CN112851383A - Infrared radiation resistant light ablation resistant composite material added with opacifier and preparation method thereof - Google Patents
Infrared radiation resistant light ablation resistant composite material added with opacifier and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 79
- 238000002679 ablation Methods 0.000 title claims abstract description 61
- 239000003605 opacifier Substances 0.000 title claims abstract description 41
- 230000005855 radiation Effects 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000835 fiber Substances 0.000 claims abstract description 69
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 31
- 239000005011 phenolic resin Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 31
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 30
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 28
- 239000004917 carbon fiber Substances 0.000 claims description 28
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 28
- 239000002243 precursor Substances 0.000 claims description 27
- 238000002791 soaking Methods 0.000 claims description 22
- 238000005470 impregnation Methods 0.000 claims description 21
- 238000001723 curing Methods 0.000 claims description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 9
- 239000012362 glacial acetic acid Substances 0.000 claims description 9
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 8
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 8
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- 150000001282 organosilanes Chemical class 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 2
- 229920000297 Rayon Polymers 0.000 claims description 2
- 239000010426 asphalt Substances 0.000 claims description 2
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229920002866 paraformaldehyde Polymers 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- 239000010439 graphite Substances 0.000 abstract description 6
- 229910002804 graphite Inorganic materials 0.000 abstract description 6
- 238000009413 insulation Methods 0.000 abstract description 4
- 230000014759 maintenance of location Effects 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 23
- 239000000463 material Substances 0.000 description 11
- 239000004744 fabric Substances 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 238000010998 test method Methods 0.000 description 5
- 239000004408 titanium dioxide Substances 0.000 description 4
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 239000011151 fibre-reinforced plastic Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
An infrared radiation resistant light ablation resistant composite material added with an opacifier and a preparation method thereof. The invention belongs to the field of preparation of ablation-resistant composite materials. The invention aims to solve the technical problems of large ablation amount, uneven ablation and high density of the existing ablation-resistant composite material. The invention relates to an anti-infrared ray composition added with an opacifierThe radiation light ablation-resistant composite material consists of a fiber woven body and TiO filled in the fiber woven body2Ceramics, SiOC and phenolic resins. The method comprises the following steps: step one, TiO-containing2Preparing a braided body; step two, preparing a SiOC-containing woven body; step three, preparing a light ablation-resistant braided body; and step four, replacing the solvent and drying. The density of the composite material prepared by the invention is 0.30-0.90g/cm3The graphite plate has the advantages that the room-temperature thermal conductivity is 0.093-0.230W/m.K, the longitudinal tensile strength is 3.59-5.38MPa, the longitudinal compressive strength is 1.48-11.02MPa, and the graphite plate shows non (micro) ablation and good heat insulation and shape retention capacity in a graphite plate radiation heating examination test.
Description
Technical Field
The invention belongs to the field of preparation of ablation-resistant composite materials, and particularly relates to an infrared radiation resistant light ablation-resistant composite material added with an opacifier and a preparation method thereof.
Background
With the development of the state to the aerospace industry, higher requirements are put forward on the thermal protection materials of the aircrafts. The ablation material is taken as a main material category, the carbon fiber has excellent specific strength, specific rigidity and specific modulus, and has important application prospect in the field of aerospace, and experts at home and abroad carry out deep research in recent years. The addition of the opacifier functional phase can enable the composite material to have high-temperature heat radiation resistance, also has the functions of resisting oxidation and blocking heat flow from spreading inwards, and has better heat-proof effect.
At present, the composite material is prepared by adopting a sol-gel method of filler and matrix phase by adopting a dipping-curing process, carbon fiber is used as a reinforcement, and the processes of multi-step dipping, curing, cracking, drying and the like are carried out on fiber fabric for multiple times so as to realize the composite of the material and the improvement of the performance, and finally the requirements of the designed strength, performance and function are met. However, the materials used at present have the disadvantages of large ablation amount, uneven ablation, high density and the like, so that a novel light ablation-resistant heat-insulating composite material is urgently needed to be developed to meet the requirements of an aircraft.
