CN113698221A - Preparation method of modified carbon fiber toughened silicon carbide ceramic material and modified carbon fiber toughened silicon carbide ceramic material - Google Patents
Preparation method of modified carbon fiber toughened silicon carbide ceramic material and modified carbon fiber toughened silicon carbide ceramic material Download PDFInfo
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Abstract
The invention provides a preparation method of a modified carbon fiber toughened silicon carbide ceramic material. The invention also provides a modified carbon fiber toughened silicon carbide ceramic material, which comprises silicon carbide and modified carbon fibers dispersed in the silicon carbide, wherein the modified carbon fibers comprise carbon fibers, and a graphene oxide layer, an aluminum oxide layer and a SiC layer which are sequentially coated outside the carbon fibers from inside to outside. According to the silicon carbide ceramic material provided by the invention, the carbon fibers of the graphene oxide layer, the aluminum oxide layer and the SiC layer which are sequentially coated from inside to outside are utilized for toughening, and the multi-layer protection structure greatly improves the oxidation resistance of the carbon fibers, so that the toughness of the silicon carbide ceramic material is greatly improved.
Description
Technical Field
The invention belongs to the field of new materials, and particularly relates to a preparation method of a modified carbon fiber toughened silicon carbide ceramic material and the modified carbon fiber toughened silicon carbide ceramic material.
Background
Silicon carbide is used as an important structural ceramic material, and by virtue of excellent high-temperature mechanical strength, high hardness, high elastic modulus, high wear resistance, high thermal conductivity, corrosion resistance and other properties, the silicon carbide is not only applied to the traditional industrial fields of high-temperature kiln furniture, combustion nozzles, heat exchangers, sealing rings, sliding bearings and the like, but also can be used as a bulletproof armor material, a space reflector, a clamp material in semiconductor wafer preparation and a nuclear fuel cladding material.
Silicon carbide materials have properties such as high hardness, wear resistance, and high elastic modulus, which are largely determined by their high covalent bonding and stable crystal structure. The silicon carbide has two crystal structures of beta and alpha, beta-SiC is a face-centered cubic sphalerite structure, and alpha-SiC is a hexagonal wurtzite structure. The alpha-SiC derives 2H, 4H, 6H, 15R and other polytypes due to different stacking modes of the structural unit layers, wherein the 6H polytype is the most widely applied in industry. Although SiC exists in many polytypes and has varying lattice constants, its densities are very close. The density of the beta-SiC is 3.215g/cm3The densities of the various alpha-SiC variants were essentially the same, 3.217g/cm3. beta-SiC, commonly referred to as "low temperature modification", is a metastable phase at room temperature that converts to one or more polytypes of alpha-SiC at temperatures above 2100 ℃ and the conversion is irreversible. The 15R variant is thermodynamically less stable, is the mesophase generated when the β -SiC → 6H-SiC conversion occurs, and is absent at high temperatures. In addition, SiC synthesized at 2000 ℃ or lower in the production of silicon carbide powder is mainly β -type, while SiC synthesized at 2200 ℃ or higher is mainly α -SiC and mainly 6H.
The concept of fiber reinforced ceramic matrix composites was first introduced in the early 70 s of the 20 th century and was proposed by j. The appearance of the ceramic material opens up a new field for the research and development of high-performance ceramic materials. In a plurality of reinforcing phases of the fiber reinforced ceramic matrix composite, the carbon fiber has a series of advantages of high specific modulus, high specific strength, corrosion resistance, fatigue resistance, creep resistance, good electrical conductivity, high thermal conductivity, low expansion, excellent high-temperature performance under the condition of non-oxidizing medium and the like. As a reinforcing phase, the carbon fiber can endow the composite material with toughness and impact resistance, improve the inherent brittleness weakness of the ceramic matrix and simultaneously retain good mechanical properties of the ceramic matrix. In the carbon fiber-reinforced ceramic matrix composite, Cfthe/SiC composite material has low density (1.7-2.5 g/cm)3) High modulus (>100GPa), high strength (tensile strength)>350MPa and bending strength>500MPa (fabric reinforcement) and low thermal expansion coefficient (1.8-4.1 x 10)-6/° c (20-1000 ℃)), high thermal shock resistance (2100 ℃/s), and good chemical corrosion resistance, and are materials that are most likely to be applied in high temperature environments. In addition, CfThe matrix of the/SiC composite material has relatively good oxidation resistance and is considered to be secondary CfThe new strategic material behind the/C composite material is the technical key for improving the performance of the existing weaponry and developing future advanced weaponry, and developed countries are competitive in development.
