CN113845367A - Preparation method of high-temperature oxidation-resistant carbon fiber toughened zirconia ceramic material and high-temperature oxidation-resistant carbon fiber toughened zirconia ceramic material - Google Patents
Preparation method of high-temperature oxidation-resistant carbon fiber toughened zirconia ceramic material and high-temperature oxidation-resistant carbon fiber toughened zirconia ceramic material Download PDFInfo
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Abstract
The invention provides a preparation method of a high-temperature antioxidant carbon fiber toughened zirconia ceramic material. The invention also provides a high-temperature antioxidant carbon fiber toughened zirconia ceramic material, which comprises zirconia, zirconium tungstate and modified carbon fibers dispersed in the zirconia, wherein the modified carbon fibers comprise carbon fibers, and a graphene oxide layer, an aluminum oxide layer and a zirconia layer which are sequentially coated outside the carbon fibers from inside to outside. According to the zirconia ceramic material provided by the invention, the carbon fibers of the graphene oxide layer, the aluminum oxide layer and the zirconia 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 zirconia 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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material and the high-temperature antioxidant carbon fiber toughened zirconia ceramic material.
Background
With the development of science and technology, the function of materials in various fields is more and more prominent, new materials are more and more important to discover and prepare, and the discovery of new materials is limited by various conditions such as chance, so that the preparation of new materials by using the existing materials and changing or adjusting the preparation process becomes an important requirement for the materials. In this respect, the composite material has incomparable advantages, and has various excellent properties which are not possessed by a single material. The ceramic matrix composite has excellent performances of high temperature resistance, wear resistance, corrosion resistance and the like, so that the ceramic matrix composite is widely applied to the field of aerospace.
The ceramic material has larger expansion with heat and contraction with cold, which can reduce the structural stability and the safety reliability of the heat-proof parts and weaken and even destroy the heat-proof and oxidation-resistant ablation capacity of the material. When the environmental temperature is increased or decreased, if the volume of the material is changed little or hardly under the influence of the temperature, the problems of cracks, stress concentration and the like caused by the shape or volume change of the material in the application process can be reduced. That is, if the thermal expansion coefficient of the material itself is small, the material will play a crucial role in the important research fields of aerospace, precision instruments and the like. According to the principle of composite materials, materials with positive and negative thermal expansion coefficients are compounded, and materials with low expansion, zero expansion and even controllable thermal expansion coefficients can be obtained. Most materials in life expand at high temperature and contract at low temperature, and the thermal expansion coefficients of the materials are positive. However, there are also a small fraction of materials that shrink at high temperatures and expand at low temperatures, i.e., exhibit "cold swell and thermal shrinkage," and their coefficients of thermal expansion are negative, i.e., have "negative thermal expansion. In the thirties of the twentieth century, the phenomenon of "cold swelling and hot shrinking" of materials was observed, such as the perovskite ferroelectric material PbTiO3, cordierite 2 MgO.2A 12O 3.5 SiO2, beta-eucryptite LiAlSiO4, zeolite, and the like. However, the negative expansion of these materials is not considered to be important because the temperature range in which the negative expansion phenomenon occurs is too narrow, or the negative expansion behavior is anisotropic, so that the materials are likely to be microcracked during thermal cycling, have poor thermal shock resistance, and the like, and are difficult to be put into practical use.
Because of high melting point, high fracture toughness and high-temperature strength, low density, oxidation resistance, thermal shock resistance and good chemical stability, ZrO2 has wide application in the field of materials, and can be used as a thermal insulation layer of a rocket, a cylinder sleeve and a piston top of an internal combustion engine, various nozzles, ceramic valves, continuous casting nozzles and crucibles in smelting, a high-temperature corrosion-resistant thermometer and the like. The absolute values of the thermal expansion coefficients of ZrO2 and ZrW2O8 are similar and no chemical reaction occurs, ZrW2O8 is added into ZrO2, and the low-expansion or zero-expansion ZrO2/ZrW2O8 ceramic matrix composite material is obtained through component blending, so that the influence of temperature change on the dimensional accuracy in the service process of aviation and spacecrafts can be further reduced, the accuracy of heat-proof parts is improved, the internal stress generated by high-temperature expansion in the high-temperature material is further reduced, the thermal shock resistance of the material is increased, and the ceramic matrix composite material has wide and potential application value in the aerospace field.
