CN114907145B - Carbon fiber composite material surface silicon carbide coating adhesive and preparation and use method thereof - Google Patents
Carbon fiber composite material surface silicon carbide coating adhesive and preparation and use method thereof Download PDFInfo
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- CN114907145B CN114907145B CN202210655501.8A CN202210655501A CN114907145B CN 114907145 B CN114907145 B CN 114907145B CN 202210655501 A CN202210655501 A CN 202210655501A CN 114907145 B CN114907145 B CN 114907145B
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- 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
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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
- C04B41/009—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
- C04B41/50—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
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Abstract
The invention relates to a silicon carbide coating adhesive on the surface of a carbon fiber composite material and a preparation and use method thereof, wherein the silicon carbide coating adhesive comprises the following components: 35-55% of water, 20-40% of silicon carbide powder, 1-10% of phenolic resin, 1-5% of adhesive and 15-30% of furan resin; the silicon carbide powder is divided into coarse silicon carbide powder and fine silicon carbide powder. Aiming at the defects of the existing slurry coating method, the invention improves the formula and the coating mode of the silicon carbide coating adhesive, and solves the problems of powder falling and poor oxidation resistance of the silicon carbide coating adhesive after graphitization; the preparation process avoids the introduction of metal impurities and oxides, thereby reducing the pollution of the metal impurities and the fiber loss caused by oxidation and prolonging the service life of the product; by adopting a twice coating mode, the bonding stress of the coating is reduced, the problem of stress cracking of the coating is avoided, the continuity and the integrity of the coating are ensured, and the coating does not have powder falling or coating cracks, so that the oxidation resistance of the silicon carbide is exerted to the maximum extent.
Description
Technical Field
The invention relates to the technical field of inorganic functional coating materials, in particular to a silicon carbide coating adhesive on the surface of a carbon fiber composite material and a preparation and use method thereof.
Background
Monocrystalline silicon has higher photoelectric conversion efficiency and prominent commercial advantages as a photovoltaic power generation material, and has become a mainstream material for solar photovoltaic power generation. The thermal field system is the most important component for single crystal silicon growth, and mainly consists of carbon materials (graphite materials, carbon/carbon composite materials and carbon fiber thermal insulation materials). With the continuous increase of the size of monocrystalline silicon, the size requirement of thermal field components is getting larger and larger, and carbon/carbon composite materials and carbon fiber thermal insulation materials become the first choice of thermal field materials for monocrystalline silicon due to the factors of excellent size stability, mechanical properties and the like.
During the process of pulling the monocrystalline silicon, silicon vapor and molten silicon are generated by melting the silicon material, so that the silicification erosion of the carbon/carbon thermal field material is caused, and the mechanical property and the service life of the carbon/carbon thermal field material are seriously influenced. The silicon carbide coating is the first choice for the surface protection coating of the carbon/carbon thermal field material due to the characteristics of excellent thermal shock resistance, wear resistance and the like. The silicon carbide coating is used for coating the surface of a target matrix, and the anti-oxidation performance and the service life of the carbon fiber composite material can be improved by utilizing the wear resistance, the corrosion resistance and the oxidation resistance of the silicon carbide.
Silicon carbide coatings are produced by a number of methods, including embedding, slurry coating, chemical Vapor Reaction (CVR), and Chemical Vapor Deposition (CVD). At present, a slurry coating method is commonly used for preparing SiC samples in a laboratory, and the specific process is as follows: and preparing a mixture from the coating material and the adhesive, uniformly coating the mixture on the surface of the substrate, drying, and sintering the coated test piece at high temperature in an inert atmosphere to obtain the required coating.
The slurry coating method has the advantages of simple operation and easy control of the thickness of the coating; the defects are that the coating and the matrix have low bonding strength, poor thermal shock resistance and low coating uniformity, so that the silicon carbide coating is easy to shed powder and poor in oxidation resistance, and cannot meet the requirements of customers.