The untreated carbon fiber has poor wettability, low reactivity and high inertness on the surface, which leads to poor interfacial properties between the untreated carbon fiber and a matrix, so that the carbon fiber needs to be subjected to surface modification to improve the interfacial properties of the composite material.
Disclosure of Invention
The technical problem is as follows: in order to overcome the defects of the prior art, the invention provides a preparation method of a modified carbon fiber toughened silicon carbide ceramic material and the modified carbon fiber toughened silicon carbide ceramic material.
The technical scheme is as follows: the invention provides a preparation method of a modified carbon fiber toughened silicon carbide ceramic material, which comprises the following steps:
(1) oxidizing the surface of the carbon fiber, grafting graphene oxide on the surface of the carbon fiber by adopting a silane coupling agent, coating a polycarbosilane precursor solution on the surface of the carbon fiber modified by the graphene oxide, and curing and pyrolyzing at high temperature to form the graphene oxide modified carbon fiber;
(2) introducing the graphene oxide modified carbon fiber into a fluidized bed reactor, pyrolyzing the secondary butyl aluminum in the fluidized bed reactor into aluminum oxide by taking argon as a carrier gas and secondary butyl aluminum as an aluminum source, and depositing on the surface of the graphene oxide modified carbon fiber to form the graphene oxide modified carbon fiber coated with the aluminum oxide;
(3) depositing a SiC layer on the surface of a base material by using a chemical vapor deposition method by using alumina-coated graphene oxide modified carbon fiber as the base material and trichloromethylsilane, hydrogen and argon as gas sources to form modified carbon fiber;
(4) mixing silicon carbide powder with the particle size of 45-75 microns, modified carbon fiber and sintering aid, adding the mixture into a ball mill, and adding phenolic resin, graphite powder and deionized water for ball milling;
(5) placing the slurry obtained after ball milling into a vacuum pressure tank, performing vacuum treatment, and injecting into a mold for dry pressing molding; curing for 6-12h at 50-90 ℃;
(6) in a vacuum furnace, in an inert atmosphere, heating to 1400 ℃ and 1500 ℃ at the heating rate of 5-10 ℃/min, and carrying out heat preservation sintering for 2-6 h; and cooling along with the furnace to obtain the modified carbon fiber toughened silicon carbide ceramic material.
In the step (1), the surface oxidation treatment method for the carbon fiber comprises the following steps: immersing the carbon fiber in acetone, and heating and refluxing for 10-15 h; immersing in concentrated nitric acid at 30-90 deg.C for 1-3h after drying, taking out, washing, and drying; the method for grafting the graphene oxide comprises the following steps: dispersing graphene oxide and a silane coupling agent in an ethanol solvent, immersing oxidized carbon fibers in the solution, taking out and drying, wherein the use amount of the carbon fibers, the graphene oxide, the silane coupling agent and the ethanol is 1 g: (2-4) g: (6-8) g: (400- > 600) ml; the silane coupling agent is gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane or N-beta (aminoethyl) -gamma-aminopropyltriethoxysilane; the curing temperature is 100-; the high-temperature cracking temperature is 1200 ℃ and 1400 ℃, and the high-temperature cracking time is 1-2 h.
In the step (1), the preparation method of the polycarbosilane precursor solution comprises the following steps:
(a) uniformly dispersing nano boehmite in an aqueous solution of KH550, and ultrasonically oscillating for 0.5-2 hours to obtain a mixture 1;
(b) distilling polydimethylsiloxane PDMS, collecting the fraction at 103 ℃, and drying; and then dropwise adding an organic solvent into the mixture and continuously stirring until the mass ratio of the organic solvent to the polydimethylsiloxane PDMS is (5-15): 100, denoted as solution 2;
(c) pouring the mixture 1 into the solution 2, heating in water bath at 60-80 ℃, and stirring for 2-6 hours to obtain a mixture 3;
(d) putting the mixture 3 into a reaction kettle, introducing mixed gas of CO2 and inert gas, and pressurizing to 5-10 MPa; heating to 500-520 ℃ according to a certain heating program, and preserving heat for 12-24 hours; cooling to room temperature along with the furnace to obtain a crude product 4;
(e) and (3) dissolving the crude product 4 in an organic solvent to obtain a polycarbosilane precursor solution, wherein the mass percentage content of the polycarbosilane precursor solution is 60-70%.
