CN103664213A - Preparation method of high-temperature wave-transparent composite material toughened by hybrid-woven fibers - Google Patents
Preparation method of high-temperature wave-transparent composite material toughened by hybrid-woven fibers Download PDFInfo
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- CN103664213A CN103664213A CN201210337246.9A CN201210337246A CN103664213A CN 103664213 A CN103664213 A CN 103664213A CN 201210337246 A CN201210337246 A CN 201210337246A CN 103664213 A CN103664213 A CN 103664213A
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- phosphate sol
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- 239000000835 fiber Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 title claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 25
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 18
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 229910052582 BN Inorganic materials 0.000 claims abstract description 9
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 9
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229940001007 aluminium phosphate Drugs 0.000 claims description 12
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 7
- 238000009954 braiding Methods 0.000 claims description 5
- 238000006424 Flood reaction Methods 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 4
- 238000005470 impregnation Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000009941 weaving Methods 0.000 abstract 2
- 238000009940 knitting Methods 0.000 abstract 1
- 239000010453 quartz Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 238000007669 thermal treatment Methods 0.000 abstract 1
- 239000012780 transparent material Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 6
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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Abstract
The invention provides a preparation method of a high-temperature wave-transparent composite material toughened by hybrid-woven fibers. The preparation method comprises the following steps: (1), weaving boron nitride fibers, high silica fibers and quartz fibers into prefab forms in a hybrid manner by virtue of a weaving method or a knitting method, wherein the prefab types are 2.5-dimensional or 3-dimensional forms; (2), mixing phosphoric acid in a certain mass fraction with aluminum hydroxide, adding deionized water and sufficiently stirring until mixing uniformly, and standing for 2 hours-4 hours to prepare aluminum phosphate sol; (3), placing fiber prefabs in the prepared aluminum phosphate sol, and sufficiently impregnating; (4), placing the fiber prefabs impregnated by the aluminum phosphate sol into an oven for carrying out a thermal-treatment drying process; (5), placing a dried composite material at 700 DEG C-900 DEG C for sintering and treating for 1 hour-2 hours; and (6), repeating the processes in step (3) to step (5) for 5-7 times to prepare the compact composite material. According to the invention, the technical process is relatively simple, easy to operate and low in cost; and the prepared composite material has very good high temperature resistance and wave-transparent performance.
Description
Technical field
The present invention relates to a kind of preparation method of wave-penetrating composite material, particularly relate to the preparation method of the fiber reinforced high temperature wave-penetrating composite material of a kind of shuffling.
Background technology
High temperature wave-transparent material is a kind of dielectric material that has resistance to elevated temperatures and wave penetrate capability concurrently, it is the basis of high speed precise guidance spacecraft, be one of development hypersonic speed surface-to-air ballistic missile, antiradiation missile and the indispensable gordian technique of cruise missile, it is directly restricting the development of advanced spacecraft.Pneumatic friction heating during high-speed flight can cause aircraft to produce huge thermal stresses, especially aircraft radome material.In order to bear various load, aircraft radome material intensity is higher, and material must have good fracture toughness property simultaneously.Due under hot conditions, all can there is obvious variation in the dielectric properties of conventional electromagnetic wave transparent material and intensity, so the exploitation of high temperature wave-penetrating composite material seems and is even more important.
There is larger input in the developed country such as the U.S., Russia in high temperature wave-transparent material field always, and has obtained significant achievement, and some novel materials and preparation technology have reached practical standard.Electromagnetic wave transparent material is mainly divided into organic electromagnetic wave transparent material and inorganic electromagnetic wave transparent material, i.e. so-called polymer electromagnetic wave transparent material and ceramic wave-transmitting material.Polymer electromagnetic wave transparent material mainly comprises fiber reinforcement various types of resins matrix material.Ceramic wave-transmitting material comprises the ceramic composites such as alumina-ceramic, silicon nitride ceramics and glass fibre and adaptation fiber reinforcement silicon oxide.The specific inductivity of quartz-ceramics is very stable to frequency and temperature, and thermal shock resistance is good, but because its porosity is high, the easy moisture absorption, rainresistance is poor.Silicon nitride ceramics has high strength, the feature that high temperature resistant, thermal shock resistance is good, but its easy-sintering not.
