CN114368984B - Coating of carbon substrate and preparation method and application thereof - Google Patents
Coating of carbon substrate and preparation method and application thereof Download PDFInfo
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- CN114368984B CN114368984B CN202210111120.3A CN202210111120A CN114368984B CN 114368984 B CN114368984 B CN 114368984B CN 202210111120 A CN202210111120 A CN 202210111120A CN 114368984 B CN114368984 B CN 114368984B
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- 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
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- 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
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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
- C04B41/45—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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Abstract
The invention provides a carbon substrate coating and a preparation method and application thereof, wherein the preparation method at least comprises the following steps: mixing the hydrogel and the organosilane to form a mixture; applying the mixture to the surface of the carbon substrate to form a first coating layer; coating an organic tantalum solution on the first coating to form a second coating, wherein the second coating and the first coating form a composite coating; and heating and annealing the composite coating to form the coating of the carbon substrate. The coating of the carbon matrix, the preparation method and the application thereof can effectively improve the corrosion of the raw materials to the graphite crucible in the growth process of the silicon carbide crystal.
Description
Technical Field
The invention belongs to the field of film preparation, and particularly relates to a coating of a carbon substrate, and a preparation method and application thereof.
Background
The carbon-based material has excellent temperature resistance, excellent structural strength, good thermal conductivity, chemical properties, dimensional stability and the like, and is widely applied in various fields. With the continuous expansion of the application field and the continuous improvement of the performance requirements of application components, the working environment of the carbon-based material is increasingly harsh, and the carbon-based material has the problems of high-temperature oxidation ablation, solid particle scouring, chemical corrosion, molten salt erosion and the like.
In the application scene of the growth of the silicon carbide crystal, the raw materials have obvious corrosion effect on a graphite crucible, a graphite support piece and the like at high temperature, so that the silicon carbide crystal cannot be directly used for the crystal growth. Therefore, the development of a ceramic coating with high melting point, excellent oxidation and ablation resistance and stronger chemical corrosion resistance is very critical.
Disclosure of Invention
The invention provides a carbon matrix coating and a preparation method and application thereof, which can effectively improve the corrosion of raw materials to a graphite crucible in the growth process of a silicon carbide crystal, effectively solve the problem of thermal mismatch caused by overlarge difference of expansion coefficients of tantalum carbide and the carbon matrix by adopting a composite coating, prevent the coating from peeling off in the use process and improve the adhesiveness of the coating.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention provides a preparation method of a carbon substrate coating, which at least comprises the following steps:
mixing the hydrogel and the organosilane to form a mixture;
applying the mixture to the surface of the carbon substrate to form a first coating layer;
coating an organic tantalum solution on the first coating to form a second coating, wherein the second coating and the first coating form a composite coating; and
and heating and annealing the composite coating to form the coating of the carbon matrix.
In an embodiment of the present invention, the hydrogel is any one of graphene hydrogel, polyacrylic acid, polymethacrylic acid, polyacrylamide, poly-N-polyacrylamide, and chitosan.
In an embodiment of the present invention, the organosilane is any one or a mixture of polysilane, polysiloxane, and polycarbosilane.
In an embodiment of the present invention, the organic tantalum is any one of tantalum ethoxide, tantalum pentamethyl oxide, tantalum isopropoxide, tantalum butoxide or tantalum amyl alcohol.
In an embodiment of the present invention, the heating step includes placing the composite coating into a furnace cavity, and performing staged heating.
In an embodiment of the present invention, the heating step includes raising the temperature in the furnace cavity to 280-320 ℃, and the hydrogel, the organosilane and the organic tantalum are cracked and volatilized.
In an embodiment of the present invention, the heating step includes raising the temperature in the furnace chamber to 1100-1300 ℃ to bond silicon and carbon to form β -silicon carbide.
In an embodiment of the invention, the heating step includes raising the temperature in the furnace chamber to 1750-1850 ℃, and the second coating has long grains to fill gaps generated by gas volatilization.
