CN112745132A - High-compactness high-strength quartz ceramic matrix composite material and preparation method thereof - Google Patents
High-compactness high-strength quartz ceramic matrix composite material and preparation method thereof Download PDFInfo
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Abstract
The quartz ceramic-based composite material with high compactness and high strength mainly comprises the following components in parts by mass: 90-95 parts of amino modified fused quartz, 2-3 parts of N-hydroxymethyl acrylamide, 1-2 parts of carbon fiber, 1-1.5 parts of N, N-methylene bisacrylamide, 0.5-1 part of ammonium citrate, 0.5-1 part of sodium carboxymethylcellulose, 0.5-1 part of epoxy resin, 0.25-0.35 part of ammonium sulfate, 0.15-0.20 part of sodium borohydride and 0.01-0.02 part of reduced graphene oxide. The high-compactness high-strength quartz ceramic-based composite material and the preparation method thereof have reasonable formula arrangement, overcome the defects of brittleness and mechanical property of quartz ceramic under the synergistic action of the carbon fiber, the ammonium sulfate, the sodium borohydride and the BN nanosheet prepared by reducing the graphene oxide, enhance the mechanical property of the quartz ceramic-based composite material, and simultaneously have the advantages of excellent thermal shock resistance, low dielectric constant, low loss angle tangent value, small thermal expansion coefficient and the like, and have simple preparation process and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of quartz ceramic-based composite materials, and particularly relates to a high-compactness high-strength quartz ceramic-based composite material and a preparation method thereof.
Background
Quartz ceramic materials are widely used because of their advantages such as good thermal shock resistance, low and stable dielectric constant and loss tangent, low thermal expansion coefficient, and low manufacturing cost. At present, the demand of military industry fields such as aerospace and the like on high-performance quartz ceramic materials still accounts for a great proportion, which is mainly determined by special application scenes and performance demands, and aircrafts such as missiles, rockets and the like inevitably generate great friction heat in atmospheric environment to cause surface temperature rise due to extremely high flying speed. Electronic components, wireless equipment and the like in the aircraft are relatively fragile, a thermal insulation layer needs to be added for protection, and the built-in wireless equipment at a specific position also requires that external protective materials have good wave permeability. In addition, internal power systems such as engines have high working temperature, structural load and thermal shock. The melting point of the quartz ceramic material is generally more than three thousand ℃, the quartz ceramic material can keep the stability of chemical properties and physical properties in extreme environments, can be applied to complex external environment extreme environments consisting of extreme environments such as ultrahigh temperature, high radiation, high-strength mechanical load, ultrahigh mechanical wear, high particle beam collision, high impact strength and the like, and the performance characteristics well meet the harsh working environment and performance requirements, so that the quartz ceramic material is an ideal material choice.
With the continuous progress of the aerospace field and the development towards high speed, long distance, high precision, high maneuverability and the like, the quartz ceramic material matched with the quartz ceramic material has higher requirements on heat resistance, wave transmission, bearing and the like. The brittleness of the quartz ceramic limits the application of the quartz ceramic in materials in the field of aerospace to a certain extent.
Therefore, in order to further improve the shortages of brittleness and mechanical property of the quartz ceramic, a high-density and high-strength quartz ceramic matrix composite and a preparation process thereof need to be developed to solve the technical problems.
Chinese patent application No. CN201811513497.1 discloses a preparation method of glass fiber reinforced quartz ceramic, quartz powder with different grain diameters is evenly mixed with glass fiber according to different proportions to obtain A, a proper amount of polyvinyl alcohol and water are added into the A for granulation, the glass fiber or woven fiber cloth is placed in a cavity of a forming die, the granulated powder is used for filling gaps, the mixture is pressed into a quartz ceramic blank after the completion, the quartz ceramic blank is dried, the quartz ceramic blank is sintered at high temperature to prepare the glass fiber reinforced quartz ceramic, and the compactness and the strength of the quartz ceramic matrix composite material need to be further improved.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects, the invention aims to provide the high-compactness and high-strength quartz ceramic-based composite material and the preparation method thereof, the formula is reasonably set, the defects of brittleness and mechanical property of quartz ceramic are improved through the synergistic effect of carbon fiber, ammonium sulfate, sodium borohydride and BN nanosheet prepared by reducing graphene oxide, the mechanical property of the quartz ceramic-based composite material is enhanced, and the composite material has the advantages of excellent thermal shock resistance, low dielectric constant, low loss tangent value, small thermal expansion coefficient and the like, and has simple preparation process and wide application prospect.
The purpose of the invention is realized by the following technical scheme:
the high-compactness high-strength quartz ceramic matrix composite material mainly comprises the following components in parts by mass: 90-95 parts of amino modified fused quartz, 2-3 parts of N-hydroxymethyl acrylamide, 1-2 parts of carbon fiber, 1-1.5 parts of N, N-methylene bisacrylamide, 0.5-1 part of ammonium citrate, 0.5-1 part of sodium carboxymethylcellulose, 0.5-1 part of epoxy resin, 0.25-0.35 part of ammonium sulfate, 0.15-0.20 part of sodium borohydride and 0.01-0.02 part of reduced graphene oxide.
The high-compactness high-strength quartz ceramic-based composite material disclosed by the invention is reasonable in formula arrangement, overcomes the defects of brittleness and mechanical property of quartz ceramic under the synergistic action of the carbon fibers, ammonium sulfate, sodium borohydride and reduced graphene oxide, enhances the mechanical property of the quartz ceramic-based composite material, and has the advantages of excellent thermal shock resistance, low dielectric constant, low loss angle tangent value, small thermal expansion coefficient and the like.
The chemical bonds in the quartz ceramic are mainly ionic bonds and covalent bonds, and the two chemical bonds have directionality and associativity, so that the ceramic material has high brittleness and is difficult to generate plastic deformation, and the practical application of the ceramic material is limited. According to the invention, the BN nano-sheets are prepared by adopting ammonium sulfate, sodium borohydride and reduced graphene oxide, the sodium borohydride is a boron source, the ammonium sulfate is a nitrogen source, the RGO is a template, and the carbon fiber and the BN nano-sheets have excellent mechanical properties, good thermal conductivity, excellent high-temperature and chemical stability and good biocompatibility, can be used as a composite material additive phase to play a role of strengthening and toughening phases, and generate a synergistic effect between the carbon fiber and the BN nano-sheets, so that the mechanical properties of the quartz ceramic matrix composite material are greatly improved. The sodium carboxymethyl cellulose in the formula plays roles of bonding and pore forming, can be decomposed and volatilized in the subsequent sintering process, and cannot have adverse effects caused by the existence of residues; through the solidification effect of a three-dimensional network structure formed by N-hydroxymethyl acrylamide and N, N-methylene bisacrylamide, under the action of auxiliaries such as ammonium citrate and epoxy resin, the components interact, are interdependent and complement each other, and a synergistic effect is achieved.
