CN107698271B - High-temperature-resistant high-strength and high-toughness silicon nitride-based wave-transparent composite material and preparation method thereof - Google Patents
High-temperature-resistant high-strength and high-toughness silicon nitride-based wave-transparent composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-temperature-resistant high-strength and high-toughness silicon nitride-based wave-transparent composite material and a preparation method thereof3N4Obtaining porous Si after drying and binder removal of whisker biscuit3N4Preparing Boron Nitride (BN) interface in the whisker preform by Chemical Vapor Infiltration (CVI), and preparing multilayer alternative BN/Si by CVI3N4A substrate. Aiming at design requirements of high-temperature wave-transparent radome structure and performance, multilayer alternative BN/Si is realized through CVI regulation and control3N4The microstructure, the number of layers and the thickness of each layer of the matrix are regulated and controlled to realize the regulation and the optimization of the structure and the performance of the composite material, and the Si with high temperature resistance, high strength and toughness, wide frequency wave transmission and excellent thermophysical performance is obtained3N4A fundamental wave-transparent composite material.
Description
Technical Field
The invention belongs to the technology of silicon nitride-based wave-transparent composite materials, and relates to a high-temperature-resistant high-strength-toughness silicon nitride-based wave-transparent composite material and a preparation method thereof.
Background
The antenna cover is an important structural member for protecting a system of a missile and other spacecrafts from being influenced by the environment under severe environment conditions, such as communication, remote measurement, guidance, detonation and the like, and is widely applied to radio systems of missiles, radars, satellites and the like. Modern military demands on high-Mach-number (Ma is more than or equal to 8) missiles and other aircrafts are urgent, and further more severe use requirements are provided for antenna covers. The performance of the antenna housing is directly dependent on the selected material, and in order to realize high-Mach flight and accurate guidance of an aircraft, the antenna housing material is required to integrate multiple functions of temperature resistance, thermal shock resistance, bearing, broadband wave transmission, rain erosion resistance and the like.
Si3N4The material has excellent performances of relatively low density, high strength, thermal shock resistance, rain erosion resistance and the like, and excellent dielectric properties of low dielectric loss, lower dielectric constant and the like, and is an ideal high-temperature wave-transmitting material. The solid-phase sintering method (such as reaction sintering, hot-pressing sintering, hot isostatic pressing sintering and the like) is currently used for preparing Si3N4The most common approach is the radome. In general, the ceramic material has high sintering temperature, difficult control of sintering process, difficult machining and high production cost. Dense Si prepared by sintering process3N4Although the material has high strength, the toughness is insufficient, the dielectric constant is high, and the use requirement of an aircraft with high Mach number cannot be met. For example, the homogeneous alloy and the like are sintered by hot pressing in the literature' the preparation process progress of the ceramic matrix composite material antenna housing3N4Material having a density of 3.2g/cm3The bending strength is 391MPa, the dielectric constant is 7.9, the mechanical property is excellent, but the dielectric constant is higher. Porous Si prepared by sintering method by changing forming process (such as compression molding or 3D printing forming) or introducing pore-forming agent3N4The dielectric constant of the material is obviously reduced, but the related process is not beneficial to improving the mechanical property of the material. For example, Zhang Jian et al in "a preparation method of porous silicon nitride wave-transparent ceramic with low dielectric constant and high strength" (CN200910150098.8)3N4Powder and metal oxidationThe material is used as raw material, and is sintered in nitrogen atmosphere by adopting a cold press molding method to prepare porous Si3N4The material has porosity higher than 40%, bending strength higher than 71MPa, and dielectric loss lower than 6.5X 10-3The dielectric constant is less than 3.5, the dielectric property is excellent, but the strength is to be improved. In view of the above problems, there is an urgent need to develop a Si3N4The novel preparation method of the material has the characteristics of low preparation temperature, good process regulation and control performance, good processability and the like, and can realize Si3N4The structure and the performance of the material are optimized, so that Si is obtained3N4The material has high toughness and wide-band wave-transmitting property, and effectively solves the problem of high-temperature wave-transmitting Si at present3N4The research of materials is difficult.
