the single crystal/polycrystal thermal field crucible is still made of carbon-carbon composite materials, and a few of the single crystal/polycrystal thermal field crucibles use graphite; when the carbon-carbon composite material is applied to a thermal field crucible, the service life of the carbon-carbon composite material is easily influenced by silicon corrosion; meanwhile, softening occurs in the use process of the quartz crucible, the carbon-carbon composite material crucible bearing the quartz crucible is firmly adsorbed together and is difficult to clean, the quartz crucible is often required to be knocked and broken to be taken out, the production process of products is greatly influenced, and the production cost is indirectly increased.
Disclosure of Invention
Aiming at the problems in the prior art, the first aim of the invention is to provide a preparation method of a carbon-carbon thermal field crucible with a composite ceramic coating, which has the advantages of long service life and easy cleaning.
The second purpose of the invention is to provide a carbon-carbon thermal field crucible which is prepared by the preparation method and contains the composite ceramic coating and has high service life and easy cleaning.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a preparation method of a carbon-carbon thermal field crucible containing a composite ceramic coating, which comprises the steps of spraying slurry A containing silicon carbide whiskers and silicon on the surface of a carbon-carbon crucible substrate for the first time, solidifying for the first time to obtain a carbon-carbon crucible containing an inner coating layer, spraying slurry B containing boron nitride and silicon on the surface of the carbon-carbon crucible containing the inner coating layer for the second time, solidifying for the second time to obtain a carbon-carbon crucible containing a double coating layer, carrying out chemical vapor deposition on carbon, and carrying out heat treatment to obtain the carbon-carbon thermal field crucible containing the composite ceramic coating.
According to the preparation method, firstly, the resin solution is sprayed on the surface of the carbon-carbon crucible substrate to mix silicon carbide whisker and silicon slurry, the mixture is placed into an oven for curing, then the resin solution is continuously sprayed to mix boron nitride and silicon slurry, the mixture is placed into the oven for curing to obtain a composite coating blank, and then the carbonized spray coating is firmly and compactly adsorbed through vapor deposition; finally, the product is prepared by high-temperature heat treatment; the silicon carbide whisker of the inner coating has certain toughness, and can slow down the cracking phenomenon of the coating, thereby greatly prolonging the service life of the coating and further greatly prolonging the service life on the basis of a carbon-carbon crucible; the boron nitride of the outer coating has poor wettability to silicon, silicon oxide and the like, and is favorable for disassembling the quartz crucible after being used; in addition, a small amount of silicon is doped in the coating, and the silicon can react with carbon to form a whole coating, so that silicon carbide is generated at the same time, and the silicon corrosion resistance of the product is improved.
Preferably, the slurry A comprises the following components in parts by weight: 4-6 parts of phenolic resin, 4-6 parts of ethanol, 6-10 parts of silicon carbide whisker and 3-5 parts of silicon powder.
In the slurry A, the silicon carbide whisker has good toughness, can modify the quality of the coating, and slows down the cracking phenomenon of the coating, thereby greatly prolonging the service life of the coating; the silicon post-process in the coating can react with carbon on the surface of the carbon-carbon thermal field crucible and resin carbon to generate silicon carbide, so that the adsorptivity and the silicon corrosion resistance of the composite coating are further improved. However, the silicon carbide whisker content needs to be effectively controlled, the too large thickness of the slurry A can cause too high viscosity, so that the spray gun cannot be used normally, the thickness uniformity of a sprayed coating is difficult to ensure, the utilization rate of the slurry A is reduced, and the cost is comprehensively increased to reduce the quality of the coating; the toughness of the coating is reduced due to the too small content of silicon carbide whisker, and the cracking risk of the coating is increased;
preferably, the length of the silicon carbide whisker is 10-100 mu m, and the diameter is 0.1-1.0 mu m; the granularity of the silicon powder is 1000-3000 meshes. The silicon carbide whisker and the silicon powder with the sizes can effectively ensure the quality of the coating and smoothly pass through the spray gun.
Preferably, the caliber of the spray gun used for the first spraying is phi 2.0-5.0mm, the spraying pressure is 0.2-0.4MPa, and the spraying distance is 100-200mm. The inventors found that the smoothness of the slurry of the present invention was optimal by controlling the caliber of the spray gun within the above range, and the spray pressure and the spray distance within the above range, and the quality of the finally sprayed inner coating layer was optimal, and the utilization of the slurry was highest.
