CN110078517B - Mixed-woven fiber reinforced nitride composite material radome and preparation method thereof - Google Patents
Mixed-woven fiber reinforced nitride composite material radome and preparation method thereof Download PDFInfo
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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Abstract
The invention discloses a mixed fiber reinforced nitride composite material antenna housing and a preparation method thereof, wherein the method comprises the following steps: (1) preparing a fiber preform: the radome head is completely woven by BN fibers, a mode that the BN fibers and the quartz fibers are mixed and woven in a region from the radome head to a next cone is adopted, and the volume ratio of the BN fibers to the quartz fibers is (3-4): (2-1), weaving a second cone area at the root part by using quartz fibers; (2) removing the wetting agent on the surface of the fiber preform; (3) carrying out dipping forming and cracking ceramic treatment; (4) after precision processing, carrying out impregnation forming and cracking ceramic treatment again; (5) carrying out ceramic treatment at 850-1000 ℃. The preparation method of the hybrid fiber reinforced nitride composite radome, disclosed by the embodiment of the invention, can meet the requirements of the radome on high temperature resistance and accurate striking, does not influence other performances, saves the consumption of BN fiber, and can meet the preparation requirement of a large-size radome.
Description
Technical Field
The invention relates to an antenna housing and a preparation method thereof, in particular to a hybrid fiber reinforced nitride composite material antenna housing and a preparation method thereof.
Background
Along with the development of aerospace technology, the flying speed of a missile is higher and higher, the flying speed of certain novel missiles can reach 20Ma, the stagnation point temperature of a radome which is a key part of the missile can reach more than 2500 ℃ due to harsh aerodynamic heat, the existing mature quartz fiber reinforced quartz composite material can resist the temperature of 1200 ℃ for a long time, and the head part of the radome has larger change of the aerodynamic shape of the radome due to large loss on ignition, so that the requirement of accurate striking can not be met.
The BN fiber reinforced nitride composite material can meet the use requirement of more than 2500 ℃. But the production quantity of the BN fiber is limited at present, and the preparation of the cover body cannot be met.
Disclosure of Invention
Based on the prior art, the invention aims to provide a hybrid fiber reinforced nitride composite material radome and a preparation method thereof, and solves the problems that the radome in the prior art cannot be produced in a large scale and is high-temperature resistant, the pneumatic appearance of the radome is changed greatly, and accurate striking cannot be met.
In a first aspect, an embodiment of the present application provides a method for preparing a hybrid fiber reinforced nitride composite radome, including the following steps:
(1) preparation of a fiber preform (preferred: 2.5D braided structure): the radome head is completely woven by BN fibers, a mode that the BN fibers and the quartz fibers are mixed and woven in a region from the radome head to a next cone is adopted, and the volume ratio of the BN fibers to the quartz fibers is (3-4): (2-1), weaving a second cone area at the root part by using quartz fibers;
(2) removing the wetting agent on the surface of the fiber preform;
(3) carrying out dipping forming and cracking ceramic treatment until weight is not increased;
(4) after precision processing, carrying out impregnation molding and cracking ceramic treatment again until weight is not increased any more;
(5) and carrying out ceramic treatment at 850-1000 ℃ to obtain the hybrid fiber reinforced nitride composite material radome.
Preferably: and (2) preparing a fiber preform by adopting a 2.5D weaving structure in the step (1).
Preferably: the specific steps of the step (2) are as follows: and removing the wetting agent on the surface of the fiber preform by adopting a mode of combining benzene solution soaking and heat treatment. Further: the heat treatment temperature is 400-600 ℃.
Preferably: the specific steps of the step (3) are as follows: the method adopts the liquid phase dipping molding of the silicon boron oxygen nitrogen precursor, and the dipping process adopts a mode of combining vacuum and high pressure. The vacuum degree is 5-15Pa, and the pressure is 5-10 MPa. Further: the high pressure process adopts nitrogen as a pressure gas source, and gel curing is carried out at RT-90 ℃.
Preferably: the cracking atmosphere of the cracking ceramic treatment in the step (3) is nitrogen or ammonia, and the cracking temperature is 600-800 ℃.
Preferably: and (4) adopting a dry grinding mode in the precision machining process in the step (4).
Preferably: the ceramic treatment temperature in the step (5) is as follows: 850-1000 ℃.
In a second aspect, an embodiment of the present application provides an antenna cover prepared by any one of the above methods for preparing a hybrid fiber reinforced nitride composite material antenna cover.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method of the hybrid fiber reinforced nitride composite radome, disclosed by the embodiment of the invention, can meet the requirements of the radome on high temperature resistance and accurate striking, does not influence other performances, saves the consumption of BN fiber, and can meet the preparation requirement of a large-size radome.
2. According to the preparation method of the mixed-woven fiber reinforced nitride composite material radome disclosed by the embodiment of the invention, the head part can resist the high-temperature ablation resistance requirement of 2500 ℃, meanwhile, the fiber mixed-woven mode is adopted, the preparation method is simple, and the preparation method is suitable for industrial mass production of radomes.