Chemical Vapor Infiltration (CVI) is one of the most advanced ceramic matrix composite fabrication technologies at present. The ceramic matrix composite material prepared by the process has high purity, good compactness and excellent mechanical property, and the process has low preparation temperature, large process regulation space and rich processing ways, is suitable for preparing large-scale complex components, thereby being used as high-performance Si3N4Excellent candidates for materials. The prefabricated body with controllable pore structure is prepared by adopting CVI method to prepare high-performance Si3N4Precondition for the material, currently BN or Si3N4The fiber preform has the problems of high difficulty in developing fibers, difficulty in weaving ceramic fibers, influence of matrix deposition effect due to weaving pores, anisotropy of the preform structure (such as a two-dimensional, two-dimensional and half-dimensional or three-dimensional weaving structure) and the like; and BN or Si3N4The particle prefabricated body has the problems of poor connectivity of sintered particles, insufficient mechanical property, difficult regulation and control of pore structures, difficult maintenance of structural uniformity and the like. Therefore, the materials and the structure of the prefabricated body need to be reselected and optimally designed so as to meet the requirement of preparing high-performance Si by a subsequent CVI method3N4The requirements of the material.
The gel casting process is suitable for preparing porous prefabricated body, and can realize near net size formation, and the prepared blank has certain strength, is favorable to rough machining, and has high technological regulation and control performance, short period and low cost. Si3N4The whisker is a whisker with excellent performanceThe mechanical property, the environmental property and the excellent dielectric property of the reinforcement material are compounded with the ceramic matrix, so that the toughness of the material can be obviously improved. In view of the above process and material advantages, the present invention proposes to prepare Si by gel injection molding first3N4And (3) preparing a whisker preform. In the preform, Si3N4The whiskers are mutually crossed and connected and are uniformly distributed in the three-dimensional reticular polymer, so that the skeleton function can be fully exerted, three-dimensional holes formed among the whiskers are uniformly distributed and have good connectivity, and the preparation and densification of a subsequent matrix are facilitated. Thus, it can be seen that Si is prepared by gel injection molding3N4The whisker preform can realize the aims of isotropy, porous structure and obdurability, and meets the requirements of high-performance Si3N4The preform structure requirements of the material.
Due to Si3N4The crystal whisker is in a crystalline structure and is applied to Si by a CVI method3N4Si prepared in whisker preform3N4The matrix is usually amorphous structure, and in order to relieve thermal expansion and modulus mismatch between the whisker and the matrix, a BN interface with lower modulus and fracture energy, low dielectric constant and dielectric loss is required to be introduced between the whisker and the matrix. Meanwhile, in order to meet the requirements of strength, toughness and electrical property of different antenna covers, Si is required3N4Preparation of multilayer alternating BN/Si in whisker preform3N4The matrix realizes BN and Si through CVI process regulation3N4The microstructure, relative content, layer number and layer thickness of the substrate are regulated, the pore structure and performance of the composite material are improved, and the comprehensive requirements of the antenna housing material on excellent mechanical, thermal and dielectric properties are met.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a high-temperature-resistant high-strength and high-toughness silicon nitride-based wave-transmitting composite material and a preparation method thereof, and aims to solve the problem of the existing Si3N4The base wave-transparent material has insufficient obdurability and wave-transparent property, can not meet the use requirement of high-Mach number aircrafts and the like, and provides a high-performance Si3N4Whisker reinforced BN/Si3N4Fundamental wave-transparent complexThe gel casting of the composite material is combined with a CVI technology preparation method.
Technical scheme
A high-temperature-resistant high-strength and high-toughness silicon nitride-based wave-transparent composite material is characterized in that: the composite material is multilayer alternating BN/Si3N4The substrate, the innermost layer is BN substrate, and the middle layer is alternative BN/Si3N4A substrate with Si as the outermost layer3N4A substrate.