Disclosure of Invention
The invention aims to solve the technical problems of large ablation amount, nonuniform ablation and high density of the existing ablation-resistant composite material, and provides an infrared radiation-resistant light ablation-resistant composite material added with an opacifier and a preparation method thereof.
The invention relates to an infrared radiation resistant light ablation resistant composite material added with an opacifier, which comprises a fiber woven body and TiO filled in the fiber woven body2The composite material consists of ceramic, SiOC and phenolic resin, wherein the mass fraction of a fiber braided body in the composite material is 20-80%, and TiO is2The mass fraction of the ceramic is 2-10%, the mass fraction of the SiOC is 2-10%, the mass fraction of the phenolic resin is 8-68%, and the density of the composite material is 0.30g/cm3～0.90g/cm3。
The preparation method of the infrared radiation resistant light ablation resistant composite material added with the opacifier is carried out according to the following steps:
step one, TiO-containing2Preparation of the braid: mixing absolute ethyl alcohol, deionized water, butyl titanate and glacial acetic acid solution, adding an acidic solvent to adjust the pH value to 4-6, stirring until the pH value is uniformly mixed to obtain an opacifier precursor solution, soaking a fiber woven body in the opacifier precursor solution for 20-40 min by adopting an atmospheric pressure soaking method or a vacuum soaking method, taking out the fiber woven body, then aging the fiber woven body at 30-40 ℃, heating to 450-550 ℃ under the protection of inert gas, and calcining at the temperature for 1.5-2.5 h to obtain the TiO-containing fiber woven body2A braid;
step two, preparing the SiOC-containing braid: uniformly mixing organosilane mixture, ammonia water and solvent to obtain SiOC precursor solution, and then adopting normal pressure impregnation method or vacuum impregnation method to make TiO-containing precursor solution2Soaking the woven body in SiOC precursor solution, taking out the fiber woven body, curing at 70-90 ℃, soaking for 3 times by using absolute ethyl alcohol, and drying at 80-100 ℃ to obtain the SiOC-containing woven body;
step three, preparing a light ablation-resistant braided body: uniformly mixing phenolic resin, a curing agent and a solvent to obtain a phenolic resin solution, then soaking the SiOC-containing woven body in the phenolic resin solution by adopting a normal pressure impregnation method or a vacuum impregnation method, taking out the fiber woven body, then carrying out sol-gel at 80-100 ℃, and then immediately aging at 150-180 ℃ for 5-30 h;
step four, solvent replacement and drying: and immersing the woven body obtained in the third step in absolute ethyl alcohol, replacing the absolute ethyl alcohol once every 24 hours for 3-5 times, and performing vacuum drying at 170-190 ℃ to obtain the infrared radiation resistant light ablation resistant composite material added with the opacifier.
Further limiting, in the first step, the mass ratio of the absolute ethyl alcohol, the deionized water, the butyl titanate and the glacial acetic acid solution is (18-22): (1-2): (2-4): 1.
further, in the first step, the acidic solvent is glacial acetic acid or concentrated hydrochloric acid.
Further limiting, in the step one, the fiber braided body is a carbon fiber braided body; the carbon fiber is polyacrylonitrile-based carbon fiber, viscose-based carbon fiber or asphalt-based carbon fiber.
Further, the structure of the fiber woven body in the first step is a continuous carbon fiber needle punched structure, a net tire structure, a 2.5D woven structure or a three-dimensional woven structure.
Further limiting, the fiber braided body in the step one is in a random layering mode, and the density is 0.15g/cm3～0.50g/cm3The thickness is 10 mm-30 mm, the monofilament diameter is 6 μm-7 μm, and the needling density is 15 needles/cm2About 20 needles/cm2。
Further, the pressure of the atmospheric impregnation in the first step is 101.3kPa, and the pressure of the vacuum impregnation is 0kPa to 10 kPa.