Based on the preparation method, the invention also provides a coating of the carbon substrate, which at least comprises the following components:
a first coating applied to a surface of the carbon substrate, the first coating being a mixture of a hydrogel and an organosilane; and
and the second coating is coated on the first coating and forms a composite coating with the first coating, and the second coating comprises an organic tantalum solution.
The invention also provides a crucible, and the surface of the crucible is provided with the coating of the carbon matrix.
The invention provides a carbon matrix coating and a preparation method and application thereof, which can effectively improve the corrosion of raw materials to a graphite crucible in the growth process of a silicon carbide crystal, effectively solve the problem of thermal mismatch caused by overlarge difference of expansion coefficients of tantalum carbide and the carbon matrix by adopting a composite coating, prevent the coating from peeling off in the use process and improve the adhesiveness of the coating.
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FIG. 1 is a schematic flow diagram of the present invention.
Fig. 2 is a schematic structural diagram of the present invention.
Description of reference numerals:
a 100-carbon matrix; 200-a first coating; 300-second coating.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It should be noted that the drawings provided in the present embodiment are only for illustrating the basic idea of the present invention, and the components related to the present invention are only shown in the drawings rather than drawn according to the number, shape and size of the components in actual implementation, and the type, quantity and proportion of the components in actual implementation may be changed freely, and the layout of the components may be more complicated.
The technical solutions of the present invention are further described in detail below with reference to several embodiments and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The graphite crucible is processed by taking natural crystalline flake graphite as a main raw material and plastic refractory clay or carbon as a binder, and has the characteristics of high temperature resistance, strong heat conduction performance, good corrosion resistance, long service life and the like. In the high-temperature use process, the thermal expansion coefficient is small, and the high-temperature heat-resistant steel has certain strain resistance to rapid cooling and rapid heating. Has strong corrosion resistance to acidic and alkaline solutions, has excellent chemical stability, and does not participate in any chemical reaction in the smelting process. In the field of silicon carbide crystal growth, crucibles and other supports made of graphite play an important role in the preparation of silicon carbide crystals. However, the graphite crucible cannot be directly used for crystal growth due to the corrosive action of the raw materials on the crucible wall at high temperature. And the tantalum carbide coating is covered on the surface of the graphite, so that the graphite crucible can be prevented from being corroded. Referring to FIG. 1, the present invention provides a method for preparing a coating on a carbon substrate, including but not limited to the following steps S1-S4.
S1, mixing the hydrogel and organosilane to form a mixture.
And S2, coating the mixture on the surface of the carbon substrate 100 to form a first coating layer 200.
And S3, coating the organic tantalum solution on the first coating 200 to form a second coating 300, wherein the second coating 300 and the first coating 200 form a composite coating.
S4, heating and annealing the composite coating to form the coating of the carbon substrate.
Referring to fig. 1-2, in one embodiment of the present invention, the carbon substrate 100 is a graphite substrate, for example. Further, in order to ensure better bonding force and reactivity between the carbon substrate and the coating layer, impurities on the surface of the carbon substrate 100 may be removed in advance. In one embodiment of the present invention, the graphite substrate may be roughened by sand paper, and then placed in an ultrasonic device for ultrasonic cleaning, and then placed in an oven for drying. In an embodiment of the present invention, in the ultrasonic cleaning step, the ultrasonic cleaning liquid is an organic solution. Further, the cleaning solution is, for example, ethanol, acetone, acetonitrile, or ethyl acetate, and the ultrasonic time is, for example, 30 to 90min, and further, the ultrasonic time is, for example, 60min. In one embodiment of the present invention, in the step of drying in the oven, the drying temperature is, for example, 80 to 100 ℃, further, the drying temperature is, for example, 80 ℃, and the drying time is, for example, 8 to 10 hours.