A method for preparing the high-temperature-resistant high-strength and high-toughness silicon nitride-based wave-transmitting composite material is characterized by comprising the following steps of:
step 1, Si3N4Preparing a whisker biscuit: si with the volume fraction of 20-50%3N4Dissolving crystal whiskers and 1.5-2.5 wt.% of dispersant polyacrylamide in deionized water, and adding tetramethylammonium hydroxide as a pH value regulator to regulate the pH value of the slurry to 9-11; adding 4-10 wt.% of monomer acrylamide AM and 0.2-1.0 wt.% of cross-linking agent methylene bisacrylamide MBAM, ball-milling for 24-36 h, and removing bubbles in vacuum for 10 min; then adding 0.2-0.5 wt.% of initiator ammonium persulfate APS and 0.02-0.1 wt.% of catalyst tetramethylethylenediamine TEMED, stirring, pouring into a mold, and molding to obtain Si3N4Biscuit of whisker;
step 2: mixing Si3N4Naturally drying the whisker biscuit at room temperature for 12-36 h, and then drying in an oven at 50-100 ℃; then placing the mixture in a muffle furnace, and carrying out empty burning and glue discharging for 2-4 h at 400-700 ℃ to obtain Si3N4Preparing a whisker preform;
step 3, preparing an interface: mixing Si3N4Placing the whisker preform in a deposition furnace, and preparing a BN interface by adopting a CVI method, wherein the thickness of the interface is 0.8-1.5 mu m; si containing BN interface may then be added3N4Placing the whisker preform in a high-temperature furnace for heat treatment, wherein the treatment temperature is 1300 ℃, and the treatment time is 2-6 h;
step 4, preparation of a matrix: si containing BN interface obtained in step 33N4The whisker preform is placed in a deposition furnace, and multilayer alternative BN/Si is prepared by adopting a CVI method3N4The innermost layer of the base body is a BN groupBulk, intermediate layer of alternating BN/Si3N4A substrate with Si as the outermost layer3N4A substrate.
And (2) forming the Si3N4 whisker preform in the step 1 by gel casting.
Advantageous effects
The invention provides a high-temperature-resistant high-strength and high-toughness silicon nitride-based wave-transparent composite material and a preparation method thereof3N4Obtaining porous Si after drying and binder removal of whisker biscuit3N4Preparing Boron Nitride (BN) interface in the whisker preform by Chemical Vapor Infiltration (CVI), and preparing multilayer alternative BN/Si by CVI3N4A substrate. Aiming at design requirements of high-temperature wave-transparent radome structure and performance, multilayer alternative BN/Si is realized through CVI regulation and control3N4The microstructure, the number of layers and the thickness of each layer of the matrix are regulated and controlled to realize the regulation and the optimization of the structure and the performance of the composite material, and the Si with high temperature resistance, high strength and toughness, wide frequency wave transmission and excellent thermophysical performance is obtained3N4A fundamental wave-transparent composite material.
Has the advantages that:
1. the invention adopts the gel casting process to form the porous Si3N4The whisker preform has high forming precision and strong process controllability, and can realize the near net size forming of the radome with a complex shape. Si after forming3N4The whisker biscuit has certain strength, can be roughly processed, further reduces the processing cost and solves the problem that the densified ceramic material is difficult to process. Porous Si3N4The crystal whisker microstructure, the volume fraction, the preform pore structure and other gel casting process parameters in the crystal whisker preform can be regulated and controlled, and Si is favorably adopted3N4Designing and optimizing the microstructure and the mechanical/wave-transparent performance of the whisker preform.
2. The invention relates to a method for preparing Si for high-temperature application at low temperature3N4The base wave-transparent composite material is prepared at low temperature, so that the damage of a reinforcing phase can be effectively reduced, the composite material obtains excellent mechanical property, the process difficulty can be reduced, and the process stability can be improved.