In the step (2), the temperature of the pyrolysis reaction temperature zone of the secondary aluminum butoxide is 200-3/h。
In the step (3), the SiC deposition conditions are as follows: the deposition temperature is 900 ℃ and 1200 ℃, and the deposition pressure is 5-10mm Hg; the flow rate of trichloromethylsilane is 80-100g/h, and the flow rate of hydrogen is 0.1-0.2m3H, argon flow of 0.1-0.2m3H; after a period of deposition, the mixture is turned over and deposited again, wherein the deposition time is 10-20h each time, and the deposition is carried out for 2 times or 4 times.
In the step (4), the mass ratio of the silicon carbide powder, the modified carbon fiber, the sintering aid, the phenolic resin, the graphite powder and the deionized water is (60-70): (5-15): (2-4): (4-10): (2-4): 1000, parts by weight; the ball milling speed is 150-.
In the step (5), the dry pressing method comprises the following steps: placing the mold filled with the slurry at 50-90 deg.C and 80-100MPa, and unidirectionally pressurizing for 1-3 min; and inverting the mold, and continuously pressurizing in one direction at 50-90 deg.C and 80-100MPa for 1-3 min.
In the step (6), the vacuum degree in the vacuum furnace is 2-9 KPa.
The invention also provides the modified carbon fiber toughened silicon carbide ceramic material prepared by the method.
The invention also provides a modified carbon fiber toughened silicon carbide ceramic material, which comprises silicon carbide and modified carbon fibers dispersed in the silicon carbide, wherein the modified carbon fibers comprise carbon fibers, and a graphene oxide layer, an aluminum oxide layer and a SiC layer which are sequentially coated outside the carbon fibers from inside to outside.
Has the advantages that: according to the silicon carbide ceramic material provided by the invention, the carbon fibers of the graphene oxide layer, the aluminum oxide layer and the SiC layer which are sequentially coated from inside to outside are utilized for toughening, and the multi-layer protection structure greatly improves the oxidation resistance of the carbon fibers, so that the toughness of the silicon carbide ceramic material is greatly improved.
Detailed Description
The present invention is further explained below.
Example 1
The preparation method of the modified carbon fiber toughened silicon carbide ceramic material comprises the following steps:
(1) oxidizing the surface of the carbon fiber, grafting graphene oxide on the surface of the carbon fiber by adopting a silane coupling agent, coating a polycarbosilane precursor solution on the surface of the carbon fiber modified by the graphene oxide, and curing and pyrolyzing at high temperature to form the graphene oxide modified carbon fiber;
the method for oxidizing the surface of the carbon fiber comprises the following steps: immersing the carbon fiber in acetone, and heating and refluxing for 12 h; immersing in concentrated nitric acid at 60 ℃ for 2h after drying, taking out, washing and drying; the method for grafting the graphene oxide comprises the following steps: dispersing graphene oxide and a silane coupling agent in an ethanol solvent, immersing oxidized carbon fibers in the solution, taking out and drying, wherein the use amount of the carbon fibers, the graphene oxide, the silane coupling agent and the ethanol is 1 g: 3 g: 7 g: 500 ml; the silane coupling agent is gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane or N-beta (aminoethyl) -gamma-aminopropyltriethoxysilane; the curing temperature is 150 ℃, and the curing time is 2 hours; the pyrolysis temperature is 1300 ℃, and the pyrolysis time is 1.5 h.
