CN107935614B - Carbon-ceramic composite material and preparation method thereof - Google Patents
Carbon-ceramic composite material and preparation method thereof Download PDFInfo
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- CN107935614B CN107935614B CN201711235448.1A CN201711235448A CN107935614B CN 107935614 B CN107935614 B CN 107935614B CN 201711235448 A CN201711235448 A CN 201711235448A CN 107935614 B CN107935614 B CN 107935614B
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- C04B35/806—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The invention belongs to the field of preparation of carbon-ceramic composite materials, and particularly relates to a carbon-ceramic composite material and a preparation method thereof. Which comprises the following steps: (1) coating bonding slurry on the surface of carbon fiber to obtain pretreated carbon fiber, wherein the bonding slurry is prepared by dissolving a bonding agent in a solvent; (2) preparing ceramic powder containing carbon powder and silicon powder, wherein the molar ratio of silicon to carbon is more than 1: 1; (3) weaving the pretreated carbon fibers to obtain a reticular pretreated carbon fiber preform, and filling the ceramic powder in gaps of the reticular pretreated carbon fiber preform to form a carbon-ceramic composite material preform; (4) and sintering the carbon-ceramic composite material preform to obtain the carbon-ceramic composite material, wherein the obtained carbon-ceramic composite material has better toughness and compressive strength, and has small abrasion loss when used as a friction material.
Description
Technical Field
The invention belongs to the field of preparation of carbon-ceramic composite materials, and particularly relates to a carbon-ceramic composite material and a preparation method thereof.
Background
The carbon-ceramic composite material is a carbon fiber reinforced silicon carbide ceramic composite material, has the characteristics of low density, good oxidation resistance, corrosion resistance and the like, and has the advantages of low density of a carbon disc, stable braking, small abrasion weight loss ratio and the like as a brake material, so that more and more attention and research are drawn in the field of friction materials. The traditional preparation process mainly comprises a chemical vapor deposition method and a liquid immersion method, wherein the chemical vapor deposition method comprises the steps of preparing a carbon disc (weaving carbon fibers into a shape designed by a product), fumigating the carbon disc with hydrogen-containing chlorosilane for many times under a certain temperature condition until densification is achieved, and the method has the advantages of long process period of 2-3 months, high energy consumption and high cost. The liquid dipping method is to prepare a carbon disk and polysilane or polysilane carbon, then permeate polysilane or polycarbosilane into the carbon disk under the protection of vacuum, nitrogen or argon, and then heat treat the carbon disk for many times until densification is achieved. Therefore, the development of a low-cost and fast-forming carbon ceramic composite material preparation method becomes a research hotspot and an important development direction.
The 3D printing technology is an advanced manufacturing technology developed in the later stage of the 80 th 20 th century, and can rapidly manufacture a sample piece, a mold or a model of a new product according to product design data directly, so that the processing period of the product is greatly shortened, and the development cost is reduced. The 3D printing technology is applied to the preparation of the carbon-ceramic composite material, so that the problems in the prior art can be well solved.
To this end, chinese patent document CA106927847A discloses a method and an apparatus for forming a fiber-reinforced ceramic composite material based on a 3D printing technique. The forming method comprises the following steps: (1) continuously supplying the continuous reinforced ceramic fibers to the main printing head, simultaneously supplying the ceramic slurry to the main printing head through a slurry inlet B, and introducing compressed gas from an opening A to provide uniform pressure; (2) the ceramic slurry at the nozzle of the main printing head wraps continuous fibers and is extruded out of the nozzle under the pressure of compressed gas, (3) the initiator is sprayed out of the nozzle of the initiator and is sprayed onto the printed ceramic slurry in a mist state, and the ceramic slurry is solidified under the dual actions of ultraviolet lamp light irradiation and the initiator, so that the current section is printed; (4) after the section of the current layer of the model is finished, the lifting device drives the workbench to descend together for a layering thickness, and the steps are repeated until the parts are finished; (5) and irradiating and curing the printed part under an ultraviolet lamp, and degreasing and sintering the cured part at high temperature to obtain the formed fiber reinforced ceramic matrix composite. The method can obtain fiber reinforced ceramic parts with certain toughness and strength, but the method has poor interfacial bonding capability between continuous fibers and ceramic slurry, the toughness and the strength of the parts are to be improved, and the parts have large abrasion loss as friction materials.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects of poor toughness and compressive strength and large abrasion loss of the carbon-ceramic composite material prepared based on the prior art in the prior art, so that the carbon-ceramic composite material prepared by the method has better toughness and compressive strength and small abrasion loss as a friction material.