Referring to fig. 1-2, in step S1, the hydrogel is mixed with the organosilane to form a viscous mixture of amber bodies with organosilane as an intermediate compound and arranged as a gel surrounding the organosilane. In some embodiments of the invention, the hydrogel is, for example, a graphene hydrogel, polyacrylic acid, polymethacrylic acid, polyacrylamide, poly-N-polyallylamine, or chitosan. In some embodiments of the present invention, the organosilane is, for example, one or more of polysilane, polysiloxane, polycarbosilane, or a mixture thereof.
Referring to fig. 1-2, in an embodiment of the present invention, the hydrogel in step S2 is, for example, a graphene-based hydrogel. The graphene-based hydrogel is formed by combining hydrogel and two-dimensional graphene nanosheets, has the characteristics of large specific surface area and porous structure, is similar to a carbon matrix material, does not introduce other impurities, and ensures the purity of the carbon matrix coating. In the embodiment, the organic silicon solution is polysilane, for example. The polysilane is mixed with the graphene-based hydrogel to form a three-dimensional arrangement stacking structure using the hydrogel as a main body and the polysilane as a cross-linking agent, as the first coating 200. In another embodiment of the present invention, the hydrogel is, for example, polyacrylic acid hydrogel, and the organosilane is, for example, liquid polycarbosilane, which are mixed uniformly to form a three-dimensional multi-layer structure mixture with polyacrylic acid hydrogel as a main body and polycarbosilane as an adhesive between gels, which is used as the first coating 200. In other embodiments, the first coating 200 may be a mixture of any other hydrogel and organosilane.
Referring to fig. 1-2, in some embodiments of the present invention, the organic tantalum solution in step S3 is, for example, a tantalum alkoxide, and further, is, for example, tantalum ethoxide, tantalum pentamethyl-oxide, tantalum isopropoxide, tantalum butoxide or tantalum amyl alcohol. In an embodiment of the present invention, when the organic tantalum solution is tantalum propoxide, for example, and the first coating 100 is a mixture of graphene-based hydrogel and polysilane, the graphene hydrogel outer layer absorbs the tantalum propoxide solution, and as the temperature gradually increases, the tantalum propoxide solution permeates to one side of the carbon substrate and contacts with the polysilane under different absorption effects of the multi-layer hydrogel. And with the continuous increase of the temperature, the silicon-hydrogen bond in the polysilane reacts with the carbon matrix and the tantalum propanol to form a C-Si-C crosslinking structure. The C-Si-C cross-linked structure has the advantage of tight bonding, and can remarkably improve the bonding of the tantalum carbide (TaC) coating and the carbon matrix. In another embodiment of the present invention, when the organic tantalum solution is, for example, tantalum ethoxide, and the first coating 100 is, for example, a mixture of polyacrylic hydrogel and liquid polycarbosilane, as the temperature increases, the tantalum ethoxide permeates toward one side of the carbon substrate under different adsorption of the multiple layers of hydrogel, the temperature increases to 1150 ℃, the active Si-H bond in the polycarbosilane reacts with the tantalum ethoxide to form Si-C-Ta, and as the temperature continues to increase, the gas phase Si reacts with the carbon substrate to form a C-Si chemical bond, and finally a transition bond of C-Si-C-Ta is formed, so as to achieve the purpose of forming a tantalum carbide (TaC) coating on the surface of the carbon substrate.