The invention also relates to a preparation method of the high-compactness high-strength quartz ceramic matrix composite material, which comprises the following steps:
(1) preparation of BN nanosheets: weighing ammonium sulfate, sodium borohydride and reduced graphene oxide according to the formula, and preparing a BN nanosheet through a high-pressure solid-phase method;
(2) amino-modified fused silica: adding fused quartz powder into the mixed solution of ethanol/deionized water, carrying out ultrasonic treatment for 0.3-0.5h at room temperature, adding gamma-aminopropyltriethoxysilane, and carrying out ultrasonic treatment for 0.1-0.2h at room temperature; heating to 60 ℃, continuously stirring for 10-12h, vacuum-filtering, collecting the treated product, repeatedly washing the collected product with ethanol and deionized water, and drying at 60-80 ℃ for 20-24h to obtain amino-modified fused quartz;
(3) preparing the quartz ceramic matrix composite material: preparing amino modified fused quartz, N-hydroxymethyl acrylamide, carbon fiber, N-methylene bisacrylamide, ammonium citrate, sodium carboxymethyl cellulose and epoxy resin according to the formula; taking the BN nanosheet, wherein the mass ratio of the BN nanosheet to the amino-modified fused quartz is 0.4-0.6: 100; adding carbon fiber, epoxy resin and sodium carboxymethylcellulose into the amino modified fused quartz, and performing ball milling and powder mixing by using a ball mill for 2-3h to obtain mixed powder; dissolving N-hydroxymethyl acrylamide and N, N-methylene bisacrylamide in deionized water, uniformly stirring, and adjusting the pH value with lactic acid and ammonia water to prepare a precursor solution; adding mixed powder into the precursor solution, adding ammonium citrate, adjusting the pH value to 4-5, and treating for 10-12h by combining high-speed stirring with ultrasonic dispersion to form a first suspension; dissolving a BN nano sheet in deionized water, treating for 8-10h in a high-speed stirring and ultrasonic dispersion mode to form a second suspension, and adjusting the pH value of the second suspension to 4-5 by hydrochloric acid and an ammonia water solution; slowly adding the suspension II into the suspension I while continuously stirring; after mixing, standing, wherein a flocculation reaction generates a precipitate in the standing process; after the flocculation reaction is finished, collecting the obtained composite powder through vacuum filtration;
(4) and (3) drying: putting the composite powder into a drying oven, drying and heating to 70-80 ℃, and drying and molding at constant temperature to obtain a quartz ceramic-based green body;
(5) microwave sintering: and carrying out microwave sintering on the quartz ceramic-based green body to obtain the quartz ceramic-based composite material.
The fused quartz is modified by amino, the carbon fiber and BN nanosheets are uniformly dispersed in the quartz ceramic matrix through a flocculation method assisted by surface modification, and the carbon fiber and BN nanosheets are not easy to stack together due to pi-pi interaction, so that the reinforcing and toughening effects of the carbon fiber and BN nanosheets on the quartz ceramic matrix are improved; the preparation step also reduces the porosity of the subsequent fused quartz ceramic roller green compact and improves the compactness of the quartz ceramic matrix.
Further, the preparation method of the high-density high-strength quartz ceramic-based composite material in the step (1) specifically includes the following steps: uniformly mixing by grinding; putting the uniformly mixed reactants into a stainless steel high-pressure reaction kettle, sealing the reaction kettle, putting the reaction kettle into a crucible resistance furnace, heating to 600-700 ℃, preserving heat for 10-12 hours, and cooling the reaction kettle to room temperature along with the furnace after stopping heating; and after cooling, opening the reaction kettle, taking out, and repeatedly washing with hydrochloric acid and deionized water to obtain the BN nanosheet.
Further, in the preparation method of the high-compactness high-strength quartz ceramic matrix composite material, in the step (2), 30-35g of fused quartz powder and 3-4mL of gamma-aminopropyltriethoxysilane are added into each 1L of ethanol/deionized water mixed solution; the volume ratio of the ethanol to the deionized water in the ethanol/deionized water mixed solution is 98: 2.
further, in the preparation method of the high-density high-strength quartz ceramic-based composite material, the BN nanosheet in the step (3) is subjected to hydroxyl modification.
Further, the preparation method of the high-compactness high-strength quartz ceramic matrix composite material, wherein the hydroxyl modification of the BN nanosheet, comprises the following steps: uniformly mixing BN nano-sheets and an aqueous solution of sodium hydroxide, then transferring the mixture into a stainless steel ball-milling tank, carrying out ball milling for 20-24h at the rotation speed of 200-300rpm, collecting the ball-milled product through vacuum filtration, repeatedly washing the collected product with hydrochloric acid and deionized water, drying, and dispersing the product in an ethanol/water mixed solution again for ultrasonic treatment for 3-4h to obtain a suspension; centrifuging the suspension for 0.4-0.5h under the condition of 2500-3500rpm, collecting supernatant by vacuum filtration, and drying the product on the filter paper for 20-24h at 80-90 ℃ to obtain the hydroxyl modified BN nanosheet.
The surface of the BN nanosheet can be provided with hydroxyl functional groups through modifying the hydroxyl on the surface of the BN nanosheet, and the hydrophobicity of the BN nanosheet can be regulated and controlled through the hydroxyl on the surface, so that the dispersibility of the BN nanosheet in an aqueous solution can be improved through surface modification, the introduced hydroxyl can promote the electrostatic repulsion among the BN nanosheets, so that the BN nanosheets can be promoted to form stable suspension, and the uniform distribution of the BN nanosheets in a quartz ceramic matrix can be realized more easily through a flocculation method.