The technical scheme of the invention is as follows:
a preparation method of a carbon-ceramic composite material comprises the following steps: (1) coating bonding slurry on the surface of carbon fiber to obtain pretreated carbon fiber, wherein the bonding slurry is prepared by dissolving a bonding agent in a solvent; (2) preparing ceramic powder containing carbon powder and silicon powder, wherein the molar ratio of silicon to carbon is more than 1: 1; (3) weaving the pretreated carbon fibers to obtain a reticular pretreated carbon fiber preform, and filling the ceramic powder in gaps of the reticular pretreated carbon fiber preform to form a carbon-ceramic composite material preform; (4) and sintering the carbon-ceramic composite material preform to obtain the carbon-ceramic composite material.
Weaving the pretreated carbon fibers to obtain a reticular pretreated carbon fiber layer, and filling the ceramic powder in gaps of the pretreated carbon fiber layer to form a carbon-ceramic composite material layer; repeating the operation to obtain the carbon ceramic composite material prefabricated body formed by overlapping a plurality of carbon ceramic composite material layers.
In the step (1), the concentration of the bonding slurry is 5-40% by mass percent, and the binder is one or more of epoxy resin, phenolic resin or modified asphalt.
In the step (1), the solvent is acetone, n-hexane or gasoline.
In the step (4), the sintering temperature is 1500-.
In the step (4), the sintering pressure is 10MPa-200 MPa.
In the step (2), the ceramic powder further comprises a binder which accounts for 2% -5% of the total mass of the ceramic powder.
The ceramic powder also comprises one or more of pure boron, diboron trioxide or boric acid, wherein the boron accounts for 1-3% of the total mass of the ceramic powder.
The carbon powder in the ceramic powder is one or more of activated carbon, tar pitch, furan resin, phenolic resin or carbon black.
The silicon powder in the ceramic powder is polycrystalline silicon powder.
The preparation method is a 3D printing method, and comprises the steps of (1) continuously supplying the pretreated carbon fibers to at least one printing head, and simultaneously continuously supplying the ceramic powder to the rest printing heads; (2) according to a set program, the printing heads eject the pretreated carbon fibers, a reticular pretreated carbon fiber preform is obtained by weaving, and the rest printing heads fill the ceramic powder in the gaps of the reticular pretreated carbon fiber preform, so that the carbon-ceramic composite material preform is printed; (3) and sintering the carbon-ceramic composite material preform to obtain the carbon-ceramic composite material.
The step (2) comprises the steps that according to a set program, the printing heads eject the pretreated carbon fibers and are woven to obtain a reticular pretreated carbon fiber layer, and the rest of the printing heads fill the ceramic powder in gaps of the reticular pretreated carbon fibers, so that the pretreated carbon fiber layer filled with the ceramic powder, namely the carbon-ceramic composite material layer, is printed; repeating the operation to obtain the carbon ceramic composite material prefabricated body formed by overlapping a plurality of carbon ceramic composite material layers.
A carbon-ceramic composite material prepared by the preparation method of the carbon-ceramic composite material.