The preparation method of the polycarbosilane precursor solution comprises the following steps:
(a) uniformly dispersing nano boehmite in an aqueous solution of KH550, and ultrasonically oscillating for 1 hour to obtain a mixture 1;
(b) distilling polydimethylsiloxane PDMS, collecting the fraction at 103 ℃, and drying; and then dropwise adding an organic solvent into the mixture and continuously stirring the mixture until the mass ratio of the organic solvent to the polydimethylsiloxane PDMS is 10: 100, denoted as solution 2;
(c) pouring the mixture 1 into the solution 2, heating in a water bath at 70 ℃, and stirring for 4 hours to obtain a mixture 3;
(d) putting the mixture 3 into a reaction kettle, introducing mixed gas of CO2 and inert gas, and pressurizing to 8 MPa; heating to 510 ℃ according to a certain heating program, and preserving heat for 18 hours; cooling to room temperature along with the furnace to obtain a crude product 4;
(e) and (3) dissolving the crude product 4 in an organic solvent to obtain a polycarbosilane precursor solution, wherein the polycarbosilane precursor solution has a mass percentage of 65%.
(2) Introducing the graphene oxide modified carbon fiber into a fluidized bed reactor, pyrolyzing the secondary butyl aluminum in the fluidized bed reactor into aluminum oxide by taking argon as a carrier gas and secondary butyl aluminum as an aluminum source, and depositing on the surface of the graphene oxide modified carbon fiber to form the graphene oxide modified carbon fiber coated with the aluminum oxide;
the temperature of a pyrolysis reaction temperature zone of the sec-butyl alcohol aluminum is 450 ℃, and the flow of argon is 0.15m3/h。
(3) Depositing a SiC layer on the surface of a base material by using a chemical vapor deposition method by using alumina-coated graphene oxide modified carbon fiber as the base material and trichloromethylsilane, hydrogen and argon as gas sources to form modified carbon fiber;
the SiC deposition conditions were: the deposition temperature is 1100 ℃, and the deposition pressure is 8mm Hg; the trichloromethylsilane flow rate is 90g/h, and the hydrogen flow rate is 0.15m3H, argon flow of 0.15m3H; after a period of deposition, the mixture is turned over and deposited again, wherein the deposition time is 15h each time, and 4 times of deposition are carried out.
(4) Mixing silicon carbide powder with the particle size of 45-75 microns, modified carbon fiber and sintering aid, adding the mixture into a ball mill, and adding phenolic resin, graphite powder and deionized water for ball milling;
the mass ratio of the silicon carbide powder to the modified carbon fibers to the sintering aid to the phenolic resin to the graphite powder to the deionized water is 65: 10: 3: 7: 3: 1000, parts by weight; the ball milling speed is 200 r/min, and the ball milling time is 4 h.
(5) Placing the slurry obtained after ball milling into a vacuum pressure tank, performing vacuum treatment, and injecting into a mold for dry pressing molding; curing for 10 hours at the temperature of 70 ℃;
the dry pressing method comprises the following steps: placing the mould filled with the slurry at 70 ℃ and under the pressure of 90MPa, and carrying out unidirectional pressurization for 2 min; and then inverting the mold, and continuously pressurizing in one direction at the temperature of 70 ℃ and under the pressure of 90MPa, wherein the pressure maintaining time is 2 min.
(6) In a vacuum furnace, in an inert atmosphere, heating to 1450 ℃ at the heating rate of 8 ℃/min, carrying out heat preservation sintering for 4h, wherein the vacuum degree in the vacuum furnace is 6 KPa; and cooling along with the furnace to obtain the modified carbon fiber toughened silicon carbide ceramic material.
Example 2
The preparation method of the modified carbon fiber toughened silicon carbide ceramic material comprises the following steps:
(1) oxidizing the surface of the carbon fiber, grafting graphene oxide on the surface of the carbon fiber by adopting a silane coupling agent, coating a polycarbosilane precursor solution on the surface of the carbon fiber modified by the graphene oxide, and curing and pyrolyzing at high temperature to form the graphene oxide modified carbon fiber;
the method for oxidizing the surface of the carbon fiber comprises the following steps: immersing the carbon fiber in acetone, and heating and refluxing for 10 hours; immersing in concentrated nitric acid at 30 ℃ for 3h after drying, taking out, washing and drying; the method for grafting the graphene oxide comprises the following steps: dispersing graphene oxide and a silane coupling agent in an ethanol solvent, immersing oxidized carbon fibers in the solution, taking out and drying, wherein the use amount of the carbon fibers, the graphene oxide, the silane coupling agent and the ethanol is 1 g: 2 g: 8 g: 400 ml; the silane coupling agent is gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane or N-beta (aminoethyl) -gamma-aminopropyltriethoxysilane; the curing temperature is 100 ℃, and the curing time is 3 hours; the pyrolysis temperature is 1200 ℃, and the pyrolysis time is 2 h.