Detailed Description
In order to better understand the technical solution of the present invention, the following embodiments are provided to further explain the present invention.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
Example one
(1) Preparing a fiber preform by adopting a 2.5D weaving structure, weaving quartz fibers and BN fibers in a mixed weaving mode, weaving the BN fibers at the head of the radome, weaving the BN fibers and the quartz fibers in a mixed weaving mode from the head to the next cone region, wherein the volume ratio of the BN fibers to the quartz fibers is 3:2, and the requirements on temperature resistance and strength are met; the root part secondary cone area is completely woven by quartz fibers, so that the strength requirement is met.
(2) Removing the wetting agent on the surface of the fiber preform by adopting a mode of combining benzene solution soaking and heat treatment, wherein the heat treatment temperature is 400 ℃;
(3) the method adopts the liquid phase dipping molding of the silicon boron oxygen nitrogen precursor, the dipping process adopts a mode of combining vacuum and high pressure, the vacuum degree is 10Pa, the pressure is 5-10MPa, and the high pressure process adopts nitrogen as a pressure gas source. And gel curing at 25 ℃;
(4) carrying out cracking ceramic treatment on the gelled fiber reinforced silicon-boron-oxygen-nitrogen composite material, wherein the cracking atmosphere is nitrogen or ammonia, and the cracking temperature is 800 ℃;
(5) circularly dipping, cracking and ceramizing according to the technical processes of the (3) and (4) until weight is not increased any more;
(6) performing precision machining in a dry grinding mode;
(7) after the precision machining is finished, circularly dipping, cracking and ceramizing the technical processes (3) and (4) until weight is not increased any more;
(8) and carrying out ceramic treatment at 1000 ℃ to obtain the hybrid fiber reinforced nitride composite material radome.
Example 2
(1) Preparing a fiber preform by adopting a 2.5D weaving structure, weaving quartz fibers and BN fibers in a mixed weaving mode, weaving the BN fibers at the head of the radome, weaving the BN fibers and the quartz fibers in a mixed weaving mode from the head to the next cone region, wherein the volume ratio of the BN fibers to the quartz fibers is 2:1, and the requirements on temperature resistance and strength are met; the root part secondary cone area is completely woven by quartz fibers, so that the strength requirement is met.
(2) Removing the wetting agent on the surface of the fiber preform by adopting a mode of combining benzene solution soaking and heat treatment, wherein the heat treatment temperature is 450 ℃;
(3) adopting a liquid phase dipping forming of a silicon boron oxygen nitrogen precursor, wherein the dipping process adopts a mode of combining vacuum and high pressure, the vacuum degree is 10Pa, the pressure is 5-10MPa, the high pressure process adopts nitrogen as a pressure gas source, and the gel is solidified at 55 ℃;
(4) carrying out cracking ceramic treatment on the gelled fiber reinforced silicon-boron-oxygen-nitrogen composite material, wherein the cracking atmosphere is nitrogen or ammonia, and the cracking temperature is 750 ℃;
(5) circularly dipping, cracking and ceramizing according to the technical processes of the (3) and (4) until weight is not increased any more;
(6) performing precision machining in a dry grinding mode;
(7) after the precision machining is finished, circularly dipping, cracking and ceramizing the technical processes (3) and (4) until weight is not increased any more;
(8) and carrying out ceramic treatment at 950 ℃ to obtain the hybrid fiber reinforced nitride composite material radome.
Example 3
(1) Preparing a fiber preform by adopting a 2.5D weaving structure, weaving quartz fibers and BN fibers in a mixed weaving mode, weaving the BN fibers at the head part of the radome completely, weaving the BN fibers and the quartz fibers in a mixed weaving mode in a large area from the head part to the next cone, wherein the volume ratio of the BN fibers to the quartz fibers is 5:2, and the temperature resistance and strength requirements are met; the root part secondary cone area is completely woven by quartz fibers, so that the strength requirement is met.
(2) Removing the wetting agent on the surface of the fiber preform by adopting a mode of combining benzene solution soaking and heat treatment, wherein the heat treatment temperature is 500 ℃;
(3) adopting a liquid phase dipping forming of a silicon boron oxygen nitrogen precursor, wherein the dipping process adopts a mode of combining vacuum and high pressure, the vacuum degree is 13-15Pa, the pressure is 5MPa, the high pressure process adopts nitrogen as a pressure gas source, and the gel is solidified at 80 ℃;
(4) carrying out cracking ceramic treatment on the gelled fiber reinforced silicon-boron-oxygen-nitrogen composite material, wherein the cracking atmosphere is nitrogen or ammonia, and the cracking temperature is 650 ℃;
(5) circularly dipping, cracking and ceramizing according to the technical processes of the (3) and (4) until weight is not increased any more;
(6) performing precision machining in a dry grinding mode;
(7) after the precision machining is finished, circularly dipping, cracking and ceramizing the technical processes (3) and (4) until weight is not increased any more;
(8) and carrying out ceramic treatment at 850 ℃ to obtain the hybrid fiber reinforced nitride composite material radome.