Further, in the first step, the inert gas is nitrogen or argon.
Further limiting, the temperature rising rate in the step one is 4-6 ℃/min.
Further limiting, in the second step, the organosilane mixture is a mixture of methyltrimethoxysilane and dimethyldiethoxysilane, wherein the mass ratio of the methyldimethoxysilane to the dimethyldiethoxysilane is (3-5): 1.
further limiting, in the second step, the mass ratio of the organosilane mixture, the ammonia water and the solvent is 1: (0.6-2.6): (4-12).
Further limiting, in the second step, the solvent is one or a mixture of several of absolute ethyl alcohol, deionized water, propanol and methanol according to any ratio.
Further, in the second step, the pressure of the atmospheric impregnation is 101.3kPa, and the pressure of the vacuum impregnation is 0kPa to 10 kPa.
Further limiting, in the third step, the curing agent is one or a mixture of several of paraformaldehyde, hexamethylenetetramine, aniline, formaldehyde and melamine according to any ratio.
Further limiting, in the third step, the solvent is one or a mixture of several of absolute ethyl alcohol, deionized water, propanol, methanol and ethylene glycol according to any ratio.
Further limiting, in the third step, the mass ratio of the phenolic resin, the curing agent and the solvent is 20: (1-5): (80-120).
Further, the pressure of the atmospheric impregnation in the third step is 101.3kPa, and the pressure of the vacuum impregnation is 0kPa to 10 kPa.
Compared with the prior art, the invention has the advantages that:
1) in-situ synthesis of TiO on the basis of traditional carbon phenolic aldehyde2The ceramic functional phase and the SiOC precursor with a specific morphology improve the heat radiation resistance, ablation resistance and oxidation resistance of the composite material, so that the composite material has more excellent comprehensive performance. Compared with other preparation methods of the ablation composite material, the preparation method has the advantages of simplicity, high efficiency and stability, and the material can realize the coupling effect of multiple heat-proof mechanisms through regulation and control design, thereby providing a new idea for the preparation of a new generation of ablation material.
2) The invention relates to a preparation method of an infrared radiation resistant light ablation resistant composite material added with an opacifier, which utilizes carbon fiber as a composite materialThe material provides a supporting framework and certain mechanical property, the carbon fiber can play a role in maintaining the shape and reducing the ablation retreat amount in a severe and complex pneumatic scouring environment, and TiO added in the matrix2The ceramic opacifier and the SiOC ceramic precursor together provide the composite material with excellent ablation resistance and dimensional performance. The material has the characteristics of low density, good oxidation resistance, excellent temperature resistance and strong structural stability, and can be applied to the environment of heat insulation and ablation resistance.
3) Compared with the prior art, the density of the composite material prepared by the invention is 0.30-0.90g/cm3The room temperature thermal conductivity is 0.093-0.230W/m.K, the longitudinal tensile strength is 3.59-5.38MPa, the longitudinal compressive strength is 1.48-11.02MPa, and the peak heat flow is 1.5MW/m in a graphite plate radiation heating examination test2The duration is 80s, the total examination time is 240s, the surface peak temperature is more than 1900 ℃, the back surface temperature rise is less than 100 ℃, and non (micro) ablation and good heat insulation and shape retention capability are shown.
Drawings
FIG. 1 shows the TiO-containing material obtained in the first step of example 12A microstructure of the braid;
FIG. 2 is a microstructure diagram of the composite material obtained in example 1;
FIG. 3 is a graph showing the tensile strength of the composite obtained in example 1;
FIG. 4 is a graph showing the compressive strength of the composite obtained in example 1;
FIG. 5 is a graph showing the comparison of the morphology of the composite material obtained in example 1 before and after ablation by a graphite lamp, and a surface temperature and back temperature; wherein a is the morphology before ablation, b is the morphology after ablation, c is the surface temperature curve, and d is the back temperature curve.