Referring to fig. 1-2, in step S4, the step of heating includes placing the carbon substrate coated with the composite coating into a furnace chamber, vacuuming, filling a protective gas, and performing a step-wise heating process. In the present embodiment, the flow rate of the shielding gas is 450-550mbar, for example, argon (Ar). In other embodiments, the shielding gas is also, for example, nitrogen (N) 2 )。
Referring to fig. 1-2, in an embodiment of the invention, the step-type heating step includes a plurality of heating stages, specifically, five heating stages. In the first temperature-raising heating stage, the temperature-raising rate is, for example, 1 to 2 ℃/min, the temperature is raised to, for example, 280 to 320 ℃, further, the heating temperature is, for example, 300 ℃, and the holding time is, for example, 2.5 to 3.5 hours. In the first heating stage, the hydrogel and the organic silane polymer are fully cracked and volatilized. In the second temperature-raising heating stage, the temperature-raising rate is, for example, 2 to 3 ℃/min, for example, the temperature is raised to 880 to 920 ℃, further, the heating temperature is, for example, 900 ℃, and the holding time is, for example, 1.5 to 2.5 hours. In the second heating stage, the composite coating is completely decomposed and foamed. In the third temperature-raising heating stage, the temperature-raising rate is, for example, 1 to 3 ℃/min, for example, the temperature is raised to 1100 to 1300 ℃, further, the heating temperature is, for example, 1200 ℃, and the reaction time is, for example, 7 to 9 hours. In the third temperature-increasing heating stage, si-C bonds are formed to form β -SiC. In the fourth temperature-raising heating stage, the temperature-raising rate is, for example, 1-3 ℃/min, the temperature is raised to, for example, 1750-1850 ℃, further, the heating temperature is, for example, 1800 ℃, and the holding time is, for example, 7-9h. In the fourth heating stage, the surface coating grows up in grains, and gaps caused by gas volatilization are filled. In the fifth heating stage, the heating rate is, for example, 1-3 deg.C/min, the temperature is increased to, for example, 2300-2500 deg.C, further, the heating temperature is, for example, 2400 deg.C, and the holding time is, for example, 9-11h. In the fifth ramping-up heating stage, the heat resistant tantalum carbide coating is fully formed.
Referring to fig. 1-2, in the step of heating at a stepwise temperature, as the temperature increases, the organic hydrogel adsorbs more organic tantalum solution to penetrate to a side close to the carbon substrate, the organosilane reacts with the carbon element in the carbon substrate and the organic tantalum respectively to form Si-C bonds, and as the reaction degree increases, the C-Si-C-Ta bonds are finally formed on the surface of the carbon substrate. Since the thermal expansion coefficients of the C/C composite material and the graphite are very low, the thermal expansion coefficients are respectively 1.0 multiplied by 10 -6 And 2.1 to 2.6X 10 -6 K, and TaC has a thermal expansion coefficient of 6.3X 10 -6 and/K, the difference of the thermal expansion coefficients of the coating and the substrate is too large, so that the common physical adsorption coating can generate cracks due to the generation of thermal stress after high-low temperature conversion in the preparation and application processes. Compared with a physical adsorption coating, the coating of the carbon matrix provided by the invention has strong adhesive force, reduces the difference of the thermal expansion coefficients of substances by being used as a transition connection layer, and greatly avoids the problems of thermal mismatch and coating peeling-off between the tantalum carbide coating and the carbon matrix at high temperature.
Referring to fig. 1-2, in one embodiment of the present invention, in step S4, the annealing step is, for example, a step-type cooling annealing step, which can prevent the coating from cracking due to rapid cooling, and the annealing step includes, for example, four cooling annealing stages. In the first temperature-reducing annealing stage, the temperature-reducing rate is, for example, 1-2 ℃/min, for example, the temperature is reduced to 1750-1850 ℃, further, the annealing temperature is, for example, 1800 ℃, and the holding time is, for example, 1.5-2.5h, so that the composite coating can be stably recrystallized. In the second cooling annealing stage, the cooling rate is, for example, 1 to 2 ℃/min, for example, the temperature is reduced to 1100 to 1300 ℃, further, the annealing temperature is, for example, 1200 ℃, and the holding time is, for example, 1.5 to 2.5 hours, so that the purpose of releasing thermal stress at medium temperature is achieved, and the coating is prevented from generating cracks. In the third temperature-reducing annealing stage, the temperature-reducing rate is, for example, 1 to 2 ℃/min, for example, the temperature is reduced to 750 to 850 ℃, further, the annealing temperature is, for example, 800 ℃, and the holding time is, for example, 1.5 to 2.5 hours, so as to achieve the purpose of releasing the thermal stress at low temperature. And in the fourth cooling and annealing stage, the composite coating is naturally cooled to room temperature along with the reaction furnace.