The preparation method of the polycarbosilane precursor solution comprises the following steps:
(a) uniformly dispersing nano boehmite in an aqueous solution of KH550, and ultrasonically oscillating for 2 hours to obtain a mixture 1;
(b) distilling polydimethylsiloxane PDMS, collecting the fraction at 103 ℃, and drying; and then dropwise adding an organic solvent into the mixture and continuously stirring the mixture until the mass ratio of the organic solvent to the polydimethylsiloxane PDMS is 15: 100, denoted as solution 2;
(c) pouring the mixture 1 into the solution 2, heating in water bath at 60 ℃, and stirring for 6 hours to obtain a mixture 3;
(d) putting the mixture 3 into a reaction kettle, introducing mixed gas of CO2 and inert gas, and pressurizing to 5 MPa; heating to 520 ℃ according to a certain heating program, and keeping the temperature for 24 hours; cooling to room temperature along with the furnace to obtain a crude product 4;
(e) and (3) dissolving the crude product 4 in an organic solvent to obtain a polycarbosilane precursor solution, wherein the mass percentage content of the polycarbosilane precursor solution is 60%.
(2) Introducing the graphene oxide modified carbon fiber into a fluidized bed reactor, pyrolyzing the secondary butyl aluminum in the fluidized bed reactor into aluminum oxide by taking argon as a carrier gas and secondary butyl aluminum as an aluminum source, and depositing on the surface of the graphene oxide modified carbon fiber to form the graphene oxide modified carbon fiber coated with the aluminum oxide;
the temperature of the pyrolysis reaction temperature zone of the sec-butyl alcohol aluminum is 200 ℃, and the argon flow is 0.1m3/h。
(3) Depositing a SiC layer on the surface of a base material by using a chemical vapor deposition method by using alumina-coated graphene oxide modified carbon fiber as the base material and trichloromethylsilane, hydrogen and argon as gas sources to form modified carbon fiber;
the SiC deposition conditions were: the deposition temperature is 900 ℃, and the deposition pressure is 10mm Hg; the flow rate of trichloromethylsilane was 100g/h and the hydrogen flow rate was 0.1m3H, argon flow of 0.2m3H; after a period of deposition, the mixture is turned over and deposited again, wherein the deposition time is 20h each time, and 4 times of deposition are carried out.
(4) Mixing silicon carbide powder with the particle size of 45-75 microns, modified carbon fiber and sintering aid, adding the mixture into a ball mill, and adding phenolic resin, graphite powder and deionized water for ball milling;
the mass ratio of the silicon carbide powder to the modified carbon fibers to the sintering aid to the phenolic resin to the graphite powder to the deionized water is 60: 5: 4: 10: 2: 1000, parts by weight; the ball milling speed is 150 r/min, and the ball milling time is 6 h.
(5) Placing the slurry obtained after ball milling into a vacuum pressure tank, performing vacuum treatment, and injecting into a mold for dry pressing molding; curing for 12 hours at the temperature of 50 ℃;
the dry pressing method comprises the following steps: placing the mold filled with the slurry at 50 ℃ and under 100MPa, and carrying out unidirectional pressurization for 1 min; and then inverting the mold, and continuously pressurizing in one direction at the temperature of 50 ℃ and under the pressure of 100MPa, wherein the pressure maintaining time is 1 min.
(6) In a vacuum furnace, in an inert atmosphere, heating to 1400 ℃ at the heating rate of 5 ℃/min, carrying out heat preservation sintering for 2h, wherein the vacuum degree in the vacuum furnace is 2 KPa; and cooling along with the furnace to obtain the modified carbon fiber toughened silicon carbide ceramic material.