The technical scheme of the invention has the following advantages:
1. the preparation method of the carbon ceramic composite material comprises the steps of coating bonding slurry on the surface of carbon fiber to obtain pretreated carbon fiber, wherein the molar ratio of silicon to carbon in ceramic powder is larger than 1:1, the bonding slurry is coated on the surface of the carbon fiber, so that the process operability of carbon fiber weaving forming is improved, the binder in the bonding slurry on the surface of the carbon fiber is carbonized in the sintering process of the step (4), the carbonized carbon content of the binder is 45-65%, and the carbonized binder can react with excessive silicon powder in the ceramic powder, so that the chemical bonding of the interface between the carbon fiber and the ceramic powder is strengthened, and the toughness, compressive strength and wear resistance of the carbon ceramic composite material are improved.
2. According to the preparation method of the carbon-ceramic composite material, the ceramic powder also comprises the binder, the binder has high carbon content after carbonization, and carbon reacts with redundant silicon, so that the interface chemical bonding between the carbon fiber and the silicon carbide ceramic is improved.
3. According to the preparation method of the carbon-ceramic composite material, provided by the invention, pure boron, diboron trioxide or boric acid is added into the ceramic powder, so that the sintering temperature can be reduced, and the production is facilitated; on the other hand, in the sintering process, pure boron can be generated from the diboron trioxide and the boric acid, and can react with the carbonized carbon adhered to the surface of the carbon fiber, so that the bonding strength between the carbon fiber and the ceramic powder is improved, and the folding resistance, the compressive strength and the wear resistance of the product are further improved.
4. According to the preparation method of the carbon-ceramic composite material, the carbon powder in the ceramic powder is selected from one or more of activated carbon, tar pitch, furan resin, phenolic resin or carbon black, and the carbon powder has the characteristics of high activity and high carbon content, so that the sintering temperature can be reduced, the production is convenient, the bonding strength between the carbon powder and the silicon powder can be increased, and the toughness, compressive strength and wear resistance of the carbon-ceramic composite material are improved.
5. According to the preparation method of the carbon-ceramic composite material, the carbon powder and the silicon powder in the slurry are uniformly distributed in the gaps of the reticular pretreated carbon fiber layer, so that the carbon powder and the silicon powder can fully react in the sintering process to obtain uniformly distributed silicon carbide, and further the carbon-ceramic composite material with good uniformity is obtained.
6. According to the preparation method of the carbon ceramic composite material, the carbon ceramic material is prepared by adopting a 3D printing technology, the number of the 3D printing heads is increased along with the upgrading of 3D printing equipment and the improvement of command execution speed, and the processing period is greatly shortened.
7. The preparation method of the carbon-ceramic composite material provided by the invention adopts cheap carbon powder and silicon powder which can react at high temperature to generate silicon carbide, so that the production cost is reduced.
8. According to the preparation method of the carbon-ceramic composite material, the carbon-ceramic material is prepared by adopting a 3D printing technology, the setting program of a 3D printer can be set according to actual production needs, the size, the weaving sequence and the shape of the pores in the obtained reticular pretreated carbon fiber preform are set, and different carbon-ceramic composite materials are further obtained.
9. The structure of the carbon-ceramic composite material obtained by the invention has better designability and uniformity.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The manufacturer of the polycrystalline silicon powder is Shanghai oil-blown powder material Co.
Example 1
Pretreatment of carbon fibers: dissolving epoxy resin in an acetone solution to obtain bonding slurry with the mass fraction of 5%, and soaking carbon fibers in the bonding slurry to obtain the pretreated carbon fibers.
Preparing ceramic powder: 308g of polycrystalline silicon powder is made into silicon powder particles, and 122g of activated carbon is uniformly mixed.