The Chinese patent application with the publication number of CN110498684A discloses a preparation method of a silicon carbide coating, which comprises the following steps: (1) selecting and manufacturing a primary blank material: machining to dimensional accuracy to obtain an initial blank sample; (2) pretreatment of a primary blank sample: grinding, polishing, ultrasonically cleaning and drying for later use; (3) performing priming pretreatment on the primary blank sample: uniformly coating a priming paint on the surface, and then placing the priming paint in an oven for drying; (4) coating slurry brushing: coating silicon carbide coating slurry and drying; (5) sintering treatment: carrying out atmosphere sintering treatment on the dried primary blank sample; and a compact silicon carbide coating is generated on the surface of the primary blank sample after the sintering treatment. In the technical scheme, yttrium oxide powder is used, namely, metal impurities are introduced, and the influence on single crystal and semiconductor crystal growth is caused. In addition, it uses silica sol, the main component of which is SiO 2 At high temperature, the carbon fiber reacts with the carbon fiber to cause fiber oxidation corrosion and coating microcracks to accelerate oxygenThe loss is reduced, and the service life of the product is shortened.
Chinese patent application publication No. CN 110158309A discloses "a method for preparing carbon fibers having a silicon carbide coating on the surface", which comprises heating the carbon fibers for pretreatment, and then cooling to room temperature; uniformly mixing and stirring the SiC powder and the silicon rubber according to the mass ratio of 5-10; fully mixing carbon fibers with the mixed slurry according to the mass ratio of 3-5; and heating the carbon fiber fully soaked with the slurry to 400-600 ℃, reacting for 1-2h, and then cooling to room temperature to obtain the carbon fiber with the silicon carbide coating on the surface. The technical scheme is that carbon fibers are coated on the surfaces of the carbon fibers, siC powder and SiO generated after silicon rubber is pyrolyzed can be remained on the surfaces of the carbon fibers after reaction 2 The particles, when further treated at high temperature, will react with SiO 2 Occurs in a reaction that consumes carbon, causing oxidation of the fibers.
Disclosure of Invention
The invention provides a silicon carbide coating adhesive on the surface of a carbon fiber composite material and a preparation and use method thereof, aiming at the defects of the existing slurry coating method, the problems of powder falling and poor oxidation resistance of the silicon carbide coating adhesive after graphitization are solved by improving the formula and the coating mode of the silicon carbide coating adhesive; the preparation process avoids the introduction of metal impurities and oxides, thereby reducing the pollution of the metal impurities and the fiber loss caused by oxidation and prolonging the service life of the product; by adopting a twice coating mode, the bonding stress of the coating is reduced, the stress cracking problem of the coating is avoided, the continuity and the integrity of the coating are ensured, and the coating does not have powder falling or coating cracks, so that the oxidation resistance of the silicon carbide is exerted to the maximum extent.
In order to achieve the purpose, the invention adopts the following technical scheme:
a silicon carbide coating adhesive on the surface of a carbon fiber composite material is composed of the following components in percentage by mass: 35-55% of water, 20-40% of silicon carbide powder, 1-10% of phenolic resin, 1-5% of adhesive and 15-30% of furan resin; the silicon carbide powder is divided into coarse silicon carbide powder and fine silicon carbide powder, the coarse silicon carbide powder is used for preparing coarse silicon carbide coating adhesive, and the fine silicon carbide powder is used for preparing fine silicon carbide coating adhesive; the granularity of the coarse silicon carbide powder is 120-600 meshes, and the granularity of the fine silicon carbide powder is 800-2000 meshes.
A preparation method of silicon carbide coating glue on the surface of a carbon fiber composite material comprises the following steps:
(1) Preparing a matrix solution: uniformly mixing silicon carbide powder and phenolic resin powder, adding water into the mixture, and fully stirring until no precipitate is formed to obtain a silicon carbide matrix solution; the coarse silicon carbide coating adhesive is prepared by selecting coarse silicon carbide powder, and the fine silicon carbide coating adhesive is prepared by selecting fine silicon carbide powder;
(2) Preparing an adhesive: dissolving one or two of methyl cellulose and butyl cellulose in butyl diglycol, and uniformly stirring to obtain an adhesive;
(3) Preparing silicon carbide coating adhesive: and (3) pouring the adhesive prepared in the step (2) into the silicon carbide matrix liquid prepared in the step (1), stirring while pouring, pouring furan resin for continuously stirring after stirring until the mixture is uniform, and stopping stirring after a suspension with uniform color is formed to obtain the coarse silicon carbide coating adhesive or the fine silicon carbide coating adhesive.