Aluminum phosphate fusing point is greater than 1500 ℃, at high temperature not melting, the feature such as that aluminophosphate-based matrix material has is high temperature resistant, high strength, dielectric properties are excellent, anti-oxidant and good structure designability, thermal expansivity are little, it is ideal material high temperature resistant, low-dielectric loss, can meet multiple particular requirement, therefore, aluminum phosphate is one of desirable body material of high temperature wave-transparent material.
Summary of the invention
Problem to be solved by this invention is the preparation method who proposes the fiber reinforced high temperature wave-penetrating composite material of a kind of shuffling.
Operating process:
(1) boron nitride fibre is become to prefabricated component form with silica fiber by method shuffling woven or braiding with high silica fiber, prefabricated component type can be 2.5 dimensions or 3 dimension forms, and fiber volume fraction is controlled between 30%～45%;
(2) phosphoric acid of certain mass mark is mixed with aluminium hydroxide, and add deionized water, be stirred well to even mixing, after standing 2～4 hours, make aluminium phosphate sol, wherein the mol ratio of phosphoric acid and aluminium hydroxide is controlled between 0.9～1.1;
(3) fiber preform is placed in the aluminium phosphate sol of preparation, fully floods, impregnation pressure is 2～5MPa;
(4) fiber preform after aluminium phosphate sol dipping is placed in baking oven and heat-treated stoving process;
(5) matrix material after drying and processing is placed at 700～900 ℃ to sintering processes 1～2 hour;
(6) repeat (3)～(5) operation 5～7 times.
Wherein:
In prefabricated component after shuffling, boron nitride fibre is positioned at outermost layer, and middle layer is high silica fiber, and innermost layer is silica fiber, outer in the Thickness Ratio of interior three layers of fiber be 1: 1: 1～3.
Stoving process is for to rise to 90～110 ℃ from room temperature, temperature rise rate is 2～3 ℃ of per minutes, then, at 90～110 ℃ of insulation 40-60 minute, then makes temperature rise to 160～170 ℃, temperature rise rate is 2～3 ℃ of per minutes, then 160～170 ℃ of insulations 3～5 hours.
In the present invention, major advantage is: (1) technological process is relatively simple, easy to operate, and cost is low; (2) matrix material of preparing is high temperature resistant very good with wave penetrate capability.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims to the modification of the various equivalent form of values of the present invention and limit.
Embodiment 1
(1) boron nitride fibre is become to prefabricated component form with silica fiber by method shuffling woven or braiding with high silica fiber, prefabricated component type can be 3 dimension braidings, it is 40% that fiber volume fraction is controlled, in prefabricated component after shuffling, boron nitride fibre is positioned at outermost layer, middle layer is high silica fiber, innermost layer is silica fiber, outer in the Thickness Ratio of interior three layers of fiber be 1: 1: 1;
(2) phosphoric acid of certain mass mark is mixed with aluminium hydroxide, and add deionized water, be stirred well to even mixing, after standing 34 hours, make aluminium phosphate sol, wherein the control of the mol ratio of phosphoric acid and aluminium hydroxide is 1;
(3) fiber preform is placed in the aluminium phosphate sol of preparation, fully floods, impregnation pressure is 4MPa;
(4) fiber preform after aluminium phosphate sol dipping is placed in baking oven and heat-treated stoving process, stoving process is for to rise to 100 ℃ from room temperature, temperature rise rate is 3 ℃ of per minutes, then 100 ℃ of insulations 60 minutes, then make temperature rise to 160 ℃, temperature rise rate is 2 ℃ of per minutes, then at 160 ℃, is incubated 4 hours.