Detailed Description
Example 1: the infrared radiation resistant light ablation resistant composite material added with the opacifier comprises a fiber woven body and TiO filled in the fiber woven body2The composite material consists of ceramic, SiOC and phenolic resin, wherein the mass fraction of a fiber braided body in the composite material is 30 percent, and TiO is2The mass fraction of the ceramic is 6 percent, the mass fraction of the SiOC is 6 percent, and the mass fraction of the phenolic resin is 5 percent8 percent, and the density of the composite material is 0.5g/cm3(ii) a The fiber woven body is a carbon fiber woven body, the carbon fiber is polyacrylonitrile-based carbon fiber, the structure of the fiber woven body is a continuous carbon fiber needle-punched structure, the fiber woven body is in a random layering mode, and the density of the fiber woven body is 0.15g/cm3The monofilament diameter is 6-7 μm, and the needling density is 17 needles/cm2The thickness is 20mm, the length is 200mm, and the width is 200 mm.
The method for preparing the infrared radiation resistant light ablation resistant composite material added with the opacifier, which is described in the example 1, comprises the following steps:
step one, TiO-containing2Preparation of the braid: mixing absolute ethyl alcohol, deionized water, butyl titanate and glacial acetic acid solution according to a mass ratio of 20:2:3:1, then adding concentrated hydrochloric acid to adjust the pH value to 5, stirring for 25min until the mixture is uniformly mixed to obtain an opacifier precursor solution, then soaking a fiber woven body in the opacifier precursor solution for 30min under the conditions of 35 ℃ and a vacuum degree of 5kPa, taking out the fiber woven body, then aging the fiber woven body at 35 ℃, then heating to 500 ℃ at a heating rate of 5 ℃/min under the protection of argon, and calcining for 2h at the temperature to obtain the titanium dioxide-containing titanium dioxide (TiO)2A braid;
step two, preparing the SiOC-containing braid: according to the mass ratio of methyltrimethoxysilane to dimethyldiethoxysilane to ammonia water to absolute ethyl alcohol to deionized water of 4: 1: 6: 18: 3, adding methyltrimethoxysilane and dimethyldiethoxysilane into absolute ethyl alcohol, dropwise adding deionized water and ammonia water, mixing for 30min to be uniform to obtain SiOC precursor solution, and then adding TiO-containing precursor solution2Dipping the fabric body in SiOC precursor solution for vacuum impregnation for 30min, taking out the fiber fabric body, curing for 24h at 80 ℃, then soaking for 3 times by using absolute ethyl alcohol, and drying for 8h at 80 ℃ to obtain the SiOC-containing fabric body;
step three, preparing a light ablation-resistant braided body: according to the mass ratio of the phenolic resin to the hexamethylenetetramine to the ethylene glycol of 20: 1.5: 90, dissolving hexamethylenetetramine in partial ethylene glycol, stirring for 30min to prepare a curing agent solution with the mass concentration of 10%, mixing the curing agent solution with phenolic resin and the rest ethylene glycol for 30min to be uniform to obtain a phenolic resin solution, then soaking the SiOC-containing woven body in the phenolic resin solution for 60min in vacuum, taking out the fiber woven body, treating the fiber woven body at 90 ℃ for 24h to perform sol-gel, and immediately aging the fiber woven body at 170 ℃ for 6 h;
step four, solvent replacement and drying: and (3) immersing the braided body obtained in the step three in absolute ethyl alcohol, replacing the absolute ethyl alcohol once every 24 hours for 4 times, and drying for 36 hours at 180 ℃ under the vacuum condition of 5kPa to obtain the infrared radiation resistant light ablation resistant composite material added with the opacifier.
The density of the composite material prepared in this example was about 0.5g/cm after preparation3Can be applied to an environment with radiation heat flow at 1900 ℃.