Further, in the preparation method of the high-compactness high-strength quartz ceramic matrix composite material, the aqueous solution of sodium hydroxide is 5mol/L, and 15-20gBN nanosheets are added into 1L of aqueous solution of sodium hydroxide; the volume ratio of the ethanol to the deionized water in the ethanol/water mixed solution is 55: 45.
further, the preparation method of the high-compactness high-strength quartz ceramic matrix composite material comprises the following steps of: setting the microwave early-stage heating rate to be 5-10 ℃/min, the output power to be 1500W, heating to 600 ℃, and keeping the temperature for 30 min; and (3) raising the temperature to 1100-1150 ℃ at the later-stage heating rate of 25-30 ℃/min and the output power of 2000W, and preserving the temperature for 2h to obtain the quartz ceramic matrix composite.
In order to improve the compactness of the quartz ceramic-based composite material and inhibit crystallization to a certain extent, a microwave sintering method is adopted for sintering, the heating rate in the early stage is 5-10 ℃/min, otherwise, the quartz ceramic-based green body is easy to crack, because the ceramic powder is solidified through a three-dimensional network structure formed by N-hydroxymethyl acrylamide and N, N-methylene bisacrylamide, the heating rate is too high, and the ceramic powder is not completely diffused and bonded. Once the N-methylol acrylamide and the N, N-methylene bisacrylamide are quickly removed, the N-methylol acrylamide and the N, N-methylene bisacrylamide are easy to crack, if the temperature rising rate is too slow, the process time can be prolonged, and the production cost is increased. Organic matters in the quartz ceramic-based green compact begin to be lost in the sintering process, the degreasing is basically finished when the temperature reaches about 500 ℃, but in order to prevent the organic matters from remaining, the temperature is optimally raised to 600 ℃ in the early stage, and the densification performance is enhanced by heat preservation for 30 min.
Then, the quartz ceramic matrix composite material is rapidly sintered, the heating rate is 25-30 ℃/min, the bending strength of the sintered quartz ceramic matrix composite material is increased along with the acceleration of the heating rate, the microwave is integral heating, the problem of temperature gradient can hardly occur in the heating process, and the phenomenon of thermal runaway can not be caused by rapid heating in the later stage. When the temperature reaches 1000 ℃, the bending strength is rapidly increased, which shows that the particles of the quartz ceramic matrix composite begin to participate in sintering at the temperature higher than 1000 ℃, and the bending strength gradually increases along with the continuous increase of the temperature, but the strength is weakened and cristobalite transformation begins after the temperature is increased to 1200 ℃, so that the temperature is increased to 1100-1150 ℃, the effect is best, the temperature is kept for 2 hours, the migration of mass points is completed, the bonding and solidification are carried out between the quartz particles, the temperature keeping time is prolonged, the production time is increased, the production cost is increased, and the cristobalite transformation may be caused.
Compared with the prior art, the invention has the following beneficial effects:
(1) the high-compactness high-strength quartz ceramic-based composite material disclosed by the invention is reasonable in formula arrangement, overcomes the defects of brittleness and mechanical property of quartz ceramic under the synergistic action of the carbon fibers, ammonium sulfate, sodium borohydride and reduced graphene oxide prepared BN nanosheets, enhances the mechanical property of the quartz ceramic-based composite material, and has the advantages of excellent thermal shock resistance, low dielectric constant, low loss angle tangent value, small thermal expansion coefficient and the like;
(2) the preparation method of the high-compactness high-strength quartz ceramic matrix composite material disclosed by the invention is simple and has high flexibility, and the fused quartz is modified by adopting the amino group and the hydroxyl group on the surface of the BN nanosheet is modified, so that the carbon fiber and the BN nanosheet are uniformly dispersed in the quartz ceramic matrix by adopting a surface modification assisted flocculation method, and are not easy to stack together due to pi-pi interaction, and the reinforcing and toughening effects of the carbon fiber and the BN nanosheet on the quartz ceramic matrix are improved; the preparation step also reduces the porosity of the subsequent fused quartz ceramic roller green compact and improves the compactness of the quartz ceramic matrix; the microwave sintering method is adopted for sintering, the compactness of the quartz ceramic matrix composite material is improved, and the crystallization is inhibited to a certain extent.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention are clearly and completely described in the embodiments with reference to specific experimental data, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, but not all embodiments. 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 following embodiment provides a high-compactness high-strength quartz ceramic matrix composite, which mainly comprises the following components in parts by mass: 90-95 parts of amino modified fused quartz, 2-3 parts of N-hydroxymethyl acrylamide, 1-2 parts of carbon fiber, 1-1.5 parts of N, N-methylene bisacrylamide, 0.5-1 part of ammonium citrate, 0.5-1 part of sodium carboxymethylcellulose, 0.5-1 part of epoxy resin, 0.25-0.35 part of ammonium sulfate, 0.15-0.20 part of sodium borohydride and 0.01-0.02 part of reduced graphene oxide.