The water is clean low hardness tap water.
In the adhesive, the mass ratio of cellulose consisting of methyl cellulose and/or butyl cellulose to butyl diglycol is =1:4 to 1:20.
the granularity of the phenolic resin is 800-2000 meshes, and the residual carbon value is 25-55%.
The furan resin is furfuryl alcohol resin, furfural-acetone resin or furfural-acetone-formaldehyde resin.
A method for using silicon carbide coating adhesive on the surface of a carbon fiber composite material sequentially coats coarse silicon carbide coating adhesive and fine silicon carbide coating adhesive on the surface of the carbon fiber composite material.
A use method of silicon carbide coating glue on the surface of a carbon fiber composite material specifically comprises the following steps:
1) Selecting a carbon fiber composite material, machining the carbon fiber composite material into a required shape and size to obtain a matrix, and cleaning the surface of the matrix;
2) Preparing and coating a coarse silicon carbide coating adhesive; after the coarse silicon carbide coating adhesive is prepared, the adhesive is mixed according to the proportion of 200-550 g/m 2 Coating the coarse silicon carbide coating glue on the surface of the substrate; after being coated, the mixture is put into an oven and is cured at the constant temperature of 150-300 ℃ for 1.5-3 h;
3) Preparing and coating fine silicon carbide coating glue; after the fine silicon carbide coating adhesive is prepared, 150-450 g/m 2 Coating the fine silicon carbide coating adhesive on the surface of the substrate which is subjected to the primary coating in the step 2) and is cured; after being coated, the mixture is put into an oven and is cured at the constant temperature of 150-300 ℃ for 1.5-3 h;
4) Placing the carbon fiber composite material coated with the coating for 2 times obtained in the step 3) into a carbonization furnace, and carbonizing for 5-7 days at 700-1000 ℃;
5) Placing the carbon fiber composite material carbonized in the step 4) in a vacuum furnace, and graphitizing the carbon fiber composite material at 1700-2200 ℃ for 2-4 days.
The thickness of the coarse silicon carbide coating is 100-300 mu m, and the thickness of the fine silicon carbide coating is 50-100 mu m.
Compared with the prior art, the invention has the beneficial effects that:
1) Adding resin into the raw materials, and fixing the silicon carbide powder and the surface of the carbon fiber composite material together by the generated residual carbon to form a continuous coating structure;
2) And the adhesive is added for increasing the viscosity and viscosity of the coating turbid liquid, so that the silicon carbide can be firmly fixed on the surface of the carbon fiber composite material without falling off at normal temperature or in the curing process.
3) Butyl diglycol is used as a dispersing agent for improving the dispersibility of the binder and uniformly dispersing the binder into water to form a uniform and stable solution;
4) The method adopts a mode of coating twice, the surface of the substrate is sequentially coated with a coarse silicon carbide coating adhesive and a fine silicon carbide coating adhesive, and the formed coarse silicon carbide coating is taken as a transition coating of the carbon fiber composite material and the fine silicon carbide coating, so that cracks caused by stress increase in the heat treatment process due to too much penetration of the fine silicon carbide powder are avoided;
5) The silicon silicide coating adhesive can exert the oxidation resistance of silicon carbide to the maximum extent.
Drawings
FIG. 1 is a schematic structural diagram of a carbon fiber composite material and a surface silicon carbide coating according to the present invention.