The thermal conductivity at room temperature of the composite material prepared in example 1 was measured according to the test method for thermal conductivity of GBT 3139-2005 fiber reinforced plastic, and found to be 0.173W/m.K.
The tensile strength and the compressive strength of the composite material prepared in example 1 were measured according to the test method for tensile properties of GBT 1447-.
FIG. 1 shows the TiO-containing material obtained in the first step of example 12A microstructure of the braid; FIG. 2 is a microstructure diagram of the composite material obtained in example 1; FIG. 3 is a graph showing the tensile strength of the composite obtained in example 1; FIG. 4 is a graph showing the compressive strength of the composite obtained in example 1; FIG. 5 is a graph showing the comparison of the morphology of the composite material obtained in example 1 before and after ablation by a graphite lamp, and a surface temperature and back temperature; as can be seen from FIGS. 3 and 4, the composite of example 1 had a tensile strength in the machine direction of 4.03MPa and a compressive strength in the machine direction of 2.78MPa, and it can be seen from FIG. 5 that the heat flow at the peak was 1.5MW/m2Under the radiation environment with the duration of 80s and the total examination time of 240s, the surface peak temperature is more than 1900 ℃, the back surface temperature rise is less than 100 ℃, and the non (micro) ablation and good heat insulation and shape retention capability are shown.
Example 2: this implementationThe example of the infrared radiation resistant light ablation resistant composite material added with the opacifier consists of a fiber woven body and TiO filled in the fiber woven body2The composite material consists of ceramic, SiOC and phenolic resin, wherein the mass fraction of a fiber braided body in the composite material is 40 percent, and TiO is2The mass fraction of the ceramic is 9 percent, the mass fraction of the SiOC is 9 percent, the mass fraction of the phenolic resin is 42 percent, and the density of the composite material is 0.5g/cm3(ii) a The fiber woven body is a carbon fiber woven body, the carbon fiber is polyacrylonitrile-based carbon fiber, the structure of the fiber woven body is a continuous carbon fiber needle-punched structure, the fiber woven body is in a random layering mode, and the density of the fiber woven body is 0.20g/cm3The monofilament diameter is 6-7 μm, and the needling density is 19 needles/cm2The thickness is 23mm, the length is 200mm, and the width is 200 mm.
The method for preparing the infrared radiation resistant light ablation resistant composite material added with the opacifier, which is described in the embodiment 2, comprises the following steps:
step one, TiO-containing2Preparation of the braid: mixing absolute ethyl alcohol, deionized water, butyl titanate and glacial acetic acid solution according to a mass ratio of 20:2:3:1, then adding concentrated hydrochloric acid to adjust the pH value to 5, stirring for 25min until the mixture is uniformly mixed to obtain an opacifier precursor solution, then soaking a fiber woven body in the opacifier precursor solution for 20min under the conditions of 40 ℃ and a vacuum degree of 3kPa, taking out the fiber woven body, then aging the fiber woven body at 35 ℃, then heating to 450 ℃ at a heating rate of 6 ℃/min under the protection of argon, and calcining for 2.5h at the temperature to obtain the TiO-containing precursor solution2A braid;
step two, preparing the SiOC-containing braid: according to the mass ratio of methyltrimethoxysilane to dimethyldiethoxysilane to ammonia water to absolute ethyl alcohol to deionized water of 4: 1: 6: 36: 3, adding methyltrimethoxysilane and dimethyldiethoxysilane into absolute ethyl alcohol, dropwise adding deionized water and ammonia water, mixing for 30min to be uniform to obtain SiOC precursor solution, and then adding TiO-containing precursor solution2Soaking the fabric in SiOC precursor solution for 30min, taking out the fiber fabric, curing at 80 deg.C for 36 hr, and soaking in anhydrous ethanolSoaking for 4 times, and drying for 6h at 90 deg.C to obtain SiOC-containing woven body;
step three, preparing a light ablation-resistant braided body: according to the mass ratio of the phenolic resin to the hexamethylenetetramine to the ethylene glycol of 20: 3: 100, dissolving hexamethylenetetramine in partial ethylene glycol, stirring for 30min to prepare a curing agent solution with the mass concentration of 10%, mixing the curing agent solution with phenolic resin and the rest ethylene glycol for 30min to be uniform to obtain a phenolic resin solution, then soaking the SiOC-containing woven body in the phenolic resin solution for 120min in vacuum, taking out the fiber woven body, treating the fiber woven body at 100 ℃ for 24h for sol-gel, and immediately aging the fiber woven body at 180 ℃ for 15 h;
step four, solvent replacement and drying: and (3) immersing the braided body obtained in the third step in absolute ethyl alcohol, replacing the absolute ethyl alcohol once every 24 hours for 4 times, and drying for 72 hours at the temperature of 170 ℃ and under the vacuum condition of 3kPa to obtain the infrared radiation resistant light ablation resistant composite material added with the opacifier.