Inputting a set program in an operating system of a 3D printer, continuously supplying pretreated carbon fibers to a printing head, weaving the pretreated carbon fibers sprayed by the printing head according to the set program to obtain a reticular pretreated carbon fiber layer, continuously supplying ceramic powder to another printing head, filling the ceramic powder in gaps of the reticular pretreated carbon fiber layer by the printing head according to the set program, printing the pretreated carbon fiber layer filled with the ceramic powder, namely a carbon ceramic composite material layer, lowering the two printing heads and the lifting device together by a layered thickness by the lifting device with the worktable after finishing one layer, repeatedly operating the two printing heads and the lifting device to obtain a plurality of carbon ceramic composite material layers which are overlapped, fixing the plurality of carbon ceramic composite material layers which are overlapped in a sewing way to obtain a carbon ceramic composite material preform, and putting the carbon ceramic composite material preform into a graphite mold, and putting the graphite mould into a vacuum high-temperature sintering furnace, preserving the heat for 30min under the conditions of 1500 ℃ and 200MPa under the protection of argon, wherein the carbon content of the carbonized epoxy resin is 50 percent under the conditions, removing the pressure, and taking out the obtained carbon-ceramic composite material when the temperature of the vacuum high-temperature sintering furnace is reduced to below 200 ℃.
Example 2
Pretreatment of carbon fibers: dissolving phenolic resin in 500ml of normal hexane solution to obtain bonding slurry with the mass fraction of 40%, and soaking carbon fibers in the bonding slurry to obtain pretreated carbon fibers.
Preparing ceramic powder: 364g of polycrystalline silicon powder is prepared into silicon powder particles, 74g of tar pitch and 50g of carbon black are mixed uniformly.
Inputting a set program in an operating system of a 3D printer, continuously supplying pretreated carbon fibers to a printing head, driving the pretreated fibers to weave according to the set program by the printing head to obtain a reticular pretreated fiber layer, continuously supplying ceramic powder to another printing head, filling the ceramic powder in gaps of the reticular pretreated carbon fiber layer by the printing head according to the set program, printing the pretreated carbon fiber layer filled with the ceramic powder, namely a carbon ceramic composite material layer, lowering the working platform by a layered thickness by a lifting device together after one layer is finished, repeatedly operating the two printing heads and the lifting device to obtain a plurality of carbon ceramic composite material layers which are overlapped, fixing the plurality of carbon ceramic composite material layers which are overlapped in a sewing mode to obtain a carbon ceramic composite material preform, putting the carbon ceramic composite material preform into a graphite mold, and putting the graphite mold into a vacuum high-temperature sintering furnace, and (3) preserving the heat for 3 hours at the temperature of 1800 ℃ and the pressure of 150MPa under the protection of argon, removing the pressure after the carbon content of the phenolic resin is 65 percent after the phenolic resin is carbonized under the conditions, and taking out the obtained carbon-ceramic composite material when the temperature of the vacuum high-temperature sintering furnace is reduced to be below 200 ℃.
Example 3
Pretreatment of carbon fibers: and dissolving the modified asphalt in 500ml of gasoline solution to obtain bonding slurry with the mass fraction of 10%, and soaking the carbon fibers in the bonding slurry to obtain the pretreated carbon fibers.
Preparing ceramic powder: 336g of polycrystalline silicon powder is prepared into silicon powder particles, 120g of carbon black and 14g of modified asphalt are mixed uniformly and granulated.
Inputting a set program in an operating system of a 3D printer, continuously supplying pretreated carbon fibers to a printing head, driving the pretreated fibers to weave according to the set program by the printing head to obtain a reticular pretreated fiber layer, continuously supplying ceramic powder to another printing head, filling the ceramic powder in gaps of the reticular pretreated carbon fiber layer by the printing head according to the set program, printing the pretreated carbon fiber layer filled with the ceramic powder, namely a carbon ceramic composite material layer, lowering the working platform by a layered thickness by a lifting device together after one layer is finished, repeatedly operating the two printing heads and the lifting device to obtain a plurality of carbon ceramic composite material layers which are overlapped, fixing the plurality of carbon ceramic composite material layers which are overlapped in a sewing mode to obtain a carbon ceramic composite material preform, putting the carbon ceramic composite material preform into a graphite mold, and putting the graphite mold into a vacuum high-temperature sintering furnace, and (3) under the protection of argon, keeping the temperature for 1h under the conditions that the temperature is 1560 ℃ and the pressure is 30MPa, removing the pressure until the carbon content of the carbonized modified asphalt is 60%, and taking out the obtained carbon-ceramic composite material when the temperature of the vacuum high-temperature sintering furnace is reduced to below 200 ℃.