In the actual operation process, the spray gun can be pneumatic or electric.
Preferably, the temperature of the first cure is 150 to 220 ℃, preferably 180 ℃, and the time of the first cure is 1 to 3 hours, preferably 2 hours.
Preferably, in the carbon-carbon crucible containing an inner coating layer, the thickness of the inner coating layer is 0.1 to 0.4mm, preferably 0.3mm. Too thin coating layer has insufficient capability of enhancing the modifying ability, and the risk of cracking and falling off caused by too thick coating layer is aggravated.
Preferably, the slurry B comprises, by mass, 4-6 parts of phenolic resin, 4-6 parts of ethanol, 6-10 parts of boron nitride and 3-5 parts of silicon.
In the slurry B, the boron nitride contained in the slurry B has poor wettability to silicon, silicon oxide and the like, so that the disassembly difficulty of the quartz crucible after use is reduced; meanwhile, the oxidation resistance and the silicon etching resistance of the carbon-carbon thermal field crucible are obviously improved.
Preferably, the grain size of the boron nitride is 1000-3000 meshes, and the grain size of the silicon powder is 1000-3000 meshes. The quality of the coating can be effectively ensured by adopting the boron nitride and the silicon powder with the sizes, and the coating can smoothly pass through the spray gun.
Preferably, the caliber of the spray gun used for the second spraying is phi 2.0-5.0mm, the spraying pressure is 0.2-0.4MPa, and the spraying distance is 100-200mm.
In the actual operation process, the spray gun can be pneumatic or electric.
Preferably, the temperature of the second cure is 150-220 ℃, preferably 180 ℃, and the time of the second cure is 1-3 hours, preferably 2 hours.
Preferably, in the carbon-carbon crucible containing a double coating layer, the thickness of the double coating layer is 0.2-0.7mm, preferably 0.5mm. Too thin coating layer has insufficient capability of enhancing the modifying ability, and the risk of cracking and falling off caused by too thick coating layer is aggravated.
Preferably, when carbon is deposited in the chemical vapor deposition mode, one of propylene, natural gas and methane is used as a carbon source atmosphere, nitrogen is used as a dilution atmosphere, and the volume ratio of the carbon source atmosphere to the dilution atmosphere is 1-3:1.
Preferably, the temperature of the chemical vapor deposition is 975-985 ℃, the pressure is 0.8-1.2KPa, and the time is 30-50h, preferably 35-45h, and more preferably 40h.
By controlling chemical vapor deposition within the above range, gaps in the double coating layers in the carbon-carbon crucible containing the double coating layers are filled with vapor deposited carbon to form a new continuous composite coating blank.
Preferably, the heat treatment is performed under an argon atmosphere at a temperature of 1800-2200 ℃, preferably 2000 ℃, for a time of 1-3 hours, preferably 2 hours.
Silicon in the new composite coating blank reacts with carbon to generate silicon carbide through high-temperature heat treatment to obtain a carbon-carbon thermal field crucible composite ceramic coating product, so that the adsorptivity and silicon erosion resistance of the composite coating are further improved; meanwhile, the high-temperature heat treatment can exude some metal impurities in the product, can play a role in purification, and can avoid pollution in the subsequent use process of the product.
The invention also provides the carbon-carbon thermal field crucible containing the composite ceramic coating, which is prepared by the preparation method.
Compared with the prior art, the invention has the following advantages:
(1) The coating spraying technology of the invention greatly improves the thickness, appearance and performance uniformity of the coating.
(2) The introduction of the silicon carbide whisker of the inner coating enhances the toughness of the coating, greatly reduces the cracking condition of the coating and prolongs the service life of the coating; the outer coating boron nitride has poor wettability to silicon, silicon oxide and the like, and reduces the disassembly difficulty of the quartz crucible after use.
(3) According to the invention, after the preparation of the composite coating blank, the carbon is deposited in a gas phase, so that the compactness, the continuity and the adsorptivity of the carbonized coating blank are all repaired and improved, and the performance of the carbonized coating blank is ensured.