However, there is a need for further improvements in the mechanical properties, particularly toughness, of conventional ZrO2/ZrW2O8 ceramic matrix composites.
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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material and the high-temperature antioxidant carbon fiber toughened zirconia ceramic material.
The technical scheme is as follows: the invention provides a preparation method of a high-temperature antioxidant carbon fiber toughened zirconia 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 zirconium oxide layer on the surface of a substrate by using a chemical vapor deposition method by using alumina-coated graphene oxide modified carbon fiber as the substrate, ZrCl4 as a zirconium source precursor, CO2 and hydrogen as reaction gases and argon as a diluent gas to form modified carbon fiber;
(4) mixing zirconium oxide powder with the particle size of 45-75 microns, zirconium tungstate powder, 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 high-temperature antioxidant carbon fiber toughened zirconia 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 zirconia deposition conditions are as follows: the deposition temperature is 900 ℃ and 1200 ℃, and the deposition pressure is 5-10mm Hg; ZrCl4The flow rate is 80-100g/h, CO2The flow rate is 0.1-0.2m3Hydrogen flow rate of 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 zirconium oxide powder, the zirconium tungstate powder, the modified carbon fibers, the sintering aid, the phenolic resin, the graphite powder and the deionized water is (60-70): (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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material prepared by the method.
The invention also provides a high-temperature antioxidant carbon fiber toughened zirconia ceramic material, which comprises zirconia, zirconium tungstate and modified carbon fibers dispersed in the zirconia, wherein the modified carbon fibers comprise carbon fibers, and a graphene oxide layer, an aluminum oxide layer and a zirconia layer which are sequentially coated outside the carbon fibers from inside to outside.
Has the advantages that: according to the zirconia ceramic material provided by the invention, the carbon fibers of the graphene oxide layer, the aluminum oxide layer and the zirconia 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 zirconia ceramic material is greatly improved.
Detailed Description
The present invention is further explained below.
Example 1
The preparation method of the high-temperature oxidation-resistant carbon fiber toughened zirconia 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 zirconium oxide layer on the surface of a substrate by using a chemical vapor deposition method by using alumina-coated graphene oxide modified carbon fiber as the substrate, ZrCl4 as a zirconium source precursor, CO2 and hydrogen as reaction gases and argon as a diluent gas to form modified carbon fiber;
the zirconia deposition conditions were: the deposition temperature is 1100 ℃, and the deposition pressure is 8mm Hg; ZrCl4Flow rate of 90g/h, CO2The flow rate is 0.15m3H, hydrogen flow 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 zirconium oxide powder with the particle size of 45-75 microns, zirconium tungstate powder, 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 zirconium oxide powder to the zirconium tungstate powder to the modified carbon fibers to the sintering aid to the phenolic resin to the graphite powder to the deionized water is 65: 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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material.
Example 2
The preparation method of the high-temperature oxidation-resistant carbon fiber toughened zirconia 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 zirconium oxide layer on the surface of a substrate by using a chemical vapor deposition method by using alumina-coated graphene oxide modified carbon fiber as the substrate, ZrCl4 as a zirconium source precursor, CO2 and hydrogen as reaction gases and argon as a diluent gas to form modified carbon fiber;
the zirconia deposition conditions were: the deposition temperature is 900 ℃, and the deposition pressure is 10mm Hg; ZrCl4 flow rate is 100g/h, CO2The flow rate is 0.1m3H, hydrogen flow 0.1m3H, argon flow of 0.2m3H; after a certain period of deposition, turning over and depositing again, each deposition timeFor 20h, 4 depositions.
(4) Mixing zirconium oxide powder with the particle size of 45-75 microns, zirconium tungstate powder, 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 zirconia powder to the zirconium tungstate powder to the modified carbon fibers to the sintering aid to the phenolic resin is 60: 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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material.