Example 4
Pretreatment of carbon fibers: and dissolving the modified asphalt in 500ml of gasoline solution to obtain bonding slurry with the mass fraction of 30%, and soaking the carbon fibers in the bonding slurry to obtain the pretreated carbon fibers.
Preparing ceramic powder: 294g of polycrystalline silicon powder is prepared into silicon powder particles, 120g of carbon black and 8.5g of epoxy resin are mixed uniformly and granulated.
Inputting a set program in an operating system of a 3D printer, continuously supplying pretreated carbon fibers to a printing head, driving the pretreated fibers to weave according to the set program by the printing head to obtain a reticular pretreated fiber layer, continuously supplying ceramic powder to another printing head, filling the ceramic powder in gaps of the reticular pretreated carbon fiber layer by the printing head according to the set program, printing the pretreated carbon fiber layer filled with the ceramic powder, namely a carbon ceramic composite material layer, lowering the working platform by a layered thickness by a lifting device together after one layer is finished, repeatedly operating the two printing heads and the lifting device to obtain a plurality of carbon ceramic composite material layers which are overlapped, fixing the plurality of carbon ceramic composite material layers which are overlapped in a sewing mode to obtain a carbon ceramic composite material preform, putting the carbon ceramic composite material preform into a graphite mold, and putting the graphite mold into a vacuum high-temperature sintering furnace, keeping the temperature at 1780 ℃ and the pressure at 180MPa for 2.5h, removing the pressure until the carbon content of the carbonized modified asphalt is 55%, and taking out the obtained carbon-ceramic composite material when the temperature of the vacuum high-temperature sintering furnace is reduced to below 200 ℃.
Example 5
Pretreatment of carbon fibers: and dissolving the modified asphalt in 500ml of gasoline solution to obtain bonding slurry with the mass fraction of 10%, and soaking the carbon fibers in the bonding slurry to obtain the pretreated carbon fibers.
Preparing ceramic powder: 336g of polycrystalline silicon powder is prepared into silicon powder particles, 120g of carbon black, 24.3g of modified asphalt and 9.8g of boron are mixed uniformly and granulated.
Inputting a set program in an operating system of a 3D printer, continuously supplying pretreated carbon fibers to a printing head, driving the pretreated fibers to weave according to the set program by the printing head to obtain a reticular pretreated fiber layer, continuously supplying ceramic powder to another printing head, filling the ceramic powder in gaps of the reticular pretreated carbon fiber layer by the printing head according to the set program, printing the pretreated carbon fiber layer filled with the ceramic powder, namely a carbon ceramic composite material layer, lowering the working platform by a layered thickness by a lifting device together after one layer is finished, repeatedly operating the two printing heads and the lifting device to obtain a plurality of carbon ceramic composite material layers which are overlapped, fixing the plurality of carbon ceramic composite material layers which are overlapped in a sewing mode to obtain a carbon ceramic composite material preform, putting the carbon ceramic composite material preform into a graphite mold, and putting the graphite mold into a vacuum high-temperature sintering furnace, keeping the temperature at 1560 ℃ and the pressure at 30MPa for 1h, removing the pressure, and taking out the obtained carbon-ceramic composite material when the temperature of the vacuum high-temperature sintering furnace is reduced to below 200 ℃ after the carbon content of the modified asphalt carbonized under the conditions is 60%.
Example 6
Pretreatment of carbon fibers: dissolving epoxy resin in an acetone solution to obtain bonding slurry with the mass fraction of 5%, and soaking carbon fibers in the bonding slurry to obtain the pretreated carbon fibers.
Preparing ceramic powder: 308g of polycrystalline silicon powder is made into silicon powder particles, and 122g of activated carbon is uniformly mixed.