Example 3
The preparation method of the modified carbon fiber toughened silicon carbide ceramic material comprises the following steps:
(1) oxidizing the surface of the carbon fiber, grafting graphene oxide on the surface of the carbon fiber by adopting a silane coupling agent, coating a polycarbosilane precursor solution on the surface of the carbon fiber modified by the graphene oxide, and curing and pyrolyzing at high temperature to form the graphene oxide modified carbon fiber;
the method for oxidizing the surface of the carbon fiber comprises the following steps: immersing the carbon fiber in acetone, and heating and refluxing for 15 h; immersing in concentrated nitric acid at 90 ℃ for 1h after drying, taking out, washing and drying; the method for grafting the graphene oxide comprises the following steps: dispersing graphene oxide and a silane coupling agent in an ethanol solvent, immersing oxidized carbon fibers in the solution, taking out and drying, wherein the use amount of the carbon fibers, the graphene oxide, the silane coupling agent and the ethanol is 1 g: 4 g: 8 g: 400 ml; the silane coupling agent is gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane or N-beta (aminoethyl) -gamma-aminopropyltriethoxysilane; the curing temperature is 200 ℃, and the curing time is 1 h; the pyrolysis temperature is 1400 ℃, and the pyrolysis time is 1 h.
The preparation method of the polycarbosilane precursor solution comprises the following steps:
(a) uniformly dispersing nano boehmite in an aqueous solution of KH550, and ultrasonically oscillating for 0.5 hour to obtain a mixture 1;
(b) distilling polydimethylsiloxane PDMS, collecting the fraction at 103 ℃, and drying; and then dropwise adding an organic solvent into the mixture and continuously stirring the mixture until the mass ratio of the organic solvent to the polydimethylsiloxane PDMS is 5: 100, denoted as solution 2;
(c) pouring the mixture 1 into the solution 2, heating in water bath at 80 ℃, and stirring for 2 hours to obtain a mixture 3;
(d) putting the mixture 3 into a reaction kettle, introducing mixed gas of CO2 and inert gas, and pressurizing to 10 MPa; heating to 500 ℃ according to a certain heating program, and keeping the temperature for 12 hours; cooling to room temperature along with the furnace to obtain a crude product 4;
(e) and (3) dissolving the crude product 4 in an organic solvent to obtain a polycarbosilane precursor solution, wherein the polycarbosilane precursor solution has a mass percentage of 70%.
(2) Introducing the graphene oxide modified carbon fiber into a fluidized bed reactor, pyrolyzing the secondary butyl aluminum in the fluidized bed reactor into aluminum oxide by taking argon as a carrier gas and secondary butyl aluminum as an aluminum source, and depositing on the surface of the graphene oxide modified carbon fiber to form the graphene oxide modified carbon fiber coated with the aluminum oxide;
the temperature of the pyrolysis reaction temperature zone of the sec-butyl alcohol aluminum is 700 ℃, and the argon flow is 0.2m3/h。
(3) Depositing a SiC layer on the surface of a base material by using a chemical vapor deposition method by using alumina-coated graphene oxide modified carbon fiber as the base material and trichloromethylsilane, hydrogen and argon as gas sources to form modified carbon fiber;
the SiC deposition conditions were: the deposition temperature is 1200 ℃, and the deposition pressure is 5mm Hg; the trichloromethylsilane flow rate is 80g/h, and the hydrogen flow rate is 0.2m3H, argon flow of 0.1m3H; after a period of deposition, the mixture is turned over and deposited again, wherein the deposition time is 10h each time, and 4 times of deposition are carried out.
(4) Mixing silicon carbide powder with the particle size of 45-75 microns, modified carbon fiber and sintering aid, adding the mixture into a ball mill, and adding phenolic resin, graphite powder and deionized water for ball milling;
the mass ratio of the silicon carbide powder to the modified carbon fibers to the sintering aid to the phenolic resin to the graphite powder to the deionized water is 70: 15: 2: 4: 4: 1000, parts by weight; the ball milling speed is 250 r/min, and the ball milling time is 2 h.
(5) Placing the slurry obtained after ball milling into a vacuum pressure tank, performing vacuum treatment, and injecting into a mold for dry pressing molding; curing for 6 hours at the temperature of 90 ℃;
the dry pressing method comprises the following steps: placing the mold filled with the slurry at 90 deg.C under 80MPa, and unidirectionally pressurizing for 3 min; and inverting the mold, and continuously pressurizing in one direction at the temperature of 90 ℃ and under the pressure of 80MPa for 3 min.