3. The invention relates to a multilayer alternating BN/Si3N4The matrix passes through the innermost BN and the outermost Si3N4Intermediate BN/Si3N4The structural design idea of alternate deposition not only realizes the good matching of the multilayer matrix and the BN interface, but also can meet the environmental use requirements of the composite material such as oxidation resistance, rain erosion resistance and the like, and the designability of each layer of microstructure, layer thickness and layer number of the multilayer matrix is strong, thereby being beneficial to improving and optimizing the performance of the composite material and finally obtaining the high-strength high-toughness broadband wave-transmitting Si for the radome3N4The foundation is laid by the base composite material.
Drawings
FIG. 1 is porous Si prepared according to example 1 of the present invention3N4SEM photograph of microstructure of whisker preform.
FIG. 2 is Si prepared according to example 1 of the present invention3N4SEM photograph of the microstructure of the base composite.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the invention adopts the following technical scheme:
step 1.Si3N4Preparing a whisker biscuit: si with the volume fraction of 20-50%3N4Dissolving crystal whiskers and 1.5-2.5 wt.% of dispersant polyacrylamide in deionized water, and adding tetramethylammonium hydroxide as a pH value regulator to regulate the pH value of the slurry to 9-11; adding 4-10 wt.% of monomer Acrylamide (AM) and 0.2-1.0 wt.% of cross-linking agent Methylene Bisacrylamide (MBAM), ball-milling the slurry for 24-36 h, and removing bubbles in vacuum for 10min after uniform mixing; then adding 0.2-0.5 wt.% of initiator ammonium persulfate and 0.02-0.1 wt.% of catalyst Tetramethylethylenediamine (TEMED), uniformly stirring, pouring into a mold, and molding to obtain Si3N4And (5) biscuit of the whisker.
Step 2.Si3N4Drying of the whisker biscuit: si in the step 13N4Naturally drying the whisker biscuit at room temperature for 12-36 h, and then drying in an oven at 50-100 ℃.
Step 3.Si3N4And (3) gel discharging of the whisker biscuit: si in the step 23N4Putting the whisker biscuit in a muffle furnace, and carrying out empty burning and glue discharging for 2-4 h at 400-700 ℃ to obtain Si3N4And (3) preparing a whisker preform.
Step 4, preparing an interface: si in the step 33N4And placing the whisker preform in a deposition furnace, and preparing a BN interface by adopting a CVI method, wherein the thickness of the interface is 0.8-1.5 mu m. Si containing BN interface may then be added3N4And (3) placing the whisker preform in a high-temperature furnace for heat treatment, wherein the treatment temperature is 1300 ℃, and the treatment time is 2-6 h.
Step 5, preparing a matrix: according to the design requirements of structure and performance, Si containing BN interface in the step 43N4The whisker preform is placed in a deposition furnace, and multilayer alternative BN/Si is prepared by adopting a CVI method3N4A substrate. Wherein, the innermost layer matrix is BN, and good matching with a BN interface is realized; the outermost layer of the substrate is Si3N4And meets the use requirements of environments such as oxidation resistance, rain erosion resistance and the like. By regulating BN and Si3N4The preparation temperature, the heat treatment condition, the deposition time and other process parameters of the matrix are changed, and the multilayer alternative BN/Si is changed3N4The microstructure and relative content of each phase in the matrix and the layer structure optimize the performance of the composite material.