(5) matrix material after drying and processing is placed at 700 ℃ to sintering processes 1 hour;
(6) repeat (3)～(5) operation 5 times.
Embodiment 2
(1) boron nitride fibre is become to prefabricated component form with silica fiber by method shuffling woven or braiding with high silica fiber, prefabricated component type is that 2.5 dimensions are woven, and it is 35% that fiber volume fraction is controlled; In prefabricated component after shuffling, boron nitride fibre is positioned at outermost layer, and middle layer is high silica fiber, and innermost layer is silica fiber, outer in the Thickness Ratio of interior three layers of fiber be 1: 1: 3;
(2) phosphoric acid of certain mass mark is mixed with aluminium hydroxide, and add deionized water, be stirred well to even mixing, after standing 2 hours, make aluminium phosphate sol, wherein the control of the mol ratio of phosphoric acid and aluminium hydroxide is 1.1;
(3) fiber preform is placed in the aluminium phosphate sol of preparation, fully floods, impregnation pressure is 5MPa;
(4) fiber preform after aluminium phosphate sol dipping is placed in baking oven and heat-treated stoving process, stoving process is for to rise to 110 ℃ from room temperature, temperature rise rate is 3 ℃ of per minutes, then 110 ℃ of insulations 45 minutes, then make temperature rise to 170 ℃, temperature rise rate is 3 ℃ of per minutes, then 170 ℃ of insulations 3 hours.
(5) matrix material after drying and processing is placed at 800 ℃ to sintering processes 2 hours;
(6) repeat (3)～(5) operation 6 times.
Above are only single embodiment of the present invention, but design concept of the present invention is not limited to this, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content that does not depart from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (3)
1. a preparation method for the fiber reinforced high temperature wave-penetrating composite material of shuffling, its feature comprises the step of following order:
(1) boron nitride fibre is become to prefabricated component form with silica fiber by method shuffling woven or braiding with high silica fiber, prefabricated component type can be 2.5 dimensions or 3 dimension forms, and fiber volume fraction is controlled between 30%～45%;
(2) phosphoric acid of certain mass mark is mixed with aluminium hydroxide, and add deionized water, be stirred well to even mixing, after standing 2～4 hours, make aluminium phosphate sol, wherein the mol ratio of phosphoric acid and aluminium hydroxide is controlled between 0.9～1.1;
(3) fiber preform is placed in the aluminium phosphate sol of preparation, fully floods, impregnation pressure is 2～5MPa;
(4) fiber preform after aluminium phosphate sol dipping is placed in baking oven and heat-treated stoving process;
(5) matrix material after drying and processing is placed at 700～900 ℃ to sintering processes 1～2 hour;
(6) repeat (3)～(5) operation 5～7 times.
2. according to the method described in claims 1, it is characterized in that in the prefabricated component after shuffling, boron nitride fibre is positioned at outermost layer, middle layer is high silica fiber, and innermost layer is silica fiber, outer in the Thickness Ratio of interior three layers of fiber be 1: 1: 1～3.