In conclusion, the invention provides the coating of the carbon substrate, and the preparation method and the application thereof, which can effectively improve the corrosion of the raw materials to the graphite crucible in the growth process of the silicon carbide crystal. The composite coating is adopted to effectively improve the problem of thermal mismatch caused by overlarge difference of the expansion coefficients of the tantalum carbide and the carbon matrix, prevent the coating from falling and peeling off in the using process and improve the adhesiveness of the coating. The method has the advantages of convenient operation and low cost, and has important application value.
The above description is only a preferred embodiment of the present application and a description of the applied technical principle, and it should be understood by those skilled in the art that the scope of the present invention related to the present application is not limited to the technical solution of the specific combination of the above technical features, and also covers other technical solutions formed by any combination of the above technical features or their equivalent features without departing from the inventive concept, for example, the technical solutions formed by mutually replacing the above features with (but not limited to) technical features having similar functions disclosed in the present application.
Other technical features than those described in the specification are known to those skilled in the art, and are not described herein in detail in order to highlight the innovative features of the present invention.
Claims (7)
1. A method for preparing a coating on a carbon substrate, characterized in that it comprises at least the following steps:
mixing the hydrogel and an organosilane containing reactive silicon hydrogen bonds to form a mixture;
applying the mixture to the surface of the carbon substrate to form a first coating layer;
coating an organic tantalum solution on the first coating to form a second coating, wherein the second coating and the first coating form a composite coating; and
heating and annealing the composite coating to form a coating of the carbon matrix;
the hydrogel is any one of graphene hydrogel, polyacrylic acid, polymethacrylic acid, polyacrylamide, poly-N-polyacrylamide and chitosan, and the graphene hydrogel is formed by combining water and two-dimensional graphene;
the organosilane is any one or a mixture of more of polysilane containing active silicon-hydrogen bonds, polysiloxane containing active silicon-hydrogen bonds and polycarbosilane containing active silicon-hydrogen bonds;
the organic tantalum is any one of tantalum ethoxide, tantalum pentamethyl oxide, tantalum isopropanol, tantalum butanol or tantalum amyl alcohol.
2. The method according to claim 1, wherein the heating step comprises heating the composite coating by stepwise temperature increase in a furnace chamber.
3. The method for preparing a carbon substrate coating according to claim 2, wherein the heating step comprises heating the temperature in the furnace cavity to 280-320 ℃, and the hydrogel, the organosilane and the organic tantalum are cracked and volatilized.
4. The method for preparing the coating of the carbon substrate according to claim 2, wherein the step of heating at an elevated temperature comprises heating the temperature in the furnace chamber to 1100-1300 ℃ to bond silicon and carbon to form the beta-silicon carbide.
5. The method of claim 2, wherein the heating step comprises heating the furnace chamber to 1750-1850 ℃ to increase the temperature of the furnace chamber, and the grains of the second coating grow to fill gaps generated by gas volatilization.
6. A coating of a carbon substrate obtained by the method for preparing a coating of a carbon substrate according to any one of claims 1 to 5.
7. A crucible characterized in that the surface of the crucible is provided with a coating of the carbon matrix according to claim 6.
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| CN115975520A (en) * | 2022-12-14 | 2023-04-18 | 华侨大学 | TAC composite film for polarizer and preparation method thereof |
| CN116023169A (en) * | 2022-12-28 | 2023-04-28 | 苏州优晶光电科技有限公司 | Graphite treatment process and graphite structure |
| CN116813383A (en) * | 2023-07-14 | 2023-09-29 | 中电化合物半导体有限公司 | Tantalum carbide coating and preparation method thereof |
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