Example 1
Step 1.Si3N4Preparing a whisker biscuit: mixing 30% of Si by volume fraction3N4Dissolving whiskers and 1.5 wt.% of dispersant polyacrylamide in deionized water, adding 5 wt.% of monomer AM and 0.25 wt.% of cross-linking agent MBAM into the deionized water, performing ball milling and dispersing for 24 hours, uniformly mixing the slurry, removing bubbles in vacuum for 10 minutes, adding 0.4 wt.% of initiator APS and 0.02 wt.% of catalyst TEMED, uniformly stirring, pouring the mixture into a mold, and molding to obtain Si3N4Biscuit of whisker;
step 2.Si3N4Drying of the whisker biscuit: naturally drying the whisker biscuit in the step 1 at room temperature for 36h, and then placing the whisker biscuit in an oven at 80 ℃ for drying;
step 3.Si3N4And (3) gel discharging of the whisker biscuit: putting the dried biscuit in a muffle furnace, and carrying out empty burning at 500 ℃ for 3h to remove the glue to obtain Si3N4Preparing a whisker preform;
and 4, preparing a BN interface: by using CVI process on Si3N4And depositing a BN interface in the whisker preform. Precursor gas of BN interface is prepared from BCl3、NH3、H2And Ar, the technological parameters are as follows: proportion of reaction gas [ BCl3]/[NH3]1/3, the system pressure is 1KPa, the deposition temperature is 1100 ℃, the deposition time is 2h, the thickness of the BN interface is 800nm, and the Si containing the BN interface is treated3N4And (3) placing the whisker preform in a high-temperature furnace for heat treatment, wherein the treatment temperature is 1300 ℃, and the treatment time is 2 h.
Step 5, preparation of a multilayer matrix: si on BN interface by CVI process3N4Multilayer BN/Si alternate deposition in whisker preform3N4A substrate. The deposition process of the BN matrix is similar to that of the BN interface in step 4 of the example, except that the deposition time is 4.5 hours. CVI preparation of Si3N4The substrate and the precursor are made of SiCl4、NH3Ar and H2The process parameters are as follows: proportion of reaction gas [ SiCl ]4]/[NH3]1/2, the system pressure was 1KPa, the reaction temperature was 800 ℃, and the deposition time was 5 h. Multilayer alternating BN/Si3N4Layer structure parameters: the innermost layer is BN, and the outermost layer is Si3N4Each layer of BN and Si3N4The porosity of the finally obtained composite material was 24 vol% with the total number of substrates of 2 μm and the number of layers of 5
Example 2
Step 1.Si3N4Preparing a whisker biscuit: mixing 35% of Si by volume fraction3N4Dissolving crystal whiskers and 1.5 wt.% of dispersant polyacrylamide in deionized water, adding 5 wt.% of monomer AM and 0.25 wt.% of cross-linking agent MBAM into the deionized water, ball-milling and dispersing the mixture for 28 hours, uniformly mixing the slurry, removing bubbles in vacuum for 10 minutes, adding 0.35 wt.% of initiator APS and 0.02 wt.% of catalyst TEMED, stirring the mixture, and adding water to obtain the final productEvenly mixed and poured into a mould to obtain Si after molding3N4Biscuit of whisker;
step 2.Si3N4Drying of the whisker biscuit: naturally drying the whisker biscuit in the step 1 at room temperature for 36h, and then placing the whisker biscuit in an oven at 80 ℃ for drying;
step 3.Si3N4And (3) gel discharging of the whisker biscuit: putting the dried biscuit in a muffle furnace, and carrying out empty burning at 500 ℃ for 3h to remove the glue to obtain Si3N4Preparing a whisker preform;
and 4, preparing a BN interface: by using CVI process on Si3N4And depositing a BN interface in the whisker preform. The deposition process was similar to that of step 4 of example 1, except that the deposition time was 2.5 hours, the BN interface thickness was 1000nm, and the Si-containing BN interface was treated3N4And (3) placing the whisker preform in a high-temperature furnace for heat treatment, wherein the treatment temperature is 1300 ℃, and the treatment time is 4 h.
Step 5, preparation of a multilayer matrix: si containing interface by CVI process3N4Multilayer BN/Si alternate deposition in whisker preform3N4A substrate. BN and Si3N4The substrate deposition process was similar to that in step 5 of example 1, except that the deposition time of BN substrate was 6 hours, and Si was added3N4The deposition time of the substrate was 7 h. Multilayer alternating BN/Si3N4Layer structure parameters: the innermost layer is BN, and the outermost layer is Si3N4Each layer of BN and Si3N4The matrixes are all 2.5 mu m, the number of layers is 4, and the porosity of the finally prepared composite material is 18 vol.%.