3. according to the method described in claims 1, it is characterized in that stoving process is to rise to 90～110 ℃ from room temperature, temperature rise rate is 2～3 ℃ of per minutes, then at 90～110 ℃ of insulation 40-60 minute, then make temperature rise to 160～170 ℃, temperature rise rate is 2～3 ℃ of per minutes, then 160～170 ℃ of insulations 3～5 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210337246.9A CN103664213B (en) | 2012-09-13 | 2012-09-13 | The preparation method of the high-temperature wave-transparent composite that a kind of shuffling is fiber reinforced |
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| CN201210337246.9A CN103664213B (en) | 2012-09-13 | 2012-09-13 | The preparation method of the high-temperature wave-transparent composite that a kind of shuffling is fiber reinforced |
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| Publication Number | Publication Date |
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| CN103664213A true CN103664213A (en) | 2014-03-26 |
| CN103664213B CN103664213B (en) | 2016-06-08 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058774A (en) * | 2014-06-09 | 2014-09-24 | 青岛东方循环能源有限公司 | Synthetic method of high-compactness phosphoric-acid-based wave-transmitting material |
| CN106242550A (en) * | 2016-07-22 | 2016-12-21 | 哈尔滨工业大学 | A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof |
| CN108148548A (en) * | 2016-12-05 | 2018-06-12 | 航天特种材料及工艺技术研究所 | A kind of anti-weathering wave transparent antenna house of high temperature resistant and preparation method thereof |
| CN108455995A (en) * | 2018-02-09 | 2018-08-28 | 青海大学 | A kind of silicon carbide fibre enhancing aluminum phosphate ceramic matric composite and preparation method thereof |
| CN110078517A (en) * | 2019-04-11 | 2019-08-02 | 山东工业陶瓷研究设计院有限公司 | A kind of shuffling fiber reinforcement nitride ceramic composites antenna house and preparation method thereof |
| CN110981407A (en) * | 2019-11-21 | 2020-04-10 | 航天特种材料及工艺技术研究所 | Boron aluminum phosphate resin composite material and preparation method and application thereof |
| CN113526973A (en) * | 2021-09-07 | 2021-10-22 | 中国人民解放军国防科技大学 | Wave-transparent ceramic matrix composite with double interface phases and preparation method thereof |
| CN115417669A (en) * | 2022-09-30 | 2022-12-02 | 武汉科技大学 | High silica glass fiber reinforced zirconium pyrophosphate-based composite material and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058774A (en) * | 2014-06-09 | 2014-09-24 | 青岛东方循环能源有限公司 | Synthetic method of high-compactness phosphoric-acid-based wave-transmitting material |
| CN104058774B (en) * | 2014-06-09 | 2016-01-20 | 青岛东方循环能源有限公司 | A kind of synthetic method of high compactness phosphate electromagnetic wave transparent material |
| CN106242550A (en) * | 2016-07-22 | 2016-12-21 | 哈尔滨工业大学 | A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof |
| CN108148548A (en) * | 2016-12-05 | 2018-06-12 | 航天特种材料及工艺技术研究所 | A kind of anti-weathering wave transparent antenna house of high temperature resistant and preparation method thereof |
| CN108148548B (en) * | 2016-12-05 | 2019-11-22 | 航天特种材料及工艺技术研究所 | A kind of anti-weathering wave transparent antenna house of high temperature resistant and preparation method thereof |
| CN108455995A (en) * | 2018-02-09 | 2018-08-28 | 青海大学 | A kind of silicon carbide fibre enhancing aluminum phosphate ceramic matric composite and preparation method thereof |
| CN110078517A (en) * | 2019-04-11 | 2019-08-02 | 山东工业陶瓷研究设计院有限公司 | A kind of shuffling fiber reinforcement nitride ceramic composites antenna house and preparation method thereof |
| CN110078517B (en) * | 2019-04-11 | 2021-12-21 | 山东工业陶瓷研究设计院有限公司 | Mixed-woven fiber reinforced nitride composite material radome and preparation method thereof |
| CN110981407A (en) * | 2019-11-21 | 2020-04-10 | 航天特种材料及工艺技术研究所 | Boron aluminum phosphate resin composite material and preparation method and application thereof |
| CN113526973A (en) * | 2021-09-07 | 2021-10-22 | 中国人民解放军国防科技大学 | Wave-transparent ceramic matrix composite with double interface phases and preparation method thereof |
| CN113526973B (en) * | 2021-09-07 | 2021-11-16 | 中国人民解放军国防科技大学 | Wave-transparent ceramic matrix composite with double interface phases and preparation method thereof |
| CN115417669A (en) * | 2022-09-30 | 2022-12-02 | 武汉科技大学 | High silica glass fiber reinforced zirconium pyrophosphate-based composite material and preparation method thereof |
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