The density of the composite material prepared in this example was about 0.5g/cm after preparation3And can be applied to an environment with radiation heat flow at 1800 ℃.
The thermal conductivity at room temperature of the composite material prepared in example 2 was measured according to the standard of GBT 3139-2005 fiber reinforced plastic thermal conductivity test method, and found to be 0.180W/m.K.
The tensile strength and the compressive strength of the composite material prepared in example 2 are detected according to the standard of GBT 1447 & 2005 & gt, and the longitudinal tensile strength and the longitudinal compressive strength are 4.26MPa and 5.31MPa respectively.
Example 3: the infrared radiation resistant light ablation resistant composite material added with the opacifier comprises a fiber woven body and TiO filled in the fiber woven body2The composite material consists of ceramic, SiOC and phenolic resin, wherein the mass fraction of a fiber braided body in the composite material is 50 percent, and TiO is2The mass fraction of the ceramic is 4 percent, the mass fraction of the SiOC is 5 percent, the mass fraction of the phenolic resin is 41 percent, and the density of the composite material is 0.3g/cm3(ii) a The fiber woven body is a carbon fiber woven body, the carbon fiber is polyacrylonitrile-based carbon fiber, the structure of the fiber woven body is a continuous carbon fiber needle-punched structure, the fiber woven body is in a random layering mode, and the density of the fiber woven body is 0.15g/cm3The monofilament diameter is 6-7 μm, and the needling density is 18 needles/cm2The thickness is 20mm, the length is 200mm, and the width is 200 mm.
The method for preparing the infrared radiation resistant light ablation resistant composite material added with the opacifier in the embodiment 3 comprises the following steps:
step one, TiO-containing2Preparation of the braid: mixing absolute ethyl alcohol, deionized water, butyl titanate and glacial acetic acid solution according to a mass ratio of 20:2:3:1, then adding concentrated hydrochloric acid to adjust the pH value to 5, stirring for 25min until the mixture is uniformly mixed to obtain an opacifier precursor solution, then soaking a fiber woven body in the opacifier precursor solution for 30min under the conditions of 40 ℃ and a vacuum degree of 7kPa, taking out the fiber woven body, then aging the fiber woven body at 35 ℃, then heating to 550 ℃ at a heating rate of 4 ℃/min under the protection of argon, and calcining for 1.5h at the temperature to obtain the titanium dioxide-containing titanium dioxide composite material2A braid;
step two, preparing the SiOC-containing braid: according to the mass ratio of methyltrimethoxysilane to dimethyldiethoxysilane to ammonia water to absolute ethyl alcohol to deionized water of 4: 1: 10: 44: 6, adding methyltrimethoxysilane and dimethyldiethoxysilane into absolute ethyl alcohol, dropwise adding deionized water and ammonia water, mixing for 30min to be uniform to obtain SiOC precursor solution, and then adding TiO-containing precursor solution2Dipping the fabric body in SiOC precursor solution for 40min in vacuum, taking out the fiber fabric body, curing at 90 ℃ for 48h, then soaking with absolute ethyl alcohol for 4 times, and drying at 100 ℃ for 8h to obtain the SiOC-containing fabric body;
step three, preparing a light ablation-resistant braided body: according to the mass ratio of the phenolic resin to the hexamethylenetetramine to the ethylene glycol of 20: 4: 110, dissolving hexamethylenetetramine in partial ethylene glycol, stirring for 50min to prepare a curing agent solution with the mass concentration of 15%, mixing the curing agent solution with phenolic resin and the rest ethylene glycol for 50min to be uniform to obtain a phenolic resin solution, then soaking the SiOC-containing woven body in the phenolic resin solution for 100min in vacuum, taking out the fiber woven body, treating the fiber woven body at 90 ℃ for 36h to perform sol-gel, and immediately aging the fiber woven body at 150 ℃ for 13 h;