Inputting a set program in an operating system of a 3D printer, continuously supplying pretreated carbon fibers to a printing head, driving the pretreated fibers to weave according to the set program by the printing head to obtain a reticular pretreated fiber layer, continuously supplying ceramic powder to another printing head, filling the ceramic powder in gaps of the reticular pretreated carbon fiber layer by the printing head according to the set program, printing the pretreated carbon fiber layer filled with the ceramic powder, namely a carbon ceramic composite material layer, lowering the working platform by a layered thickness by a lifting device together after one layer is finished, repeatedly operating the two printing heads and the lifting device to obtain a plurality of carbon ceramic composite material layers which are overlapped, fixing the plurality of carbon ceramic composite material layers which are overlapped in a sewing mode to obtain a carbon ceramic composite material preform, putting the carbon ceramic composite material preform into a graphite mold, and putting the graphite mold into a vacuum high-temperature sintering furnace, and (3) under the protection of argon, keeping the temperature at 1500 ℃ for 30min, removing the pressure until the carbon content of the carbonized epoxy resin is 50%, and taking out the obtained carbon-ceramic composite material when the temperature of the vacuum high-temperature sintering furnace is reduced to below 200 ℃.
Example 7
Pretreatment of carbon fibers: and dissolving the modified asphalt in 500ml of gasoline solution to obtain bonding slurry with the mass fraction of 10%, and soaking the carbon fibers in the bonding slurry to obtain the pretreated carbon fibers.
Preparing ceramic powder: 336g of polycrystalline silicon powder is prepared into silicon powder particles, 120g of carbon black, 24.3g of modified asphalt and 9.8g of boron are mixed uniformly and granulated.
Inputting a set program in an operating system of a 3D printer, continuously supplying the pretreated carbon fiber to one printing head, weaving the pretreated carbon fiber ejected by the printing head according to the set program to obtain a reticular carbon fiber preform, continuously supplying the ceramic powder to the other printing head, filling the ceramic powder in gaps of the reticular carbon fiber preform by the printing head according to the set program, printing the carbon ceramic composite preform, putting the carbon ceramic composite preform into a graphite mold, putting the graphite mold into a vacuum high-temperature sintering furnace, preserving heat for 1h under the conditions that the temperature is 1560 ℃ and the pressure is 10MPa, removing the pressure, and taking out the obtained carbon ceramic composite when the temperature of the vacuum high-temperature sintering furnace is reduced to below 200 ℃.
Example 8
Pretreatment of carbon fibers: and dissolving the modified asphalt in 500ml of gasoline solution to obtain bonding slurry with the mass fraction of 10%, and soaking the carbon fibers in the bonding slurry to obtain the pretreated carbon fibers.
Preparing ceramic powder: 336g of polycrystalline silicon powder is prepared into silicon powder particles, 120g of carbon black, 24.8g of modified asphalt and 14.8g of boron are mixed uniformly and granulated.
Weaving the pretreated carbon fibers to obtain a reticular pretreated carbon fiber layer, filling ceramic powder in gaps of the pretreated carbon fiber layer to form a carbon-ceramic composite material layer, repeatedly weaving and filling to obtain a carbon-ceramic composite material prefabricated body formed by overlapping a plurality of carbon-ceramic composite materials, putting the carbon-ceramic composite material prefabricated body into a graphite mold, putting the graphite mold into a vacuum high-temperature sintering furnace, preserving heat for 0.5h under the conditions of 1560 ℃ and 30MPa, removing the pressure, and taking out the obtained carbon-ceramic composite material when the temperature of the vacuum high-temperature sintering furnace is reduced to below 200 ℃.
Example 9
Pretreatment of carbon fibers: dissolving phenolic resin in 500ml of normal hexane solution to obtain bonding slurry with the mass fraction of 40%, and soaking carbon fibers in the bonding slurry to obtain pretreated carbon fibers.
Preparing ceramic powder: 364g of polycrystalline silicon powder is made into silicon powder particles, and 277g of tar pitch is uniformly mixed.
