CN103664213B - The preparation method of the high-temperature wave-transparent composite that a kind of shuffling is fiber reinforced - Google Patents
The preparation method of the high-temperature wave-transparent composite that a kind of shuffling is fiber reinforced Download PDFInfo
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- CN103664213B CN103664213B CN201210337246.9A CN201210337246A CN103664213B CN 103664213 B CN103664213 B CN 103664213B CN 201210337246 A CN201210337246 A CN 201210337246A CN 103664213 B CN103664213 B CN 103664213B
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- fiber
- shuffling
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- aluminium phosphate
- 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 14
- 239000002131 composite material Substances 0.000 title claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 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
- 229940001007 aluminium phosphate Drugs 0.000 claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 10
- 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
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 9
- 238000009954 braiding 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
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005470 impregnation Methods 0.000 claims description 4
- 238000006424 Flood reaction Methods 0.000 abstract 1
- 238000000280 densification 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
- 238000013461 design Methods 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 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
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000011161 development Methods 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
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005855 radiation 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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- Aiming, Guidance, Guns With A Light Source, Armor, Camouflage, And Targets (AREA)
Abstract
The preparation method of the high-temperature wave-transparent composite that the present invention provides a kind of shuffling fiber reinforced, comprise the following steps: boron nitride fibre is become prefabricated component form with silica fiber by method shuffling that is woven or braiding with high silica fiber by (1), and pre-forms is 2.5 dimensions or 3 dimension forms; (2) phosphoric acid by certain mass mark mixes with aluminium hydroxide, and adds deionized water, is stirred well to Homogeneous phase mixing, leaves standstill and obtains aluminium phosphate sol after 2��4 hours; (3) fiber preform is placed in the aluminium phosphate sol of preparation, fully floods; (4) fiber preform after being flooded by aluminium phosphate sol is placed in baking oven and is heat-treated stoving process; (5) sintering processes 1��2 hour at the matrix material after drying and processing being placed on 700��900 DEG C; (6) (3)��(5) operation 5��7 times, the matrix material of the densification of system is repeated. Technological process of the present invention is relatively simple, easily operates, and cost is low, and the matrix material of preparation is high temperature resistant and wave penetrate capability is very good.
Description
Technical field
The present invention relates to the preparation method of a kind of wave-penetrating composite material, particularly relate to the preparation method of the fiber reinforced high-temperature wave-transparent composite of a kind of shuffling.
Background technology
High temperature wave-transparent material is a kind of dielectric material having resistance to elevated temperatures and wave penetrate capability concurrently, it it is the basis of high speed precise guidance spacecraft, being develop one of indispensable gordian technique of hypersonic speed surface-to-air ballistic missile, counter radiation guided missile and cruise missile, it directly governs 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. Owing under the high temperature conditions, all there is obvious change in dielectric properties and the intensity of conventional electromagnetic wave transparent material, therefore the exploitation of high-temperature wave-transparent composite seems especially important.
There is bigger input in the developed country such as the U.S., Russia in high temperature wave-transparent material field always, and achieves 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 composite 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 due to its porosity height, the easy moisture absorption, rainresistance is poor. The feature that silicon nitride ceramics has high strength, high temperature resistant, thermal shock resistance is good, but its not easy-sintering.
Aluminum phosphate fusing point is greater than 1500 DEG C, at high temperature not melting, aluminophosphate-based matrix material has the features such as structure designability high temperature resistant, that high strength, dielectric properties are excellent, anti-oxidant and good, thermal expansivity be little, it it is ideal material high temperature resistant, low-dielectric loss, multiple particular requirement can be met, 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 proposing the fiber reinforced high-temperature wave-transparent composite of a kind of shuffling.
Operating process:
(1) by method shuffling that is woven or braiding, boron nitride fibre being become prefabricated component form with silica fiber with high silica fiber, pre-forms can be 2.5 dimensions or 3 dimension forms, and fiber volume fraction controls between 30%��45%;
(2) phosphoric acid by certain mass mark mixes with aluminium hydroxide, and adds deionized water, is stirred well to Homogeneous phase mixing, leaves standstill and obtains aluminium phosphate sol after 2��4 hours, and wherein the mol ratio of phosphoric acid and aluminium hydroxide controls between 0.9��1.1;
(3) being placed in the aluminium phosphate sol of preparation by fiber preform, fully flood, impregnation pressure is 2��5MPa;
(4) fiber preform after being flooded by aluminium phosphate sol is placed in baking oven and is heat-treated stoving process;
(5) sintering processes 1��2 hour at the matrix material after drying and processing being placed on 700��900 DEG C;
(6) (3)��(5) operation 5��7 times are repeated.
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, and in outer, the thickness ratio of interior three layers of fiber is 1: 1: 1��3.
Stoving process is for rise to 90��110 DEG C from room temperature, temperature rise rate be 2��3 DEG C every minute, then 90��110 DEG C be incubated 40-60 minute, then make temperature rise to 160��170 DEG C, temperature rise rate be 2��3 DEG C every minute, then 160��170 DEG C be incubated 3��5 hours.
In the present invention, major advantage is: (1) technological process is relatively simple, easily operates, and cost is low; (2) matrix material prepared is high temperature resistant and wave penetrate capability is very good.
Embodiment
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of the various equivalent form of values of the present invention is all fallen within the application's claims and is limited by those skilled in the art.