Example 1
The preparation method of the high-compactness high-strength quartz ceramic matrix composite material comprises the following steps:
(1) preparation of BN nanosheets: according to the formula, 0.25 part of ammonium sulfate, 0.20 part of sodium borohydride and 0.01 part of reduced graphene oxide; weighing ammonium sulfate, sodium borohydride and reduced graphene oxide, and uniformly mixing in a grinding mode; putting the uniformly mixed reactants into a stainless steel high-pressure reaction kettle, sealing the reaction kettle, putting the reaction kettle into a crucible resistance furnace, heating to 600 ℃, preserving heat for 12 hours, and cooling the reaction kettle to room temperature along with the furnace after stopping heating; after cooling, opening the reaction kettle, taking out, and repeatedly washing with hydrochloric acid and deionized water to obtain BN nanosheets;
then, hydroxyl modification is carried out on the BN nano-sheets, and the hydroxyl modification of the BN nano-sheets comprises the following steps: uniformly mixing aqueous solutions of BN nanosheets and sodium hydroxide, transferring the mixture into a stainless steel ball milling tank, carrying out ball milling for 22 hours at the rotating speed of 250rpm, collecting ball-milled products through vacuum filtration, repeatedly washing the collected products with hydrochloric acid and deionized water, drying, and dispersing the products in an ethanol/water mixed solution again for ultrasonic treatment for 4 hours to obtain a suspension; centrifuging the suspension for 0.5h at 3000rpm, collecting supernatant by vacuum filtration, and drying a product on filter paper for 20h at 80 ℃ to obtain a hydroxyl-modified BN nanosheet; the sodium hydroxide aqueous solution is 5mol/L, and 15gBN nanosheets are added into 1L of sodium hydroxide aqueous solution; the volume ratio of the ethanol to the deionized water in the ethanol/water mixed solution is 55: 45, a first step of;
(2) amino-modified fused silica: adding fused quartz powder into the mixed solution of ethanol/deionized water, carrying out ultrasonic treatment for 0.3h at room temperature, adding gamma-aminopropyltriethoxysilane, and continuing ultrasonic treatment for 0.2h at room temperature; heating to 60 ℃, continuously stirring for 12h, carrying out vacuum filtration to collect the treated product, repeatedly washing the collected product with ethanol and deionized water, and drying at 80 ℃ for 20h to obtain amino modified fused quartz; adding 30g of fused quartz powder and 3.0mL of gamma-aminopropyltriethoxysilane into each 1L of ethanol/deionized water mixed solution; the volume ratio of the ethanol to the deionized water in the ethanol/deionized water mixed solution is 98: 2;
(3) preparing the quartz ceramic matrix composite material: according to the formula, 92 parts of amino modified fused quartz, 2 parts of N-hydroxymethyl acrylamide, 2 parts of carbon fiber, 1 part of N, N-methylene bisacrylamide, 0.5 part of ammonium citrate, 0.6 part of sodium carboxymethylcellulose and 0.5 part of epoxy resin; preparing amino modified fused quartz, N-hydroxymethyl acrylamide, carbon fiber, N-methylene bisacrylamide, ammonium citrate, sodium carboxymethyl cellulose and epoxy resin; taking the BN nanosheet, wherein the mass ratio of the BN nanosheet to the amino-modified fused quartz is 0.45: 100; adding carbon fiber, epoxy resin and sodium carboxymethylcellulose into the amino modified fused quartz, and performing ball milling and powder mixing by using a ball mill for 3 hours to obtain mixed powder; dissolving N-hydroxymethyl acrylamide and N, N-methylene bisacrylamide in deionized water, uniformly stirring, and adjusting the pH value with lactic acid and ammonia water to prepare a precursor solution; adding mixed powder into the precursor solution, adding ammonium citrate, adjusting the pH value to 4-5, and treating for 12 hours by combining high-speed stirring with ultrasonic dispersion to form a first suspension; dissolving a BN nano sheet in deionized water, treating for 10 hours in a high-speed stirring and ultrasonic dispersion mode to form a second suspension, and adjusting the pH value of the second suspension to 4-5 by hydrochloric acid and an ammonia water solution; slowly adding the suspension II into the suspension I while continuously stirring; after mixing, standing, wherein a flocculation reaction generates a precipitate in the standing process; after the flocculation reaction is finished, collecting the obtained composite powder through vacuum filtration;
(4) and (3) drying: putting the composite powder into a drying oven, drying and heating to 80 ℃, and drying and molding at constant temperature to obtain a quartz ceramic-based green compact;
(5) microwave sintering: performing microwave sintering on the quartz ceramic-based green body, setting the microwave early-stage heating rate to be 6 ℃/min, setting the output power to be 1500W, heating to 600 ℃, and keeping the temperature for 30 min; and (3) raising the temperature to 1135 ℃ at the later-stage heating rate of 25 ℃/min and the output power of 2000W, and preserving the heat for 2h to obtain the quartz ceramic matrix composite material and obtain the quartz ceramic matrix composite material.
Example 2
(2) Preparation of BN nanosheets: according to the formula, 0.30 part of ammonium sulfate, 0.20 part of sodium borohydride and 0.02 part of reduced graphene oxide; weighing ammonium sulfate, sodium borohydride and reduced graphene oxide, and uniformly mixing in a grinding mode; putting the uniformly mixed reactants into a stainless steel high-pressure reaction kettle, sealing the reaction kettle, putting the reaction kettle into a crucible resistance furnace, heating to 600 ℃, preserving heat for 1h, and cooling the reaction kettle to room temperature along with the furnace after stopping heating; after cooling, opening the reaction kettle, taking out, and repeatedly washing with hydrochloric acid and deionized water to obtain BN nanosheets;
then, hydroxyl modification is carried out on the BN nano-sheets, and the hydroxyl modification of the BN nano-sheets comprises the following steps: uniformly mixing aqueous solutions of BN nanosheets and sodium hydroxide, transferring the mixture into a stainless steel ball milling tank, carrying out ball milling for 20 hours at the rotating speed of 300rpm, collecting ball-milled products through vacuum filtration, repeatedly washing the collected products with hydrochloric acid and deionized water, drying, and dispersing the products in an ethanol/water mixed solution again for ultrasonic treatment for 3 hours to obtain a suspension; centrifuging the suspension for 0.5h at 2500rpm, collecting supernatant by vacuum filtration, and drying a product on filter paper for 22h at 90 ℃ to obtain a hydroxyl-modified BN nanosheet; the sodium hydroxide aqueous solution is 5mol/L, and 18gBN nanosheets are added into 1L of sodium hydroxide aqueous solution; the volume ratio of the ethanol to the deionized water in the ethanol/water mixed solution is 55: 45, a first step of;
(2) amino-modified fused silica: adding fused quartz powder into the mixed solution of ethanol/deionized water, carrying out ultrasonic treatment for 0.5h at room temperature, adding gamma-aminopropyltriethoxysilane, and continuing ultrasonic treatment for 0.1h at room temperature; heating to 60 ℃, continuously stirring for 12h, carrying out vacuum filtration to collect the treated product, repeatedly washing the collected product with ethanol and deionized water, and drying at 65 ℃ for 24h to obtain amino modified fused quartz; adding 35g of fused quartz powder and 4mL of gamma-aminopropyltriethoxysilane into each 1L of ethanol/deionized water mixed solution; the volume ratio of the ethanol to the deionized water in the ethanol/deionized water mixed solution is 98: 2;
(3) preparing the quartz ceramic matrix composite material: according to the formula, 93 parts of amino modified fused quartz, 2.5 parts of N-hydroxymethyl acrylamide, 1.5 parts of carbon fiber, 1.5 parts of N, N-methylene bisacrylamide, 0.6 part of ammonium citrate, 0.6 part of sodium carboxymethylcellulose and 0.5 part of epoxy resin; preparing amino modified fused quartz, N-hydroxymethyl acrylamide, carbon fiber, N-methylene bisacrylamide, ammonium citrate, sodium carboxymethyl cellulose and epoxy resin; taking the BN nanosheet, wherein the mass ratio of the BN nanosheet to the amino-modified fused quartz is 0.5: 100; adding carbon fiber, epoxy resin and sodium carboxymethylcellulose into the amino modified fused quartz, and performing ball milling and powder mixing by using a ball mill for 2 hours to obtain mixed powder; dissolving N-hydroxymethyl acrylamide and N, N-methylene bisacrylamide in deionized water, uniformly stirring, and adjusting the pH value with lactic acid and ammonia water to prepare a precursor solution; adding mixed powder into the precursor solution, adding ammonium citrate, adjusting the pH value to 4-5, and treating for 12 hours by combining high-speed stirring with ultrasonic dispersion to form a first suspension; dissolving a BN nano sheet in deionized water, treating for 8 hours in a high-speed stirring and ultrasonic dispersion mode to form a second suspension, and adjusting the pH value of the second suspension to 4-5 by hydrochloric acid and an ammonia water solution; slowly adding the suspension II into the suspension I while continuously stirring; after mixing, standing, wherein a flocculation reaction generates a precipitate in the standing process; after the flocculation reaction is finished, collecting the obtained composite powder through vacuum filtration;
(4) and (3) drying: putting the composite powder into a drying oven, drying and heating to 70 ℃, and drying and molding at constant temperature to obtain a quartz ceramic-based green compact;
(5) microwave sintering: performing microwave sintering on the quartz ceramic-based green body, setting the microwave early-stage heating rate to be 5 ℃/min, setting the output power to be 1500W, heating to 600 ℃, and keeping the temperature for 30 min; and (3) heating to 1120 ℃ at a later-stage heating rate of 30 ℃/min and an output power of 2000W, and preserving heat for 2h to obtain the quartz ceramic matrix composite material, thus obtaining the quartz ceramic matrix composite material.