(6) In a vacuum furnace, in an inert atmosphere, heating to 1500 ℃ again at the heating rate of 10 ℃/min, and carrying out heat preservation sintering for 6h, wherein the vacuum degree in the vacuum furnace is 9 KPa; and cooling along with the furnace to obtain the modified carbon fiber toughened silicon carbide ceramic material.
Comparative example 1
The preparation method of the silicon carbide ceramic material comprises the following steps:
(1) mixing silicon carbide powder with the particle size of 45-75 microns, carbon fibers and a sintering aid, adding the mixture into a ball mill, and adding phenolic resin, graphite powder and deionized water for ball milling;
the mass ratio of the silicon carbide powder to the carbon fibers to the sintering aid to the phenolic resin to the graphite powder to the deionized water is 65: 10: 3: 7: 3: 1000, parts by weight; the ball milling speed is 200 r/min, and the ball milling time is 4 h.
(2) Placing the slurry obtained after ball milling into a vacuum pressure tank, performing vacuum treatment, and injecting into a mold for dry pressing molding; curing for 10 hours at the temperature of 70 ℃;
the dry pressing method comprises the following steps: placing the mould filled with the slurry at 70 ℃ and under the pressure of 90MPa, and carrying out unidirectional pressurization for 2 min; and then inverting the mold, and continuously pressurizing in one direction at the temperature of 70 ℃ and under the pressure of 90MPa, wherein the pressure maintaining time is 2 min.
(3) In a vacuum furnace, in an inert atmosphere, heating to 1450 ℃ at the heating rate of 8 ℃/min, carrying out heat preservation sintering for 4h, wherein the vacuum degree in the vacuum furnace is 6 KPa; cooling along with the furnace to obtain the carbon fiber toughened silicon carbide ceramic material.
Examples of the experiments
The product properties of examples 1 to 3 and comparative example 1 were tested. The results are as follows:
the above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the modified carbon fiber toughened silicon carbide ceramic material is characterized by comprising the following steps: the method comprises the following steps:
(1) oxidizing the surface of the carbon fiber, grafting graphene oxide on the surface of the carbon fiber by adopting a silane coupling agent, coating a polycarbosilane precursor solution on the surface of the carbon fiber modified by the graphene oxide, and curing and pyrolyzing at high temperature to form the graphene oxide modified carbon fiber;
(2) introducing the graphene oxide modified carbon fiber into a fluidized bed reactor, pyrolyzing the secondary butyl aluminum in the fluidized bed reactor into aluminum oxide by taking argon as a carrier gas and secondary butyl aluminum as an aluminum source, and depositing on the surface of the graphene oxide modified carbon fiber to form the graphene oxide modified carbon fiber coated with the aluminum oxide;
(3) depositing a SiC layer on the surface of a base material by using a chemical vapor deposition method by using alumina-coated graphene oxide modified carbon fiber as the base material and trichloromethylsilane, hydrogen and argon as gas sources to form modified carbon fiber;
(4) mixing silicon carbide powder with the particle size of 45-75 microns, modified carbon fiber and sintering aid, adding the mixture into a ball mill, and adding phenolic resin, graphite powder and deionized water for ball milling;
(5) placing the slurry obtained after ball milling into a vacuum pressure tank, performing vacuum treatment, and injecting into a mold for dry pressing molding; curing for 6-12h at 50-90 ℃;
(6) in a vacuum furnace, in an inert atmosphere, heating to 1400 ℃ and 1500 ℃ at the heating rate of 5-10 ℃/min, and carrying out heat preservation sintering for 2-6 h; and cooling along with the furnace to obtain the modified carbon fiber toughened silicon carbide ceramic material.
2. The preparation method of the modified carbon fiber toughened silicon carbide ceramic material according to claim 1, wherein the preparation method comprises the following steps: in the step (1), the surface oxidation treatment method for the carbon fiber comprises the following steps: immersing the carbon fiber in acetone, and heating and refluxing for 10-15 h; immersing in concentrated nitric acid at 30-90 deg.C for 1-3h after drying, taking out, washing, and drying; the method for grafting the graphene oxide comprises the following steps: dispersing graphene oxide and a silane coupling agent in an ethanol solvent, immersing oxidized carbon fibers in the solution, taking out and drying, wherein the use amount of the carbon fibers, the graphene oxide, the silane coupling agent and the ethanol is 1 g: (2-4) g: (6-8) g: (400- > 600) ml; the silane coupling agent is gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane or N-beta (aminoethyl) -gamma-aminopropyltriethoxysilane; the curing temperature is 100-; the high-temperature cracking temperature is 1200 ℃ and 1400 ℃, and the high-temperature cracking time is 1-2 h.