(4) According to the invention, silicon in the coating reacts with carbon to produce silicon carbide, so that the adsorptivity and silicon corrosion resistance of the composite coating are further improved; the heat treatment also eliminates some metal impurities in the product, and the purity of the product is improved to a certain extent.
Detailed Description
The invention is further illustrated below with reference to examples and comparative examples.
Example 1
(1) Preparing phenolic resin: ethanol: silicon carbide whiskers: the mass ratio of the silicon powder is 5:5:8:4, wherein the length of the silicon carbide whisker is 10-100 mu m, and the diameter is 0.1-1.0 mu m; the granularity of the silicon powder is 1000-3000 meshes,
spraying a whisker inner coating of 0.3mm on a carbon-carbon thermal field crucible substrate by using a spray gun, and curing to obtain an inner coating blank; the caliber of a spray gun used for the first spraying is phi 4mm, the spraying pressure is controlled to be 0.3MPa during the spraying, and the spraying distance is 150mm;
(2) Preparing phenolic resin: ethanol: boron nitride: the mass ratio of the silicon powder is 5:5:8:4, wherein the grain size of the boron nitride is 1000-3000 meshes, the grain size of the silicon powder is 1000-3000 meshes,
continuously spraying a boron nitride coating with the thickness of 0.2mm by using a spray gun, and curing to obtain a composite coating blank; the caliber of a spray gun used for the second spraying is phi 4mm, the spraying pressure is controlled to be 0.3MPa during the spraying, and the spraying distance is 150mm;
(3) Introducing 1 at 980+/-5 ℃ and furnace pressure of 0.8-1.2 KPa: 1, propylene and nitrogen are subjected to vapor deposition for 40 hours to obtain a new coating blank;
(4) And (3) carrying out high-temperature heat treatment for 2 hours at 2000 ℃ in Ar atmosphere to obtain the carbon-carbon thermal field crucible composite ceramic coating product.
In the embodiment, the surface quality of the carbon-carbon thermal field crucible composite ceramic coating is smooth and intact, and obvious cracking and falling phenomena are avoided. After the product is in service for 8 months, the carbon-carbon thermal field crucible is not obviously damaged, the composite coating is slightly damaged but does not influence the continuous use, and the product still has a better protection effect. The quartz crucible is not adhered and dead in the using process of 8 months.
Example 2
Example 2 and example 1 only changed the thickness of the inner coating to 0.2mm.
In the embodiment, the composite coating is slightly damaged and falls off in a small area after the product is in service for 8 months; the coating layer has a certain protection function on the carbon-carbon thermal field crucible after product evaluation. The quartz crucible is not adhered and dead in the using process of 8 months.
Example 3
Example 3 and example 1 only changed the boron nitride coating thickness to 0.1mm.
In the embodiment, the composite coating is damaged and falls off after the product is in service for 8 months, and the surface of the carbon-carbon thermal field crucible also has slight chipping; the composite coating is peeled off because the quartz crucible is partially stuck after being used, and the composite coating is damaged together in the process of knocking the quartz crucible; the embodiment shows that the composite coating plays a good role in protecting the carbon-carbon thermal field crucible in the early 8 months of use, the protection effect of the coating in the later period is reduced, the crucible is mainly used continuously by depending on the self performance of the carbon-carbon thermal field crucible, but the service life of the product of the embodiment is still far longer than that of the carbon-carbon thermal field crucible without the coating.
Example 4
Example 4 and example 1 only changed the vapor deposition time to 30h.
In the embodiment, the surface of the carbon-carbon thermal field crucible composite ceramic coating is rough, the flatness is poor, and a certain small pit is formed. After the product is in service for 8 months, the composite coating is damaged and falls off in a small area; in the use process of 8 months, the quartz crucible has small-area adhesion phenomenon, which is presumably due to the fact that the deposition time is too short, and the pores of the composite coating blank after carbonization are not completely repaired, so that the quality of the coating is slightly reduced.
Example 5
Example 5 and example 1 only changed the vapor deposition time to 50h.