Weaving the pretreated carbon fibers to obtain a reticular pretreated carbon fiber layer, filling ceramic powder in gaps of the pretreated carbon fiber layer to form a carbon-ceramic composite material layer, repeatedly weaving and filling to obtain a carbon-ceramic composite material prefabricated body formed by overlapping a plurality of layers of carbon-ceramic composite materials, putting the carbon-ceramic composite material prefabricated body into a graphite mold, putting the graphite mold into a vacuum high-temperature sintering furnace, keeping the temperature at 1800 ℃ and the pressure at 30MPa for 0.5h, removing the pressure, and taking out the obtained carbon-ceramic composite material when the temperature of the vacuum high-temperature sintering furnace is reduced to below 200 ℃.
Comparative example 1
The preparation method in embodiment 3 of Chinese patent document CA106927847A is adopted to prepare the carbon fiber reinforced silicon carbide ceramic composite material, wherein the ceramic powder is silicon carbide powder, and the continuous reinforced fiber is carbon fiber.
Experimental example 1
The carbon-ceramic composites obtained in examples 1 to 6 and comparative examples were tested and the results are shown in table 1:
TABLE 1
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (13)
1. The preparation method of the carbon-ceramic composite material is characterized by comprising the following steps:
(1) coating bonding slurry on the surface of carbon fiber to obtain pretreated carbon fiber, wherein the bonding slurry is prepared by dissolving a bonding agent in a solvent;
(2) preparing ceramic powder containing carbon powder and silicon powder, wherein the molar ratio of silicon to carbon is more than 1: 1;
(3) weaving the pretreated carbon fibers to obtain a reticular pretreated carbon fiber preform, and filling the ceramic powder in gaps of the reticular pretreated carbon fiber preform to form a carbon-ceramic composite material preform;
(4) and sintering the carbon-ceramic composite material preform to obtain the carbon-ceramic composite material.
2. The preparation method of the carbon-ceramic composite material as claimed in claim 1, wherein the step (3) comprises weaving the pretreated carbon fibers to obtain a reticular pretreated carbon fiber layer, and filling the ceramic powder in gaps of the pretreated carbon fiber layer to form the carbon-ceramic composite material layer; repeating the operation to obtain the carbon ceramic composite material prefabricated body formed by overlapping a plurality of carbon ceramic composite material layers.
3. The preparation method of the carbon-ceramic composite material as claimed in claim 1, wherein in the step (1), the concentration of the bonding slurry is 5-40% by mass, and the binder is one or more of epoxy resin, phenolic resin or modified asphalt.
4. The preparation method of the carbon-ceramic composite material as claimed in claim 3, wherein in the step (1), the solvent is acetone, n-hexane or gasoline.
5. The method for preparing a carbon-ceramic composite material as claimed in any one of claims 1 to 4, wherein the sintering temperature in the step (4) is 1500-.
6. A preparation method of carbon-ceramic composite material according to claim 5, wherein in the step (4), the sintering pressure is 10MPa-200 MPa.
7. A preparation method of a carbon-ceramic composite material as claimed in any one of claims 1 to 4, wherein in the step (2), the ceramic powder further comprises a binder accounting for 2-5% of the total mass of the ceramic powder.
8. A preparation method of a carbon-ceramic composite material as claimed in any one of claims 1 to 4, wherein the ceramic powder further comprises one or more of pure boron, diboron trioxide and boric acid, wherein boron accounts for 1 to 3 percent of the total mass of the ceramic powder.
9. A preparation method of a carbon-ceramic composite material as claimed in any one of claims 1 to 4, wherein the carbon powder in the ceramic powder is one or more of activated carbon, tar pitch, furan resin, phenolic resin or carbon black.
10. A preparation method of a carbon-ceramic composite material as claimed in any one of claims 1 to 4, wherein the silicon powder in the ceramic powder is polycrystalline silicon powder.