In the figure: 1. carbon fiber composite material (matrix) 2. Coarse silicon carbide coating adhesive 3. Fine silicon carbide coating adhesive
Detailed Description
The invention relates to a silicon carbide coating adhesive for the surface of a carbon fiber composite material, which comprises the following components in percentage by mass: 35-55% of water, 20-40% of silicon carbide powder, 1-10% of phenolic resin, 1-5% of adhesive and 15-30% of furan resin; the silicon carbide powder is divided into coarse silicon carbide powder and fine silicon carbide powder, the coarse silicon carbide powder is used for preparing coarse silicon carbide coating adhesive, and the fine silicon carbide powder is used for preparing fine silicon carbide coating adhesive; the granularity of the coarse silicon carbide powder is 120-600 meshes, and the granularity of the fine silicon carbide powder is 800-2000 meshes.
A preparation method of silicon carbide coating glue on the surface of a carbon fiber composite material comprises the following steps:
(1) Preparing a matrix solution: uniformly mixing silicon carbide powder and phenolic resin powder, adding water into the mixture, and fully stirring until no precipitate is formed to obtain a silicon carbide matrix solution; the coarse silicon carbide powder is selected when the coarse silicon carbide coating adhesive is prepared, and the fine silicon carbide powder is selected when the fine silicon carbide coating adhesive is prepared;
(2) Preparing an adhesive: dissolving one or two of methyl cellulose and butyl cellulose in butyl diglycol, and uniformly stirring to obtain an adhesive;
(3) Preparing silicon carbide coating adhesive: and (3) pouring the adhesive prepared in the step (2) into the silicon carbide matrix liquid prepared in the step (1), stirring while pouring, pouring furan resin for continuously stirring after stirring until the mixture is uniform, and stopping stirring after a suspension with uniform color is formed to obtain the coarse silicon carbide coating adhesive or the fine silicon carbide coating adhesive.
The water is clean low hardness tap water.
In the adhesive, the mass ratio of cellulose consisting of methyl cellulose and/or butyl cellulose to butyl diglycol is =1:4 to 1:20.
the granularity of the phenolic resin is 800-2000 meshes, and the residual carbon value is 25-55%.
The furan resin is furfuryl alcohol resin, furfural-acetone resin or furfural-acetone-formaldehyde resin.
A method for using silicon carbide coating adhesive on the surface of a carbon fiber composite material is characterized in that coarse silicon carbide coating adhesive 2 and fine silicon carbide coating adhesive 3 are sequentially coated on the surface of a carbon fiber composite material 1 (as shown in figure 1).
A use method of silicon carbide coating glue on the surface of a carbon fiber composite material specifically comprises the following steps:
1) Selecting a carbon fiber composite material, machining the carbon fiber composite material into a required shape and size to obtain a matrix, and cleaning the surface of the matrix;
2) Preparing and coating a coarse silicon carbide coating adhesive; after the coarse silicon carbide coating adhesive is prepared, the adhesive is mixed according to the proportion of 200-550 g/m 2 Coating the coarse silicon carbide coating glue on the surface of the substrate; after being coated, the mixture is put into an oven and is cured at the constant temperature of 150-300 ℃ for 1.5-3 h;
3) Preparing and coating fine silicon carbide coating glue; after the fine silicon carbide coating adhesive is prepared, 150-450 g/m 2 Coating the fine silicon carbide coating adhesive on the surface of the substrate which is subjected to the primary coating in the step 2) and is cured; after being coated, the mixture is put into an oven and is cured at the constant temperature of 150-300 ℃ for 1.5-3 h;
4) Placing the carbon fiber composite material coated with the coating for 2 times obtained in the step 3) into a carbonization furnace, and carbonizing for 5-7 days at 700-1000 ℃;
5) Placing the carbon fiber composite material carbonized in the step 4) in a vacuum furnace, and graphitizing the carbon fiber composite material at 1700-2200 ℃ for 2-4 days.
The thickness of the coarse silicon carbide coating is 100-300 mu m, and the thickness of the fine silicon carbide coating is 50-100 mu m.
The following examples are carried out on the premise of the technical scheme of the invention, and detailed embodiments and specific operation procedures are given, but the scope of the invention is not limited to the following examples. The methods used in the following examples are conventional methods unless otherwise specified.