In this embodiment, the composite coating has good surface flatness, but fine cracks appear. After the product is in service for 8 months, the composite coating falls off in a smaller area, and the surface of the carbon-carbon thermal field crucible also has slight chipping; the phenomenon of adhesion and death of the quartz crucible occurs in the use process of 8 months, and presumably, due to the increase of the deposition time of the composite coating blank, the deposited carbon continues to be accumulated on the surface of the boron nitride coating after the pores of the carbonized composite coating blank are completely repaired, so that the anti-quartz adhesion of the boron nitride is affected to a certain extent.
Comparative example 1
Comparative example 1 only an uncoated carbothermal field crucible was used. After 5 months of service, the carbon-carbon thermal field crucible has the phenomena of surface corrosion, cracking and the like, and the quartz crucible is adhered for a plurality of times in the service process, so that the product is nearly scrapped.
Comparative example 2
Comparative example 2 differs from example 1 in that there is only one silicon carbide whisker coating layer, and there is no difference in the others. After 8 months of service, the surface coating is totally fallen off, and the problems of corrosion, chipping and the like of the surface of the carbon-carbon thermal field crucible occur.
Claims (6)
1. A preparation method of a carbon-carbon thermal field crucible containing a composite ceramic coating is characterized by comprising the following steps of: firstly spraying slurry A containing silicon carbide whiskers and silicon on the surface of a carbon-carbon crucible substrate for the first time, curing for the first time to obtain a carbon-carbon crucible containing an inner coating layer, then spraying slurry B containing boron nitride and silicon on the surface of the carbon-carbon crucible containing the inner coating layer for the second time, curing for the second time to obtain a carbon-carbon crucible containing double coating layers, performing chemical vapor deposition on carbon, and performing heat treatment to obtain a carbon-carbon thermal field crucible containing a composite ceramic coating layer;
the slurry A consists of the following components in parts by weight: 4-6 parts of phenolic resin, 4-6 parts of ethanol, 6-10 parts of silicon carbide whisker and 3-5 parts of silicon;
the length of the silicon carbide whisker is 10-100 mu m, and the diameter is 0.1-1.0 mu m; the granularity of the silicon is 1000-3000 meshes;
in the carbon-carbon crucible containing the inner coating layer, the thickness of the inner coating layer is 0.1-0.3mm;
the slurry B consists of the following components in parts by weight: 4-6 parts of phenolic resin, 4-6 parts of ethanol, 6-10 parts of boron nitride and 3-5 parts of silicon; the grain size of the boron nitride is 1000-3000 meshes, and the grain size of the silicon is 1000-3000 meshes;
in the carbon-carbon crucible containing the double coating layers, the thickness of the double coating layers is 0.5-0.7mm;
when the chemical vapor deposition is carried out, one of propylene, natural gas and methane is used as a carbon source atmosphere, nitrogen is used as a dilution atmosphere, and the volume ratio of the carbon source atmosphere to the dilution atmosphere is 1-3:1;
the temperature of the chemical vapor deposition is 975-985 ℃, the pressure is 0.8-1.2KPa, and the time is 30-50h;
the heat treatment is carried out in an argon atmosphere, the temperature of the heat treatment is 1800-2200 ℃, and the time of the heat treatment is 1-3 hours.
2. The method for preparing the carbon-carbon thermal field crucible containing the composite ceramic coating according to claim 1, wherein the method comprises the following steps: the caliber of the spray gun used for the first spraying is phi 2.0-5.0mm, the spraying pressure is 0.2-0.4MPa, and the spraying distance is 100-200mm.
3. The method for preparing the carbon-carbon thermal field crucible containing the composite ceramic coating according to claim 1, wherein the method comprises the following steps: the temperature of the first curing is 150-220 ℃, and the time of the first curing is 1-3h.
4. The method for preparing the carbon-carbon thermal field crucible containing the composite ceramic coating according to claim 1, wherein the method comprises the following steps: the caliber of the spray gun used for the second spraying is phi 2.0-5.0mm, the spraying pressure is 0.2-0.4MPa, and the spraying distance is 100-200mm.
5. The method for preparing the carbon-carbon thermal field crucible containing the composite ceramic coating according to claim 1, wherein the method comprises the following steps: the temperature of the second curing is 150-220 ℃, and the time of the second curing is 1-3h.
6. A carbon-carbon thermal field crucible containing a composite ceramic coating prepared by the method of any one of claims 1-5.
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