11. A method of preparing a carbon-ceramic composite material according to any one of claims 1 to 4, wherein the preparation method is a 3D printing method comprising,
(1) the pretreated carbon fibers are continuously supplied to at least one printing head, and meanwhile, the ceramic powder is continuously supplied to the rest printing heads;
(2) according to a set program, the printing heads eject the pretreated carbon fibers, a reticular pretreated carbon fiber preform is obtained by weaving, and the rest printing heads fill the ceramic powder in the gaps of the reticular pretreated carbon fiber preform, so that the carbon-ceramic composite material preform is printed;
(3) and sintering the carbon-ceramic composite material preform to obtain the carbon-ceramic composite material.
12. The preparation method of the carbon-ceramic composite material as claimed in claim 11, wherein the step (2) comprises the steps of ejecting the pretreated carbon fibers by the printing heads according to a set program, weaving to obtain a reticular pretreated carbon fiber layer, and filling the ceramic powder in gaps of the reticular pretreated carbon fibers by the rest of the printing heads, so as to print the pretreated carbon fiber layer filled with the ceramic powder, namely the carbon-ceramic composite material layer; repeating the operation to obtain the carbon ceramic composite material prefabricated body formed by overlapping a plurality of carbon ceramic composite material layers.
13. A carbon-ceramic composite material prepared by the method of any one of claims 1 to 12.
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| CN201711235448.1A CN107935614B (en) | 2017-11-30 | 2017-11-30 | Carbon-ceramic composite material and preparation method thereof |
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| CN107128914B (en) * | 2017-07-04 | 2019-04-09 | 陕西师范大学 | The preparation method of petroleum coke pilum shaped activated carbon |
| FR3093153B1 (en) * | 2019-02-27 | 2022-08-12 | Valeo Materiaux De Friction | Additive manufacturing process of a friction lining |
| CN110557853B (en) * | 2019-07-18 | 2022-08-09 | 武汉纺织大学 | Method for manufacturing high-temperature sintered body capable of generating heat by electrifying, product and application method |
| CN110423119B (en) * | 2019-08-07 | 2020-09-01 | 航天特种材料及工艺技术研究所 | Preparation method of ablation-resistant C/SiC ceramic matrix composite |
| CN110509537B (en) * | 2019-08-09 | 2021-01-29 | 北京航空航天大学 | 3D printing method for fiber reinforced composite material with matrix material filling fiber gaps |
| CN111285700A (en) * | 2020-01-07 | 2020-06-16 | 山东理工大学 | Preparation method of zirconium carbide film carbon fiber-ceramic friction material |
| CN111285690A (en) * | 2020-01-07 | 2020-06-16 | 山东理工大学 | Preparation method of titanium carbide film carbon fiber-ceramic friction material |
| CN111285689A (en) * | 2020-01-07 | 2020-06-16 | 山东理工大学 | Preparation method of boron carbide film carbon fiber-ceramic friction material |
| CN111285701A (en) * | 2020-01-07 | 2020-06-16 | 山东理工大学 | Preparation method of silicon carbide film carbon fiber-ceramic friction material |
| CN111377749A (en) * | 2020-02-24 | 2020-07-07 | 哈尔滨工业大学 | Method for realizing transportation of ceramic slurry in carbon fiber woven body by imitating transpiration effect |
| CN111635241B (en) * | 2020-06-15 | 2021-07-13 | 西安交通大学 | Additive manufacturing method of silicon carbide ceramic matrix composite structure/functional part |
| CN114621020B (en) * | 2022-05-16 | 2022-10-14 | 浙江德鸿碳纤维复合材料有限公司 | Carbon-ceramic composite structure and preparation method thereof |
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| CN100532329C (en) * | 2006-05-25 | 2009-08-26 | 南京航空航天大学 | Preparation method of carbon-silicon carbide base composite material toughened by carbon fiber |
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| US10035305B2 (en) * | 2015-06-30 | 2018-07-31 | Honeywell International Inc. | Method of making carbon fiber preforms |
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