[ example 1 ]
In this embodiment, the preparation process of the silicon carbide coating on the surface of the carbon fiber composite material is as follows:
the method comprises the following steps: preparing a carbon fiber composite material, wherein the sizes of experimental plate samples are as follows: length 36.6cm, width 29.8cm, thickness 5.1cm, weight 775g, and density 0.139g/cm 3 . And cleaning the carbon fiber powder on the surface of the plate experiment sample by using a brush for later use.
Step two: and preparing and coating the coarse silicon carbide coating adhesive.
(1) Preparing a matrix solution: and (3) uniformly mixing 30 parts of coarse silicon carbide powder and 8 parts of phenolic resin powder, adding one of the coarse silicon carbide powder and the phenolic resin powder into 50 parts of water, and fully stirring the mixture by using a stirrer until no precipitate is formed to obtain a matrix liquid containing coarse silicon carbide.
(2) Preparing an adhesive: 0.2 part of methyl cellulose was dissolved in 1.6 parts of butyl diglycol, and the mixture was stirred uniformly to obtain an adhesive.
(3) Preparing a coarse silicon carbide coating adhesive: and pouring the adhesive into the matrix liquid containing the crude silicon carbide, stirring while pouring, pouring 20 parts of furan resin into the matrix liquid after stirring until the mixture is uniform, and stopping stirring after a suspension with uniform color is formed to obtain the crude silicon carbide coating adhesive.
And (3) taking the coarse silicon carbide coating adhesive, and brushing the surfaces of the plate test samples according to the brushing quantity of 320 g/square meter. And (3) putting the coated plate experiment sample into an oven, and carrying out primary curing at the constant temperature of 150 ℃ for 1.5 h.
Step three: preparing fine silicon carbide coating glue and coating.
(1) Preparing a matrix solution: and (3) uniformly mixing 30 parts of fine silicon carbide powder and 8 parts of phenolic resin powder, adding 50 parts of water into the mixture, and fully stirring the mixture by using a stirrer until no precipitate is formed to obtain the matrix liquid containing the fine silicon carbide.
(2) Preparing an adhesive: 0.2 part of methyl cellulose was dissolved in 1.6 parts of butyl diglycol, and the mixture was stirred uniformly to obtain an adhesive.
(3) Preparing fine silicon carbide coating adhesive: pouring the adhesive into the matrix liquid containing the fine silicon carbide, stirring while pouring, pouring 20 parts of furan resin into the matrix liquid after stirring uniformly, and stopping stirring after a suspension with uniform color is formed.
Taking fine silicon carbide coating adhesive, and brushing each surface of the plate experiment sample subjected to primary coating curing according to the brushing quantity of 280 g/square meter. And (3) putting the coated plate experiment sample into an oven, and curing at the constant temperature of 150 ℃ for 1.5 h.
Step four: and (3) putting the carbon fiber composite material subjected to coating curing in the third step and the second step into a carbonization furnace, and performing carbonization treatment for 5.5 days at 1000 ℃.
Step five: and (3) placing the carbon fiber composite material subjected to the carbonization treatment in the step four in a vacuum furnace, and carrying out graphitization treatment at 1800 ℃ for 2.5 days.
Effect verification: the silicon carbide coating on the surface of the treated plate experiment sample is smooth and has no crack and powder falling phenomenon; the oxidation resistance test is carried out at 550 ℃, the weight loss is 0.24 percent after the plate is sintered for 8 hours at 550 ℃ in the air, and the experimental sample of the plate without the coating of the comparative example is sintered for 8 hours at 550 ℃ and the weight loss is 5.2 percent.
And (4) conclusion: the carbon fiber composite material provided with the silicon carbide gluing layer can prevent air from directly contacting the surface of the carbon fiber composite material and prevent the carbon fiber composite material from being oxidized and ablated, has excellent oxidation resistance and corrosion resistance, and can obviously prolong the service life of the carbon fiber composite material.
[ example 2 ]
In this embodiment, the preparation process of the silicon carbide coating on the surface of the carbon fiber composite material is as follows:
the method comprises the following steps: preparing a carbon fiber composite material, wherein the sizes of experimental plate samples are as follows: length 36.5cm, width 29.1cm, thickness 5.1cm, weight 748g, density 0.138g/cm 3 . And cleaning the carbon fiber powder on the surface of the plate experiment sample by using a brush for later use.