Example 3
Step 1.Si3N4Preparing a whisker biscuit: mixing 40% of Si by volume fraction3N4Dissolving crystal whiskers and 1.5 wt.% of dispersant polyacrylamide in deionized water, adding 4 wt.% of monomer AM and 0.2 wt.% of cross-linking agent MBAM into the deionized water, ball-milling and dispersing the mixture for 32 hours, uniformly mixing the slurry, removing bubbles in vacuum for 10 minutes, adding 0.35 wt.% of initiator APS and 0.02 wt.% of catalyst TEMED, uniformly stirring, and pouringIn a mold, Si is obtained after molding3N4Biscuit of whisker;
step 2.Si3N4Drying of the whisker biscuit: naturally drying the whisker biscuit in the step 1 at room temperature for 32h, and then placing the whisker biscuit in an oven at 80 ℃ for drying;
step 3.Si3N4And (3) gel discharging of the whisker biscuit: putting the dried biscuit in a muffle furnace, and carrying out empty burning and glue discharging at 600 ℃ for 3h to obtain Si3N4Preparing a whisker preform;
and 4, preparing a BN interface: by using CVI process on Si3N4And depositing a BN interface in the whisker preform. The deposition process was similar to that of step 4 of examples 1 and 2, except that the deposition time was 3 hours, yielding a BN interface thickness of 1200 nm.
Step 5, preparation of a multilayer matrix: si containing interface by CVI process3N4Multilayer BN/Si alternate deposition in whisker preform3N4A substrate. BN and Si3N4The substrate deposition process was similar to that of examples 1 and 2, step 5, except that the BN substrate deposition time was 3.5 hours, and Si was present3N4The deposition time of the substrate was 7 h. Multilayer alternating BN/Si3N4Layer structure parameters: the innermost layer is BN, and the outermost layer is Si3N4BN thickness per layer and Si3N4The substrates were 1.5 μm and 2.5 μm, respectively, and the number of layers was 5. Preparation of multilayer alternating BN/Si3N4And (3) carrying out heat treatment on the composite material after the substrate, wherein the heat treatment temperature is 1300 ℃, the heat treatment time is 2 hours, and the porosity of the finally prepared composite material is 16 vol.%.
Example 4
Step 1.Si3N4Preparing a whisker biscuit: mixing 45% of Si by volume fraction3N4Dissolving crystal whiskers and 1.5 wt.% of dispersant polyacrylamide in deionized water, wherein a pH regulator is tetramethylammonium hydroxide, the pH value is adjusted to be 11, then adding 4 wt.% of monomer AM and 0.2 wt.% of cross-linking agent MBAM, performing ball milling and dispersing for 36 hours, uniformly mixing slurry, removing bubbles in vacuum for 10 minutes, adding 0.25 wt.% of initiator APS and 0.02 wt.% of catalyst TEMED, stirring, and stirringEvenly mixed and poured into a mould to obtain Si after molding3N4Biscuit of whisker;
step 2.Si3N4Drying of the whisker biscuit: naturally drying the whisker biscuit in the step 1 at room temperature for 36h, and then placing the whisker biscuit in an oven at 80 ℃ for drying;
step 3.Si3N4And (3) gel discharging of the whisker biscuit: putting the dried biscuit in a muffle furnace, and carrying out empty burning at 500 ℃ for 3h to remove the glue to obtain Si3N4Preparing a whisker preform;
and 4, preparing a BN interface: by using CVI process on Si3N4And depositing a BN interface in the whisker preform. The deposition process was similar to step 4 of examples 1, 2 and 3, except that the deposition time was 3.5 hours, resulting in a BN interface thickness of 1500 nm.