step four, solvent replacement and drying: and (3) immersing the braided body obtained in the third step in absolute ethyl alcohol, replacing the absolute ethyl alcohol once every 24 hours for 3 times, and drying for 72 hours at 180 ℃ under the vacuum condition of 7kPa to obtain the infrared radiation resistant light ablation resistant composite material added with the opacifier.
The density of the composite material prepared in this example was about 0.3g/cm after preparation3And can be applied to an environment with radiation heat flow at 1800 ℃.
The thermal conductivity at room temperature of the composite material prepared in example 3 was measured according to the standard of GBT 3139-2005 fiber reinforced plastic thermal conductivity test method, and found to be 0.131W/m.K.
The tensile strength and the compressive strength of the composite material prepared in example 3 are detected according to the standard of GBT 1447 & 2005 FRP tensile property test method, and the longitudinal tensile strength and the longitudinal compressive strength are 3.97MPa and 4.38MPa respectively.
Claims (10)
1. The infrared radiation resistant light ablation resistant composite material added with the opacifier is characterized by comprising a fiber woven body and TiO filled in the fiber woven body2The composite material consists of ceramic, SiOC and phenolic resin, wherein the mass fraction of a fiber braided body in the composite material is 20-80%, and TiO is2The mass fraction of the ceramic is 2-10%, the mass fraction of the SiOC is 2-10%, the mass fraction of the phenolic resin is 8-68%, and the density of the composite material is 0.30g/cm3～0.90g/cm3。
2. The method for preparing the infrared radiation resistant lightweight ablation resistant composite material with the added opacifier according to claim 1, wherein the preparation method comprises the following steps:
step one, TiO-containing2Preparation of the braid: mixing absolute ethyl alcohol, deionized water, butyl titanate and glacial acetic acid solution, adding an acidic solvent to adjust the pH value to 4-6, stirring until the pH value is uniformly mixed to obtain an opacifier precursor solution, soaking a fiber woven body in the opacifier precursor solution for 20-40 min by adopting an atmospheric pressure soaking method or a vacuum soaking method, taking out the fiber woven body, then aging the fiber woven body at 30-40 ℃, heating to 450-550 ℃ under the protection of inert gas, and calcining at the temperature for 1.5-2.5 h to obtain the TiO-containing fiber woven body2A braid;
step two, preparing the SiOC-containing braid: uniformly mixing organosilane mixture, ammonia water and solvent to obtain SiOC precursor solution, and then adopting normal pressure impregnation method or vacuum impregnation method to make TiO-containing precursor solution2Soaking the woven body in SiOC precursor solution, taking out the fiber woven body, curing at 70-90 ℃, soaking for 3 times by using absolute ethyl alcohol, and drying at 80-100 ℃ to obtain the SiOC-containing woven body;
step three, preparing a light ablation-resistant braided body: uniformly mixing phenolic resin, a curing agent and a solvent to obtain a phenolic resin solution, then soaking the SiOC-containing woven body in the phenolic resin solution by adopting a normal pressure impregnation method or a vacuum impregnation method, taking out the fiber woven body, then carrying out sol-gel at 80-100 ℃, and then immediately aging at 150-180 ℃ for 5-30 h;
step four, solvent replacement and drying: and immersing the woven body obtained in the third step in absolute ethyl alcohol, replacing the absolute ethyl alcohol once every 24 hours for 3-5 times, and performing vacuum drying at 170-190 ℃ to obtain the infrared radiation resistant light ablation resistant composite material added with the opacifier.