Step two: and preparing and coating the coarse silicon carbide coating adhesive.
(4) Preparing a matrix solution: uniformly mixing 25 parts of coarse silicon carbide powder and 7 parts of phenolic resin powder, adding one of the coarse silicon carbide powder and 7 parts of phenolic resin powder into 48 parts of water, and fully stirring by using a stirrer until no precipitate is formed to obtain a matrix liquid containing coarse silicon carbide.
(5) Preparing an adhesive: 0.3 part of butyl cellulose is dissolved in 2 parts of butyl diglycol, and the mixture is uniformly stirred to obtain the adhesive.
(6) Preparing a coarse silicon carbide coating adhesive: and pouring the adhesive into the matrix liquid containing the crude silicon carbide, stirring while pouring, pouring 22 parts of furan resin into the matrix liquid after stirring until the mixture is uniform, and stopping stirring after a suspension with uniform color is formed to obtain the crude silicon carbide coating adhesive.
Taking coarse silicon carbide coating adhesive, and brushing each surface of the plate experiment sample according to the brushing quantity of 380 g/square meter. And (3) putting the coated plate experiment sample into an oven, and carrying out primary curing at the constant temperature of 150 ℃ for 3 hours.
Step three: preparing fine silicon carbide coating glue and coating.
(4) Preparing a matrix solution: uniformly mixing 25 parts of fine silicon carbide powder and 7 parts of phenolic resin powder, adding one of the fine silicon carbide powder and 7 parts of phenolic resin powder into 48 parts of water, and fully stirring the mixture by using a stirrer until no precipitate is formed to obtain the matrix liquid containing the fine silicon carbide.
(5) Preparing an adhesive: 0.3 part of methyl cellulose is dissolved in 2 parts of butyl diglycol, and the mixture is uniformly stirred to obtain the adhesive.
(6) Preparing fine silicon carbide coating adhesive: pouring the adhesive into the matrix liquid containing the fine silicon carbide, stirring while pouring, pouring 22 parts of furan resin into the matrix liquid after stirring uniformly, and stopping stirring after a suspension with uniform color is formed.
Taking fine silicon carbide coating adhesive, and brushing each surface of the plate experiment sample subjected to primary coating curing according to the brushing quantity of 220 g/square meter. And (3) putting the coated plate experiment sample into an oven, and curing at the constant temperature of 150 ℃ for 3 h.
Step four: and (3) putting the carbon fiber composite material subjected to coating curing in the third step and the second step into a carbonization furnace, and performing carbonization treatment for 5 days at 800 ℃.
Step five: and (4) placing the carbon fiber composite material subjected to the carbonization treatment in the step four in a vacuum furnace, and carrying out graphitization treatment at 2000 ℃ for 3 days.
Effect verification: the silicon carbide coating on the surface of the treated plate experiment sample is smooth and has no crack and powder falling phenomenon; the oxidation resistance test is carried out at 550 ℃, the weight loss is 0.22 percent after the plate is sintered for 8 hours at 550 ℃ in the air, and the experimental sample of the plate without the coating of the comparative example is sintered for 8 hours at 550 ℃ and the weight loss is 5.4 percent.
And (4) conclusion: the carbon fiber composite material provided with the silicon carbide gluing layer can prevent air from directly contacting the surface of the carbon fiber composite material and prevent the carbon fiber composite material from being oxidized and ablated, has excellent oxidation resistance and corrosion resistance, and can obviously prolong the service life of the carbon fiber composite material.
[ example 3 ] A method for producing a polycarbonate
In this embodiment, the preparation process of the silicon carbide coating on the surface of the carbon fiber composite material is as follows:
the method comprises the following steps: preparing a carbon fiber composite material, wherein the sizes of experimental plate samples are as follows: length 39.4cm, width 35.3cm, thickness 5.0cm, weight 1039g, density 0.149g/cm 3 . And cleaning the carbon fiber powder on the surface of the plate experiment sample by using a brush for later use.
Step two: and preparing and coating the coarse silicon carbide coating adhesive.