Step 5, preparation of a multilayer matrix: si containing interface by CVI process3N4Multilayer BN/Si alternate deposition in whisker preform3N4A substrate. BN and Si3N4The substrate deposition process was similar to that of examples 1, 2 and 3, step 5, except that the BN substrate deposition time was 6 hours, Si was added3N4The deposition time of the substrate was 3 h. Multilayer alternating BN/Si3N4Layer structure parameters: the innermost layer is BN, and the outermost layer is Si3N4BN thickness per layer and Si3N4The substrates were 2.5 μm and 1.5 μm, respectively, and the number of layers was 4. Preparation of multilayer alternating BN/Si3N4And (3) carrying out heat treatment on the composite material after the substrate, wherein the heat treatment temperature is 1300 ℃, the heat treatment time is 2 hours, and the porosity of the finally prepared composite material is 18 vol.%.
Claims (2)
1. A preparation method of a high-temperature-resistant high-strength and high-toughness silicon nitride-based wave-transmitting composite material is characterized by comprising the following steps of: the composite material is multilayer alternating BN/Si3N4The substrate, the innermost layer is BN substrate, and the middle layer is alternative BN/Si3N4A substrate with Si as the outermost layer3N4A substrate;
the preparation method comprises the following steps:
step 1, Si3N4Preparing a whisker biscuit: si with the volume fraction of 20-50%3N4Dissolving crystal whiskers and 1.5-2.5 wt.% of dispersant polyacrylamide in deionized water, and adding tetramethylammonium hydroxide as a pH value regulator to regulate the pH value of the slurry to 9-11; adding 4-10 wt.% of monomer acrylamide AM and 0.2-1.0 wt.% of cross-linking agent methylene bisacrylamide MBAM, ball-milling for 24-36 h, and removing bubbles in vacuum for 10 min; then adding 0.2-0.5 wt.% of initiator ammonium persulfate APS and 0.02-0.1 wt.% of catalyst tetramethylethylenediamine TEMED, stirring, pouring into a mold, and molding to obtain Si3N4Biscuit of whisker;
step 2: mixing Si3N4Naturally drying the whisker biscuit at room temperature for 12-36 h, and then drying in an oven at 50-100 ℃; then placing the mixture in a muffle furnace, and carrying out empty burning and glue discharging for 2-4 h at 400-700 ℃ to obtain Si3N4Preparing a whisker preform;
step 3, preparing an interface: mixing Si3N4Placing the whisker preform in a deposition furnace, and preparing a BN interface by adopting a CVI method, wherein the thickness of the interface is 0.8-1.5 mu m; si containing BN interface may then be added3N4Placing the whisker preform in a high-temperature furnace for heat treatment, wherein the treatment temperature is 1300 ℃, and the treatment time is 2-6 h;
step 4, preparation of a matrix: si containing BN interface obtained in step 33N4The whisker preform is placed in a deposition furnace, and multilayer alternative BN/Si is prepared by adopting a CVI method3N4The substrate, the innermost layer is BN substrate, and the middle layer is alternative BN/Si3N4A substrate with Si as the outermost layer3N4A substrate.
2. The preparation method of the high-temperature-resistant high-strength-and-toughness silicon nitride-based wave-transmitting composite material according to claim 1, which is characterized by comprising the following steps of: said step 1Si3N4And the whisker preform is molded by gel injection molding.
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| CN110156484B (en) * | 2019-05-13 | 2021-10-22 | 西北工业大学 | BN/Si3N4Whisker preform and preparation method adopting gel injection molding |
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| CN112898038B (en) * | 2021-03-22 | 2022-06-10 | 河海大学 | Preparation method of silicon nitride-based fiber monolithic ceramic wave-transmitting material |
| CN113200765B (en) * | 2021-05-13 | 2022-10-25 | 湖南世鑫新材料有限公司 | Si-containing alloy 3 N 4 Carbon-ceramic composite material crucible with BN composite coating and preparation method thereof |
| CN113248263B (en) * | 2021-05-25 | 2022-11-22 | 西北工业大学 | Si 3 N 4w Si preform and preparation of Si using the same 3 N 4w /Si 3 N 4 Method for compounding materials |
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