Example 3
The preparation method of the high-temperature oxidation-resistant carbon fiber toughened zirconia 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 zirconium oxide layer on the surface of a substrate by using a chemical vapor deposition method by using alumina-coated graphene oxide modified carbon fiber as the substrate, ZrCl4 as a zirconium source precursor, CO2 and hydrogen as reaction gases and argon as a diluent gas to form modified carbon fiber;
the zirconia deposition conditions were: the deposition temperature is 1200 ℃, and the deposition pressure is 5mm Hg; ZrCl4 flow rate is 80g/h, CO2The flow rate is 0.2m3H, hydrogen flow 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 zirconium oxide powder with the particle size of 45-75 microns, zirconium tungstate powder, 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 zirconia powder to the zirconium tungstate powder to the modified carbon fibers to the sintering aid to the phenolic resin is 70: 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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material.
Comparative example 1
The preparation method of the zirconia ceramic material comprises the following steps:
(1) mixing zirconium oxide powder with the particle size of 45-75 microns, zirconium tungstate powder, carbon fiber and sintering aid, adding into a ball mill, and adding phenolic resin, graphite powder and deionized water for ball milling;
the mass ratio of the zirconium oxide powder to the zirconium tungstate powder to the carbon fibers to the sintering aid to the phenolic resin to the graphite powder to the deionized water is 65: 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; and cooling along with the furnace to obtain the high-temperature antioxidant carbon fiber toughened zirconia 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 high-temperature oxidation-resistant carbon fiber toughened zirconia ceramic material is characterized by comprising the following steps of: 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) the method comprises the steps of taking graphene oxide modified carbon fibers coated with alumina as a base material, taking ZrCl4 as a zirconium source precursor and taking CO2And hydrogen is used as reaction gas, argon is used as diluent gas, and a zirconium oxide layer is deposited on the surface of the base material by using a chemical vapor deposition method to form modified carbon fibers;
(4) mixing zirconium oxide powder with the particle size of 45-75 microns, zirconium tungstate powder, 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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material.
2. The preparation method of the high-temperature antioxidant carbon fiber toughened zirconia ceramic material as claimed in claim 1, wherein: 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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material as claimed in claim 1, wherein: 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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material as claimed in claim 1, wherein: 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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material as claimed in claim 1, wherein: in the step (3), the zirconia deposition conditions are as follows: the deposition temperature is 900 ℃ and 1200 ℃, and the deposition pressure is 5-10mm Hg; ZrCl4The flow rate is 80-100g/h, CO2The flow rate is 0.1-0.2m3Hydrogen flow rate of 0.1-0.2m3H, argon flow of 0.1-0.2m3H; after a certain period of deposition, the mixture is turned over and deposited again, each timeThe time for the secondary deposition is 10-20h, and the deposition is carried out for 2 times or 4 times.
6. The preparation method of the high-temperature antioxidant carbon fiber toughened zirconia ceramic material as claimed in claim 1, wherein: in the step (4), the mass ratio of the zirconium oxide powder, the zirconium tungstate powder, the modified carbon fibers, the sintering aid, the phenolic resin, the graphite powder and the deionized water is (60-70): (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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material as claimed in claim 1, wherein: 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 high-temperature antioxidant carbon fiber toughened zirconia ceramic material as claimed in claim 1, wherein: in the step (6), the vacuum degree in the vacuum furnace is 2-9 KPa.
9. The high-temperature oxidation-resistant carbon fiber toughened zirconia ceramic material prepared by the method of any one of claims 1 to 8.
10. The high-temperature oxidation-resistant carbon fiber toughened zirconia ceramic material is characterized in that; the carbon fiber composite material comprises zirconium oxide, zirconium tungstate and modified carbon fibers dispersed in the zirconium oxide, wherein the modified carbon fibers comprise carbon fibers, and a graphene oxide layer, an aluminum oxide layer and a zirconium oxide layer which are sequentially coated outside the carbon fibers from inside to outside.
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