(7) Preparing a matrix solution: uniformly mixing 35 parts of coarse silicon carbide powder and 9 parts of phenolic resin powder, adding one of the coarse silicon carbide powder and 9 parts of phenolic resin powder into 55 parts of water, and fully stirring the mixture by using a stirrer until no precipitate is formed to obtain a matrix liquid containing coarse silicon carbide.
(8) Preparing an adhesive: 0.3 part of methyl cellulose and 0.2 part of butyl cellulose were dissolved in 2.4 parts of butyl diglycol, and the mixture was stirred uniformly to obtain an adhesive.
(9) Preparing a coarse silicon carbide coating adhesive: and pouring the adhesive into the matrix liquid containing the crude silicon carbide, stirring while pouring, pouring 25 parts of furan resin into the matrix liquid after stirring uniformly, and stopping stirring after a suspension with uniform color is formed to obtain the crude silicon carbide coating adhesive.
Taking the coarse silicon carbide coating adhesive, and brushing each surface of the plate experiment sample according to the brushing amount of 450 g/square meter. And (3) putting the coated plate experiment sample into an oven, and carrying out primary curing at the constant temperature of 180 ℃ for 2 hours.
Step three: preparing fine silicon carbide coating glue and coating.
(7) Preparing a matrix solution: uniformly mixing 35 parts of fine silicon carbide powder and 9 parts of phenolic resin powder, adding one of the fine silicon carbide powder and 9 parts of phenolic resin powder into 55 parts of water, and fully stirring the mixture by using a stirrer until no precipitate is formed to obtain the matrix liquid containing the fine silicon carbide.
(8) Preparing an adhesive: 0.3 part of methyl cellulose and 0.2 part of butyl cellulose were dissolved in 2.4 parts of butyl diglycol, and the mixture was stirred uniformly to obtain an adhesive.
(9) Preparing fine silicon carbide coating adhesive: pouring the adhesive into the matrix liquid containing the fine silicon carbide, stirring while pouring, pouring 25 parts of furan resin into the matrix liquid after stirring uniformly, and stopping stirring after a suspension with uniform color is formed.
Taking fine silicon carbide coating adhesive, and brushing each surface of the plate experiment sample subjected to primary coating curing according to the brushing quantity of 370 g/square meter. And (3) putting the coated plate experiment sample into an oven, and curing at the constant temperature of 180 ℃ for 2 hours.
Step four: and (3) putting the carbon fiber composite material subjected to coating curing in the third step and the second step into a carbonization furnace, and performing carbonization treatment at 800 ℃ for 6.5 days.
Step five: and (3) placing the carbon fiber composite material subjected to the carbonization treatment in the step four in a vacuum furnace, and carrying out graphitization treatment at 2100 ℃ for 3 days.
Effect verification: the silicon carbide coating on the surface of the treated plate experiment sample is smooth and has no crack and powder falling phenomenon; the oxidation resistance test is carried out at 550 ℃, the weight loss is 0.21 percent after the plate is sintered for 8 hours at 550 ℃ in the air, and the plate test sample without the coating of the comparative example is sintered for 8 hours at 550 ℃ and the weight loss is 5.1 percent.
And (4) conclusion: the carbon fiber composite material provided with the silicon carbide gluing layer can prevent air from directly contacting the surface of the carbon fiber composite material and prevent the carbon fiber composite material from being oxidized and ablated, has excellent oxidation resistance and corrosion resistance, and can obviously prolong the service life of the carbon fiber composite material.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. The silicon carbide coating adhesive for the surface of the carbon fiber composite material is characterized by comprising the following components in percentage by mass: 35-55% of water, 20-40% of silicon carbide powder, 1-10% of phenolic resin, 1-5% of adhesive and 15-30% of furan resin; the adhesive is a solution of methyl cellulose and/or butyl cellulose dissolved in butyl diglycol; the silicon carbide powder is divided into coarse silicon carbide powder and fine silicon carbide powder, the coarse silicon carbide powder is used for preparing coarse silicon carbide coating adhesive, and the fine silicon carbide powder is used for preparing fine silicon carbide coating adhesive; the granularity of the coarse silicon carbide powder is 120-600 meshes, and the granularity of the fine silicon carbide powder is 800-2000 meshes; coating coarse silicon carbide coating glue and fine silicon carbide coating glue on the surface of the carbon fiber composite material in sequence, specifically, coating the coarse silicon carbide coating glue and the fine silicon carbide coating glue on the surface of a substrate in a twice coating mode, wherein the formed coarse silicon carbide coating is used as a transition coating of the carbon fiber composite material and the fine silicon carbide coating; the thickness of the coarse silicon carbide coating is 100-300 mu m, and the thickness of the fine silicon carbide coating is 50-100 mu m.