3. The preparation method of the infrared radiation resistant light ablation-resistant composite material added with the opacifier as claimed in claim 2, wherein the mass ratio of the absolute ethyl alcohol, the deionized water, the butyl titanate and the glacial acetic acid solution in the step one is (18-22): (1-2): (2-4): 1.
4. the method for preparing the infrared radiation resistant lightweight ablation-resistant composite material added with the opacifier according to the claim 2, wherein the acidic solvent in the step one is glacial acetic acid or concentrated hydrochloric acid.
5. The method for preparing the infrared radiation resistant light ablation resistant composite material added with the opacifier as claimed in claim 2, wherein the fiber braid in the first step is a carbon fiber braid; the carbon fiber is polyacrylonitrile-based carbon fiber, viscose-based carbon fiber or asphalt-based carbon fiber; the structure of the fiber knitted body in the first step is a continuous carbon fiber needling structure, a net tire structure, a 2.5D knitted structure or a three-dimensional knitted structure; the fiber woven body in the step one is in a random layering mode, and the density is 0.15g/cm3～0.50g/cm3The thickness is 10 mm-30 mm, the monofilament diameter is 6 μm-7 μm, and the needling density is 15 needles/cm2About 20 needles/cm2。
6. The method for preparing the infrared radiation resistant light ablation resistant composite material added with the opacifier as claimed in claim 2, wherein the pressure of the atmospheric impregnation in the first step is 101.3kPa, the pressure of the vacuum impregnation is 0kPa to 10kPa, the inert gas in the first step is nitrogen or argon, and the temperature rise rate in the first step is 4 ℃/min to 6 ℃/min.
7. The method for preparing the infrared radiation resistant light-weight ablation-resistant composite material added with the opacifier as claimed in claim 2, wherein the organosilane mixture in the second step is a mixture of methyltrimethoxysilane and dimethyldiethoxysilane, wherein the mass ratio of the methyldimethoxysilane to the dimethyldiethoxysilane is (3-5): 1; in the second step, the mass ratio of the organosilane mixture to the ammonia water to the solvent is 1: (0.6-2.6): (4-12); in the second step, the solvent is one or a mixture of more of absolute ethyl alcohol, deionized water, propyl alcohol and methanol.
8. The method for preparing the infrared radiation resistant light ablation resistant composite material added with the opacifier according to the claim 2, wherein the pressure of the atmospheric impregnation in the step two is 101.3kPa, and the pressure of the vacuum impregnation is 0kPa to 10 kPa.
9. The method for preparing the infrared radiation resistant light ablation resistant composite material added with the opacifier according to the claim 2, characterized in that the curing agent in the step three is one or a mixture of several of paraformaldehyde, hexamethylenetetramine, aniline, formaldehyde and melamine; in the third step, the solvent is one or a mixture of more of absolute ethyl alcohol, deionized water, propanol, methanol and glycol; in the third step, the mass ratio of the phenolic resin to the curing agent to the solvent is 20: (1-5): (80-120).
10. The method for preparing the infrared radiation resistant light ablation resistant composite material added with the opacifier according to the claim 2, characterized in that the pressure of the atmospheric impregnation in the step three is 101.3kPa, and the pressure of the vacuum impregnation is 0kPa to 10 kPa.
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