Example 3
(3) Preparation of BN nanosheets: according to the formula, 0.32 part of ammonium sulfate, 0.18 part of sodium borohydride and 0.015 part of reduced graphene oxide; weighing ammonium sulfate, sodium borohydride and reduced graphene oxide, and uniformly mixing in a grinding mode; putting the uniformly mixed reactants into a stainless steel high-pressure reaction kettle, sealing the reaction kettle, putting the reaction kettle into a crucible resistance furnace, heating to 650 ℃, preserving heat for 12 hours, and cooling the reaction kettle to room temperature along with the furnace after stopping heating; after cooling, opening the reaction kettle, taking out, and repeatedly washing with hydrochloric acid and deionized water to obtain BN nanosheets;
then, hydroxyl modification is carried out on the BN nano-sheets, and the hydroxyl modification of the BN nano-sheets comprises the following steps: uniformly mixing aqueous solutions of BN nanosheets and sodium hydroxide, transferring the mixture into a stainless steel ball-milling tank, carrying out ball milling for 24 hours at the rotating speed of 300rpm, collecting ball-milled products through vacuum filtration, repeatedly washing the collected products with hydrochloric acid and deionized water, drying, and dispersing the products in an ethanol/water mixed solution again for ultrasonic treatment for 3-4 hours to obtain a suspension; centrifuging the suspension for 0.4h at 3500rpm, collecting supernatant by vacuum filtration, and drying the product on filter paper at 80 ℃ for 20h to obtain a hydroxyl-modified BN nanosheet; the sodium hydroxide aqueous solution is 5mol/L, and 16gBN nanosheets are added into 1L of sodium hydroxide aqueous solution; the volume ratio of the ethanol to the deionized water in the ethanol/water mixed solution is 55: 45, a first step of;
(2) amino-modified fused silica: adding fused quartz powder into the mixed solution of ethanol/deionized water, carrying out ultrasonic treatment for 0.4h at room temperature, adding gamma-aminopropyltriethoxysilane, and continuing ultrasonic treatment for 0.2h at room temperature; heating to 60 ℃, continuously stirring for 12h, carrying out vacuum filtration to collect the treated product, repeatedly washing the collected product with ethanol and deionized water, and drying at 75 ℃ for 22h to obtain amino modified fused quartz; adding 32g of fused quartz powder and 3.2mL of gamma-aminopropyltriethoxysilane into each 1L of ethanol/deionized water mixed solution; the volume ratio of the ethanol to the deionized water in the ethanol/deionized water mixed solution is 98: 2;
(3) preparing the quartz ceramic matrix composite material: according to the formula, 94 parts of amino modified fused quartz, 2.2 parts of N-hydroxymethyl acrylamide, 1.8 parts of carbon fiber, 1.2 parts of N, N-methylene bisacrylamide, 0.6 part of ammonium citrate, 0.6 part of sodium carboxymethylcellulose and 0.5 part of epoxy resin; preparing amino modified fused quartz, N-hydroxymethyl acrylamide, carbon fiber, N-methylene bisacrylamide, ammonium citrate, sodium carboxymethyl cellulose and epoxy resin; taking the BN nanosheet, wherein the mass ratio of the BN nanosheet to the amino-modified fused quartz is 0.48: 100; adding carbon fiber, epoxy resin and sodium carboxymethylcellulose into the amino modified fused quartz, and performing ball milling and powder mixing by using a ball mill for 2.2 hours to obtain mixed powder; dissolving N-hydroxymethyl acrylamide and N, N-methylene bisacrylamide in deionized water, uniformly stirring, and adjusting the pH value with lactic acid and ammonia water to prepare a precursor solution; adding mixed powder into the precursor solution, adding ammonium citrate, adjusting the pH value to 4-5, and treating for 12 hours by combining high-speed stirring with ultrasonic dispersion to form a first suspension; dissolving a BN nano sheet in deionized water, treating for 8 hours in a high-speed stirring and ultrasonic dispersion mode to form a second suspension, and adjusting the pH value of the second suspension to 4-5 by hydrochloric acid and an ammonia water solution; slowly adding the suspension II into the suspension I while continuously stirring; after mixing, standing, wherein a flocculation reaction generates a precipitate in the standing process; after the flocculation reaction is finished, collecting the obtained composite powder through vacuum filtration;
(4) and (3) drying: putting the composite powder into a drying oven, drying and heating to 75 ℃, and drying and molding at constant temperature to obtain a quartz ceramic-based green compact;
(5) microwave sintering: performing microwave sintering on the quartz ceramic-based green body, setting the microwave early-stage heating rate to be 8 ℃/min, setting the output power to be 1500W, heating to 600 ℃, and keeping the temperature for 30 min; and heating to 1138 ℃ at the later-stage heating rate of 26 ℃/min and the output power of 2000W, and preserving the heat for 2h to obtain the quartz ceramic matrix composite material and obtain the quartz ceramic matrix composite material.