Embodiment 1
(1) boron nitride fibre is become prefabricated component form with silica fiber by method shuffling that is woven or braiding with high silica fiber, pre-forms can be 3 dimension braidings, fiber volume fraction is controlled to 40%, in prefabricated component after shuffling, boron nitride fibre is positioned at outermost layer, middle layer is high silica fiber, innermost layer is silica fiber, and in outer, the thickness ratio of interior three layers of fiber is 1: 1: 1;
(2) phosphoric acid by certain mass mark mixes with aluminium hydroxide, and adds deionized water, is stirred well to Homogeneous phase mixing, leaves standstill and obtains aluminium phosphate sol after 34 hours, and wherein the mol ratio of phosphoric acid and aluminium hydroxide is controlled to 1;
(3) being placed in the aluminium phosphate sol of preparation by fiber preform, fully flood, impregnation pressure is 4MPa;
(4) fiber preform after being flooded by aluminium phosphate sol is placed in baking oven and is heat-treated stoving process, stoving process is for rise to 100 DEG C from room temperature, temperature rise rate be 3 DEG C every minute, then it is incubated 60 minutes at 100 DEG C, then temperature is made to rise to 160 DEG C, temperature rise rate be 2 DEG C every minute, then at 160 DEG C be incubated 4 hours.
(5) sintering processes 1 hour at the matrix material after drying and processing being placed on 700 DEG C;
(6) (3)��(5) operation 5 times are repeated.
Embodiment 2
(1) by method shuffling that is woven or braiding, boron nitride fibre being become prefabricated component form with silica fiber with high silica fiber, pre-forms is that 2.5 dimensions are woven, and fiber volume fraction is controlled to 35%; 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, and in outer, the thickness ratio of interior three layers of fiber is 1: 1: 3;
(2) phosphoric acid by certain mass mark mixes with aluminium hydroxide, and adds deionized water, is stirred well to Homogeneous phase mixing, leaves standstill and obtains aluminium phosphate sol after 2 hours, and wherein the mol ratio of phosphoric acid and aluminium hydroxide is controlled to 1.1;
(3) being placed in the aluminium phosphate sol of preparation by fiber preform, fully flood, impregnation pressure is 5MPa;
(4) fiber preform after being flooded by aluminium phosphate sol is placed in baking oven and is heat-treated stoving process, stoving process is for rise to 110 DEG C from room temperature, temperature rise rate be 3 DEG C every minute, then it is incubated 45 minutes at 110 DEG C, then temperature is made to rise to 170 DEG C, temperature rise rate be 3 DEG C every minute, then 170 DEG C be incubated 3 hours.
(5) sintering processes 2 hours at the matrix material after drying and processing being placed on 800 DEG C;
(6) (3)��(5) operation 6 times are repeated.
Above are only the single embodiment of the present invention, but the design of the present invention design is not limited thereto, all changes utilizing this design that the present invention carries out unsubstantiality, all should belong to the behavior invading the scope of protection of the invention. In every case being the content not departing from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling above embodiment done according to the technical spirit of the present invention, still belongs to the protection domain of technical solution of the present invention.
Claims (1)
1. the preparation method of the high-temperature wave-transparent composite that a shuffling is fiber reinforced, it is characterised in that comprise the step of following order:
(1) boron nitride fibre is become prefabricated component form with silica fiber by method shuffling that is woven or braiding with high silica fiber, in prefabricated component after shuffling, boron nitride fibre is positioned at outermost layer, middle layer is high silica fiber, innermost layer is silica fiber, in outer, the thickness ratio of interior three layers of fiber is 1: 1: 1��3, pre-forms is 2.5 dimensions or 3 dimension forms, and fiber volume fraction controls between 30%��45%;
(2) phosphoric acid by certain mass mark mixes with aluminium hydroxide, and adds deionized water, is stirred well to Homogeneous phase mixing, leaves standstill and obtains aluminium phosphate sol after 2��4 hours, and wherein the mol ratio of phosphoric acid and aluminium hydroxide controls between 0.9��1.1;
(3) being placed in the aluminium phosphate sol of preparation by fiber preform, fully flood, impregnation pressure is 2��5MPa;
(4) fiber preform after being flooded by aluminium phosphate sol is placed in baking oven and is heat-treated stoving process, it is specially and rises to 90��110 DEG C from room temperature, temperature rise rate be 2��3 DEG C every minute, then it is incubated 40-60 minute at 90��110 DEG C, then temperature is made to rise to 160��170 DEG C, temperature rise rate be 2��3 DEG C every minute, then 160��170 DEG C be incubated 3��5 hours;
(5) sintering processes 1��2 hour at the matrix material after drying and processing being placed on 700��900 DEG C;
(6) (3)��(5) operation 5��7 times are repeated.
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| CN103664213B true CN103664213B (en) | 2016-06-08 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| CN110981407B (en) * | 2019-11-21 | 2022-01-28 | 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 |
| 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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| CN101698592A (en) * | 2009-11-13 | 2010-04-28 | 航天特种材料及工艺技术研究所 | Silicon-aluminium aerogel composite material and manufacturing method thereof |
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Patent Citations (3)
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| CN101698592A (en) * | 2009-11-13 | 2010-04-28 | 航天特种材料及工艺技术研究所 | Silicon-aluminium aerogel composite material and manufacturing method thereof |
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