Example 4
(1) Preparing a fiber preform by adopting a 2.5D weaving structure, weaving quartz fibers and BN fibers in a mixed weaving mode, weaving the BN fibers at the head part of the radome completely, weaving the BN fibers and the quartz fibers in a mixed weaving mode in a large area from the head part to the next cone, wherein the volume ratio of the BN fibers to the quartz fibers is 4:1, and the requirements on temperature resistance and strength are met; the root part secondary cone area is completely woven by quartz fibers, so that the strength requirement is met.
(2) Removing the wetting agent on the surface of the fiber preform by adopting a mode of combining benzene solution soaking and heat treatment, wherein the heat treatment temperature is 600 ℃;
(3) adopting a liquid phase dipping forming of a silicon boron oxygen nitrogen precursor, wherein the dipping process adopts a mode of combining vacuum and high pressure, the vacuum degree is 5-7Pa, the pressure is 10MPa, the high pressure process adopts nitrogen as a pressure gas source, and the gel is solidified at 90 ℃;
(4) carrying out cracking ceramic treatment on the gelled fiber reinforced silicon-boron-oxygen-nitrogen composite material, wherein the cracking atmosphere is nitrogen or ammonia, and the cracking temperature is 700 ℃;
(5) circularly dipping, cracking and ceramizing according to the technical processes of the (3) and (4) until weight is not increased any more;
(6) performing precision machining in a dry grinding mode;
(7) after the precision machining is finished, circularly dipping, cracking and ceramizing the technical processes (3) and (4) until weight is not increased any more;
(8) and carrying out ceramic treatment at 890 ℃ to obtain the hybrid fiber reinforced nitride composite material radome.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (7)
1. A preparation method of a hybrid fiber reinforced nitride composite material radome is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a fiber preform: the radome head is completely woven by BN fibers, a mode that the BN fibers and the quartz fibers are mixed and woven in a region from the radome head to a next cone is adopted, and the volume ratio of the BN fibers to the quartz fibers is (3-4): (2-1), weaving a second cone area at the root part by using quartz fibers;
(2) removing the wetting agent on the surface of the fiber preform;
(3) carrying out dipping forming and cracking ceramic treatment until weight is not increased;
(4) after precision processing, carrying out impregnation molding and cracking ceramic treatment again until weight is not increased any more;
(5) performing ceramic treatment at 850-1000 ℃ to obtain the hybrid fiber reinforced nitride composite material radome;
the specific steps of the step (3) are as follows: adopting a liquid phase dipping forming of a silicon boron oxygen nitrogen precursor, wherein the dipping process adopts a mode of combining vacuum and high pressure, the vacuum degree is 5-15Pa, and the pressure is 5-10 MPa;
the cracking atmosphere of the cracking ceramic treatment in the step (3) is nitrogen or ammonia, and the cracking temperature is 600-800 ℃.
2. The method for preparing the hybrid fiber reinforced nitride composite material radome of claim 1, which is characterized in that: and (2) preparing a fiber preform by adopting a 2.5D weaving structure in the step (1).
3. The method for preparing the hybrid fiber reinforced nitride composite material radome of claim 1, which is characterized in that: the specific steps of the step (2) are as follows: and removing the wetting agent on the surface of the fiber preform by adopting a mode of combining benzene solution soaking and heat treatment.
4. The method for preparing the hybrid fiber reinforced nitride composite material radome of claim 3, which is characterized in that: the heat treatment temperature is 400-600 ℃.
5. The method for preparing the hybrid fiber reinforced nitride composite material radome of claim 1, which is characterized in that: the high pressure process adopts nitrogen as a pressure gas source, and gel curing is carried out at RT-90 ℃.
6. The method for preparing the hybrid fiber reinforced nitride composite material radome of claim 1, which is characterized in that: and (4) adopting a dry grinding mode in the precision machining process in the step (4).
7. The radome prepared by the method for preparing the hybrid fiber reinforced nitride composite radome of any one of claims 1-6.
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| CN112110733B (en) * | 2020-11-20 | 2021-02-26 | 北京玻钢院复合材料有限公司 | Ceramic fiber hybrid fabric reinforced ceramic matrix composite and preparation method thereof |
| CN115636683A (en) * | 2022-12-08 | 2023-01-24 | 北京玻钢院复合材料有限公司 | Fiber mixed fabric reinforced quartz-based composite material and preparation method thereof |
| CN116444283A (en) * | 2023-03-24 | 2023-07-18 | 山东理工大学 | Continuous carbon fiber toughening ultra-high temperature ceramic matrix composite material and preparation method thereof |
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