Example 4
(4) Preparation of BN nanosheets: according to the formula, 0.3 part of ammonium sulfate, 0.18 part of sodium borohydride and 0.02 part of reduced graphene oxide; weighing ammonium sulfate, sodium borohydride and reduced graphene oxide, and uniformly mixing in a grinding mode; putting the uniformly mixed reactants into a stainless steel high-pressure reaction kettle, sealing the reaction kettle, putting the reaction kettle into a crucible resistance furnace, heating to 650 ℃, preserving heat for 12 hours, and cooling the reaction kettle to room temperature along with the furnace after stopping heating; after cooling, opening the reaction kettle, taking out, and repeatedly washing with hydrochloric acid and deionized water to obtain BN nanosheets;
then, hydroxyl modification is carried out on the BN nano-sheets, and the hydroxyl modification of the BN nano-sheets comprises the following steps: uniformly mixing aqueous solutions of BN nanosheets and sodium hydroxide, transferring the mixture into a stainless steel ball milling tank, carrying out ball milling for 22 hours at the rotating speed of 250rpm, collecting ball-milled products through vacuum filtration, repeatedly washing the collected products with hydrochloric acid and deionized water, drying, and dispersing the products in an ethanol/water mixed solution again for ultrasonic treatment for 3-4 hours to obtain a suspension; centrifuging the suspension for 0.5h at 3000rpm, collecting supernatant by vacuum filtration, and drying a product on filter paper for 22h at 90 ℃ to obtain a hydroxyl-modified BN nanosheet; the sodium hydroxide aqueous solution is 5mol/L, and 15gBN nanosheets are added into 1L of sodium hydroxide aqueous solution; the volume ratio of the ethanol to the deionized water in the ethanol/water mixed solution is 55: 45, a first step of;
(2) amino-modified fused silica: adding fused quartz powder into the mixed solution of ethanol/deionized water, carrying out ultrasonic treatment for 0.5h at room temperature, adding gamma-aminopropyltriethoxysilane, and continuing ultrasonic treatment for 0.2h at room temperature; heating to 60 ℃, continuously stirring for 10h, carrying out vacuum filtration to collect the treated product, repeatedly washing the collected product with ethanol and deionized water, and drying at 70 ℃ for 20h to obtain amino modified fused quartz; adding 35g of fused quartz powder and 3.0mL of gamma-aminopropyltriethoxysilane into each 1L of ethanol/deionized water mixed solution; the volume ratio of the ethanol to the deionized water in the ethanol/deionized water mixed solution is 98: 2;
(3) preparing the quartz ceramic matrix composite material: according to the formula, 90 parts of amino modified fused quartz, 3 parts of N-hydroxymethyl acrylamide, 1 part of carbon fiber, 1.2 parts of N, N-methylene bisacrylamide, 0.8 part of ammonium citrate, 0.6 part of sodium carboxymethyl cellulose and 0.6 part of epoxy resin; preparing amino modified fused quartz, N-hydroxymethyl acrylamide, carbon fiber, N-methylene bisacrylamide, ammonium citrate, sodium carboxymethyl cellulose and epoxy resin; taking the BN nanosheet, wherein the mass ratio of the BN nanosheet to the amino-modified fused quartz is 0.55: 100; adding carbon fiber, epoxy resin and sodium carboxymethylcellulose into the amino modified fused quartz, and performing ball milling and powder mixing by using a ball mill for 2.5 hours to obtain mixed powder; dissolving N-hydroxymethyl acrylamide and N, N-methylene bisacrylamide in deionized water, uniformly stirring, and adjusting the pH value with lactic acid and ammonia water to prepare a precursor solution; adding mixed powder into the precursor solution, adding ammonium citrate, adjusting the pH value to 4-5, and treating for 12 hours by combining high-speed stirring with ultrasonic dispersion to form a first suspension; dissolving a BN nano sheet in deionized water, treating for 8 hours in a high-speed stirring and ultrasonic dispersion mode to form a second suspension, and adjusting the pH value of the second suspension to 4-5 by hydrochloric acid and an ammonia water solution; slowly adding the suspension II into the suspension I while continuously stirring; after mixing, standing, wherein a flocculation reaction generates a precipitate in the standing process; after the flocculation reaction is finished, collecting the obtained composite powder through vacuum filtration;
(4) and (3) drying: putting the composite powder into a drying oven, drying and heating to 80 ℃, and drying and molding at constant temperature to obtain a quartz ceramic-based green compact;
(5) microwave sintering: performing microwave sintering on the quartz ceramic-based green body, setting the microwave early-stage heating rate to be 6 ℃/min, setting the output power to be 1500W, heating to 600 ℃, and keeping the temperature for 30 min; and (3) heating to 1130 ℃ at the later-stage heating rate of 25 ℃/min and the output power of 2000W, and preserving heat for 2h to obtain the quartz ceramic matrix composite material and obtain the quartz ceramic matrix composite material.