2. The preparation method of the silicon carbide coating adhesive on the surface of the carbon fiber composite material according to claim 1, which is characterized by comprising the following steps:
(1) Preparing a matrix solution: uniformly mixing silicon carbide powder and phenolic resin powder, adding water into the mixture, and fully stirring until no precipitate is formed to obtain a silicon carbide matrix solution; the coarse silicon carbide powder is selected when the coarse silicon carbide coating adhesive is prepared, and the fine silicon carbide powder is selected when the fine silicon carbide coating adhesive is prepared;
(2) Preparing an adhesive: dissolving one or two of methyl cellulose and butyl cellulose in butyl diglycol, and uniformly stirring to obtain an adhesive;
(3) Preparing silicon carbide coating adhesive: and (3) pouring the adhesive prepared in the step (2) into the silicon carbide matrix liquid prepared in the step (1), stirring while pouring, pouring furan resin for continuously stirring after stirring until the mixture is uniform, and stopping stirring after a suspension with uniform color is formed to obtain the coarse silicon carbide coating adhesive or the fine silicon carbide coating adhesive.
3. The method for preparing the silicon carbide coating adhesive on the surface of the carbon fiber composite material according to claim 2, wherein the water is clean tap water with low hardness.
4. The method for preparing the silicon carbide coating adhesive on the surface of the carbon fiber composite material according to claim 2, wherein in the adhesive, the mass ratio of the cellulose consisting of methyl cellulose and/or butyl cellulose to butyl diglycol is =1:4 to 1:20.
5. the method for preparing the silicon carbide coating adhesive on the surface of the carbon fiber composite material according to claim 2, wherein the particle size of the phenolic resin is 800-2000 meshes, and the residual carbon value is 25-55%.
6. The method for preparing the silicon carbide coating adhesive on the surface of the carbon fiber composite material according to claim 2, wherein the furan resin is furfuryl alcohol resin, furfural-acetone resin or furfural-acetone-formaldehyde resin.
7. The use method of the silicon carbide coating adhesive on the surface of the carbon fiber composite material according to claim 1, which is characterized by comprising the following steps:
1) Selecting a carbon fiber composite material, machining the carbon fiber composite material into a required shape and size to obtain a matrix, and cleaning the surface of the matrix;
2) Preparing a coarse silicon carbide coating adhesive and coating; after the coarse silicon carbide coating adhesive is prepared, the adhesive is mixed according to the proportion of 200-550 g/m 2 Coating the coarse silicon carbide coating glue on the surface of the substrate; after being coated, the mixture is put into an oven and is cured at the constant temperature of 150-300 ℃ for 1.5-3 h;
3) Preparing and coating fine silicon carbide coating glue; after preparing the fine silicon carbide coating adhesive, the method is as follows150～450g/m 2 Coating the fine silicon carbide coating adhesive on the surface of the substrate which is subjected to the primary coating in the step 2) and is cured; after being coated, the mixture is put into an oven and is cured at the constant temperature of 150-300 ℃ for 1.5-3 h;
4) Placing the carbon fiber composite material coated with the coating for 2 times obtained in the step 3) into a carbonization furnace, and carbonizing for 5-7 days at 700-1000 ℃;
5) Placing the carbon fiber composite material carbonized in the step 4) in a vacuum furnace, and graphitizing the carbon fiber composite material at 1700-2200 ℃ for 2-4 days.
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