3. The preparation method of the modified carbon fiber toughened silicon carbide ceramic material according to claim 1, wherein the preparation method comprises the following steps: in the step (1), the preparation method of the polycarbosilane precursor solution comprises the following steps:
(a) uniformly dispersing nano boehmite in an aqueous solution of KH550, and ultrasonically oscillating for 0.5-2 hours to obtain a mixture 1;
(b) distilling polydimethylsiloxane PDMS, collecting the fraction at 103 ℃, and drying; and then dropwise adding an organic solvent into the mixture and continuously stirring until the mass ratio of the organic solvent to the polydimethylsiloxane PDMS is (5-15): 100, denoted as solution 2;
(c) pouring the mixture 1 into the solution 2, heating in water bath at 60-80 ℃, and stirring for 2-6 hours to obtain a mixture 3;
(d) putting the mixture 3 into a reaction kettle, introducing mixed gas of CO2 and inert gas, and pressurizing to 5-10 MPa; heating to 500-520 ℃ according to a certain heating program, and preserving heat for 12-24 hours; cooling to room temperature along with the furnace to obtain a crude product 4;
(e) and (3) dissolving the crude product 4 in an organic solvent to obtain a polycarbosilane precursor solution, wherein the mass percentage content of the polycarbosilane precursor solution is 60-70%.
4. The preparation method of the modified carbon fiber toughened silicon carbide ceramic material according to claim 1, wherein the preparation method comprises the following steps: in the step (2), the temperature of the pyrolysis reaction temperature zone of the secondary aluminum butoxide is 200-3/h。
5. The preparation method of the modified carbon fiber toughened silicon carbide ceramic material according to claim 1, wherein the preparation method comprises the following steps: in the step (3), the SiC deposition conditions are as follows: the deposition temperature is 900 ℃ and 1200 ℃, and the deposition pressure is 5-10mm Hg; the flow rate of trichloromethylsilane is 80-100g/h, and the flow rate of hydrogen is 0.1-0.2m3H, argon flow of 0.1-0.2m3H; after a period of deposition, the mixture is turned over and deposited again, wherein the deposition time is 10-20h each time, and the deposition is carried out for 2 times or 4 times.
6. The preparation method of the modified carbon fiber toughened silicon carbide ceramic material according to claim 1, wherein the preparation method comprises the following steps: in the step (4), the mass ratio of the silicon carbide powder, the modified carbon fiber, the sintering aid, the phenolic resin, the graphite powder and the deionized water is (60-70): (5-15): (2-4): (4-10): (2-4): 1000, parts by weight; the ball milling speed is 150-.
7. The preparation method of the modified carbon fiber toughened silicon carbide ceramic material according to claim 1, wherein the preparation method comprises the following steps: in the step (5), the dry pressing method comprises the following steps: placing the mold filled with the slurry at 50-90 deg.C and 80-100MPa, and unidirectionally pressurizing for 1-3 min; and inverting the mold, and continuously pressurizing in one direction at 50-90 deg.C and 80-100MPa for 1-3 min.
8. The preparation method of the modified carbon fiber toughened silicon carbide ceramic material according to claim 1, wherein the preparation method comprises the following steps: in the step (6), the vacuum degree in the vacuum furnace is 2-9 KPa.
9. A modified carbon fibre toughened silicon carbide ceramic material produced by the method of any one of claims 1 to 8.
10. The modified carbon fiber toughened silicon carbide ceramic material is characterized in that; the carbon fiber composite material comprises silicon carbide and modified carbon fibers dispersed in the silicon carbide, wherein the modified carbon fibers comprise carbon fibers, and a graphene oxide layer, an aluminum oxide layer and a SiC layer which are sequentially coated outside the carbon fibers from inside to outside.
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