Example 5
(5) Preparation of BN nanosheets: according to the formula, 0.32 part of ammonium sulfate, 0.16 part of sodium borohydride and 0.014 part of reduced graphene oxide; weighing ammonium sulfate, sodium borohydride and reduced graphene oxide, and uniformly mixing in a grinding mode; putting the uniformly mixed reactants into a stainless steel high-pressure reaction kettle, sealing the reaction kettle, putting the reaction kettle into a crucible resistance furnace, heating to 650 ℃, preserving heat for 10 hours, and cooling the reaction kettle to room temperature along with the furnace after stopping heating; after cooling, opening the reaction kettle, taking out, and repeatedly washing with hydrochloric acid and deionized water to obtain BN nanosheets;
then, hydroxyl modification is carried out on the BN nano-sheets, and the hydroxyl modification of the BN nano-sheets comprises the following steps: uniformly mixing aqueous solutions of BN nanosheets and sodium hydroxide, transferring the mixture into a stainless steel ball milling tank, carrying out ball milling for 20 hours at the rotating speed of 300rpm, collecting ball-milled products through vacuum filtration, repeatedly washing the collected products with hydrochloric acid and deionized water, drying, and dispersing the products in an ethanol/water mixed solution again for ultrasonic treatment for 3 hours to obtain a suspension; centrifuging the suspension for 0.4h at 3500rpm, collecting supernatant by vacuum filtration, and drying the product on filter paper for 24h at 80 ℃ to obtain a hydroxyl-modified BN nanosheet; the sodium hydroxide aqueous solution is 5mol/L, and 16gBN nanosheets are added into 1L of sodium hydroxide aqueous solution; the volume ratio of the ethanol to the deionized water in the ethanol/water mixed solution is 55: 45, a first step of;
(2) amino-modified fused silica: adding fused quartz powder into the mixed solution of ethanol/deionized water, carrying out ultrasonic treatment for 0.5h at room temperature, adding gamma-aminopropyltriethoxysilane, and continuing ultrasonic treatment for 0.1h at room temperature; heating to 60 ℃, continuously stirring for 12h, carrying out vacuum filtration to collect the treated product, repeatedly washing the collected product with ethanol and deionized water, and drying at-80 ℃ for 24h to obtain amino modified fused quartz; adding 32g of fused quartz powder and 3.6mL of gamma-aminopropyltriethoxysilane into each 1L of ethanol/deionized water mixed solution; the volume ratio of the ethanol to the deionized water in the ethanol/deionized water mixed solution is 98: 2;
(3) preparing the quartz ceramic matrix composite material: according to the formula, 94 parts of amino modified fused quartz, 2 parts of N-hydroxymethyl acrylamide, 2 parts of carbon fiber, 1.5 parts of N, N-methylene bisacrylamide, 0.5 part of ammonium citrate, 0.5 part of sodium carboxymethylcellulose and 0.5 part of epoxy resin; preparing amino modified fused quartz, N-hydroxymethyl acrylamide, carbon fiber, N-methylene bisacrylamide, ammonium citrate, sodium carboxymethyl cellulose and epoxy resin; taking the BN nanosheet, wherein the mass ratio of the BN nanosheet to the amino-modified fused quartz is 0.52: 100; adding carbon fiber, epoxy resin and sodium carboxymethylcellulose into the amino modified fused quartz, and performing ball milling and powder mixing by using a ball mill for 2 hours to obtain mixed powder; dissolving N-hydroxymethyl acrylamide and N, N-methylene bisacrylamide in deionized water, uniformly stirring, and adjusting the pH value with lactic acid and ammonia water to prepare a precursor solution; adding mixed powder into the precursor solution, adding ammonium citrate, adjusting the pH value to 4-5, and treating for 12 hours by combining high-speed stirring with ultrasonic dispersion to form a first suspension; dissolving a BN nano sheet in deionized water, treating for 10 hours in a high-speed stirring and ultrasonic dispersion mode to form a second suspension, and adjusting the pH value of the second suspension to 4-5 by hydrochloric acid and an ammonia water solution; slowly adding the suspension II into the suspension I while continuously stirring; after mixing, standing, wherein a flocculation reaction generates a precipitate in the standing process; after the flocculation reaction is finished, collecting the obtained composite powder through vacuum filtration;
(4) and (3) drying: putting the composite powder into a drying oven, drying and heating to 80 ℃, and drying and molding at constant temperature to obtain a quartz ceramic-based green compact;
(5) microwave sintering: performing microwave sintering on the quartz ceramic-based green body, setting the microwave early-stage heating rate to be 8 ℃/min, setting the output power to be 1500W, heating to 600 ℃, and keeping the temperature for 30 min; and heating to 1135 ℃ at the later-stage heating rate of 28 ℃/min and the output power of 2000W, and preserving the heat for 2h to obtain the quartz ceramic matrix composite material and obtain the quartz ceramic matrix composite material.
Effect verification:
the performance tests of the high-density, high-strength quartz ceramic-based composite materials obtained in examples 1, 2, 3, 4 and 5 were carried out according to the following criteria, and the test results are shown in tables 1 and 2.
Flexural strength resistance: the room temperature and high temperature flexural strength of the high density, high strength quartz ceramic matrix composites obtained in examples 1, 2, 3, 4, and 5 were measured by three-point bending.
(1) The room temperature flexural strength test specimens were processed as follows: the high-density and high-strength quartz ceramic-based composite materials obtained in the above examples 1, 2, 3, 4 and 5 were ground flat on a flat grinder to reduce the thickness to 4 mm. And processing the sample into a long strip with the width of 3mm and the length of 20-30mm by using an inner diameter slicer. In order to improve the test accuracy, the sand paper for the machined examples 1, 2, 3, 4 and 5 and B4And C, performing fine grinding and chamfering. The test was then carried out on an electronic universal tester with a span of 20mm, the loading rate of the test being 0.5mm/s, the loading being carried out in the hot-pressing direction. 3-4 samples were tested per example 1, example 2, example 3, example 4, example 5 and then averaged.
(2) The high temperature bending strength test was conducted on an electronic universal tester with a span of 30 mm. Examples 1, 2, 3, 4, 5 were machined into long strips of 3mm X4 mm X (30-40) mm in size. In the high temperature test, the temperature was first raised to the test temperature at a rate of 20 ℃/min, and then the temperature was maintained at 1000 ℃ for 20 minutes, so that examples 1, 2, 3, 4 and 5 were uniformly heated in a heating furnace. The process of loading and specimen fracture is completed within the test temperature range. The calculation method of the high-temperature bending strength is consistent with the normal-temperature bending strength.
Bulk density: the full-automatic electronic densimeter with the model number of MH-300A is adopted, the volume density refers to the mass of a unit volume of a material under the state of containing a real volume, an opening and a closed pore, and the fundamental principle is that the principle of an underwater displacement method of Archimedes is utilized. That is, the volume of the test sample and thus the volume density value thereof are known by measuring the volume of the water drained from the article.
TABLE 1 sample Performance test results
| Performance index | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Room temperature flexural strength (Mpa) | 98.56 | 99.64 | 100.12 | 99.67 | 101.45 |
| Bending Strength (Mpa) at 1000 ℃ | 82.87 | 84.79 | 89.64 | 88.61 | 90.12 |
| Bulk Density (g/cm3) | 2.01 | 1.95 | 1.99 | 1.98 | 1.99 |
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (8)
1. The high-compactness high-strength quartz ceramic matrix composite material is characterized by mainly comprising the following components in parts by mass: 90-95 parts of amino modified fused quartz, 2-3 parts of N-hydroxymethyl acrylamide, 1-2 parts of carbon fiber, 1-1.5 parts of N, N-methylene bisacrylamide, 0.5-1 part of ammonium citrate, 0.5-1 part of sodium carboxymethylcellulose, 0.5-1 part of epoxy resin, 0.25-0.35 part of ammonium sulfate, 0.15-0.20 part of sodium borohydride and 0.01-0.02 part of reduced graphene oxide.
2. The method for preparing a high-density, high-strength quartz ceramic matrix composite according to claim 1, comprising the steps of:
(1) preparation of BN nanosheets: weighing ammonium sulfate, sodium borohydride and reduced graphene oxide according to the formula, and preparing a BN nanosheet through a high-pressure solid-phase method;
(2) amino-modified fused silica: adding fused quartz powder into the mixed solution of ethanol/deionized water, carrying out ultrasonic treatment for 0.3-0.5h at room temperature, adding gamma-aminopropyltriethoxysilane, and carrying out ultrasonic treatment for 0.1-0.2h at room temperature; heating to 60 ℃, continuously stirring for 10-12h, vacuum-filtering, collecting the treated product, repeatedly washing the collected product with ethanol and deionized water, and drying at 60-80 ℃ for 20-24h to obtain amino-modified fused quartz;
(3) preparing the quartz ceramic matrix composite material: preparing amino modified fused quartz, N-hydroxymethyl acrylamide, carbon fiber, N-methylene bisacrylamide, ammonium citrate, sodium carboxymethyl cellulose and epoxy resin according to the formula; taking the BN nanosheet, wherein the mass ratio of the BN nanosheet to the amino-modified fused quartz is 0.4-0.6: 100; adding carbon fiber, epoxy resin and sodium carboxymethylcellulose into the amino modified fused quartz, and performing ball milling and powder mixing by using a ball mill for 2-3h to obtain mixed powder; dissolving N-hydroxymethyl acrylamide and N, N-methylene bisacrylamide in deionized water, uniformly stirring, and adjusting the pH value with lactic acid and ammonia water to prepare a precursor solution; adding mixed powder into the precursor solution, adding ammonium citrate, adjusting the pH value to 4-5, and treating for 10-12h by combining high-speed stirring with ultrasonic dispersion to form a first suspension; dissolving a BN nano sheet in deionized water, treating for 8-10h in a high-speed stirring and ultrasonic dispersion mode to form a second suspension, and adjusting the pH value of the second suspension to 4-5 by hydrochloric acid and an ammonia water solution; slowly adding the suspension II into the suspension I while continuously stirring; after mixing, standing, wherein a flocculation reaction generates a precipitate in the standing process; after the flocculation reaction is finished, collecting the obtained composite powder through vacuum filtration;
(4) and (3) drying: putting the composite powder into a drying oven, drying and heating to 70-80 ℃, and drying and molding at constant temperature to obtain a quartz ceramic-based green body;
(5) microwave sintering: and carrying out microwave sintering on the quartz ceramic-based green body to obtain the quartz ceramic-based composite material.
3. The preparation method of the high-compactness high-strength quartz ceramic matrix composite material according to claim 2, wherein the preparation of the BN nanosheet in the step (1) specifically comprises the following steps: uniformly mixing by grinding; and (2) putting the uniformly mixed reactants into a stainless steel high-pressure reaction kettle, sealing the reaction kettle, putting the reaction kettle into a crucible resistance furnace, heating to 600-700 ℃, keeping the temperature for 10-12h, cooling the reaction kettle to room temperature along with the furnace after stopping heating, opening the reaction kettle after cooling, taking out, and repeatedly washing with hydrochloric acid and deionized water to obtain the BN nanosheet.
4. The method for preparing the high-density high-strength quartz ceramic-based composite material according to claim 2, wherein in the step (2), 30-35g of fused silica powder and 3-4mL of gamma-aminopropyltriethoxysilane are added into each 1L of the ethanol/deionized water mixed solution; the volume ratio of the ethanol to the deionized water in the ethanol/deionized water mixed solution is 98: 2.
5. the method for preparing the high-density high-strength quartz ceramic-based composite material according to claim 2, wherein the BN nanosheet in the step (3) is subjected to hydroxyl modification.
6. The preparation method of the high-compactness high-strength quartz ceramic-based composite material according to claim 5, wherein the hydroxyl modification of the BN nanosheet comprises the following steps: uniformly mixing BN nano-sheets and an aqueous solution of sodium hydroxide, then transferring the mixture into a stainless steel ball-milling tank, carrying out ball milling for 20-24h at the rotation speed of 200-300rpm, collecting the ball-milled product through vacuum filtration, repeatedly washing the collected product with hydrochloric acid and deionized water, drying, and dispersing the product in an ethanol/water mixed solution again for ultrasonic treatment for 3-4h to obtain a suspension; centrifuging the suspension for 0.4-0.5h under the condition of 2500-3500rpm, collecting supernatant by vacuum filtration, and drying the product on the filter paper for 20-24h at 80-90 ℃ to obtain the hydroxyl modified BN nanosheet.
7. The preparation method of the high-compactness high-strength quartz ceramic-based composite material according to claim 6, wherein the aqueous solution of sodium hydroxide is 5mol/L, and 15-20gBN nano sheets are added into every 1L of the aqueous solution of sodium hydroxide; the volume ratio of the ethanol to the deionized water in the ethanol/water mixed solution is 55: 45.
8. the method for preparing the high-compactness high-strength quartz ceramic matrix composite according to claim 2, wherein the microwave sintering specifically comprises the following steps: setting the microwave early-stage heating rate to be 5-10 ℃/min, the output power to be 1500W, heating to 600 ℃, and keeping the temperature for 30 min; and (3) raising the temperature to 1100-1150 ℃ at the later-stage heating rate of 25-30 ℃/min and the output power of 2000W, and preserving the temperature for 2h to obtain the quartz ceramic matrix composite.
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| CN113816771A (en) * | 2021-09-27 | 2021-12-21 | 沈阳工业大学 | Structure and preparation method of porous silicon nitride ceramic surface coating |
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Application publication date: 20210504 |