CN117925089A - Flexible electromagnetic shielding ablation-resistant heat insulation coating double-component and coating and preparation method thereof - Google Patents
Flexible electromagnetic shielding ablation-resistant heat insulation coating double-component and coating and preparation method thereof Download PDFInfo
- Publication number
- CN117925089A CN117925089A CN202311720735.7A CN202311720735A CN117925089A CN 117925089 A CN117925089 A CN 117925089A CN 202311720735 A CN202311720735 A CN 202311720735A CN 117925089 A CN117925089 A CN 117925089A
- Authority
- CN
- China
- Prior art keywords
- coating
- component
- electromagnetic shielding
- ablation
- oxide powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000576 coating method Methods 0.000 title claims abstract description 290
- 239000011248 coating agent Substances 0.000 title claims abstract description 286
- 238000002679 ablation Methods 0.000 title claims abstract description 150
- 238000002360 preparation method Methods 0.000 title claims abstract description 50
- 238000009413 insulation Methods 0.000 title claims description 97
- 239000000463 material Substances 0.000 claims abstract description 126
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 183
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 149
- 239000000843 powder Substances 0.000 claims description 135
- 239000004005 microsphere Substances 0.000 claims description 85
- 229910021392 nanocarbon Inorganic materials 0.000 claims description 82
- 239000002041 carbon nanotube Substances 0.000 claims description 77
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 77
- 239000000945 filler Substances 0.000 claims description 69
- 239000000377 silicon dioxide Substances 0.000 claims description 62
- 238000003756 stirring Methods 0.000 claims description 53
- 239000003795 chemical substances by application Substances 0.000 claims description 45
- 235000012239 silicon dioxide Nutrition 0.000 claims description 45
- 238000011068 loading method Methods 0.000 claims description 32
- 239000002356 single layer Substances 0.000 claims description 32
- 239000002904 solvent Substances 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 24
- 239000003575 carbonaceous material Substances 0.000 claims description 21
- 229910021389 graphene Inorganic materials 0.000 claims description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 17
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 17
- 229910052810 boron oxide Inorganic materials 0.000 claims description 17
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 17
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 17
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000003921 oil Substances 0.000 claims description 17
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 17
- 229910001392 phosphorus oxide Inorganic materials 0.000 claims description 17
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 17
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 17
- 229920002379 silicone rubber Polymers 0.000 claims description 17
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 17
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 17
- VSAISIQCTGDGPU-UHFFFAOYSA-N tetraphosphorus hexaoxide Chemical compound O1P(O2)OP3OP1OP2O3 VSAISIQCTGDGPU-UHFFFAOYSA-N 0.000 claims description 17
- 239000000919 ceramic Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 239000011159 matrix material Substances 0.000 claims description 13
- 238000005507 spraying Methods 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000004964 aerogel Substances 0.000 claims description 8
- 239000010445 mica Substances 0.000 claims description 8
- 229910052618 mica group Inorganic materials 0.000 claims description 8
- 230000001680 brushing effect Effects 0.000 claims description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 6
- 239000012763 reinforcing filler Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 4
- 239000003085 diluting agent Substances 0.000 claims description 4
- 239000003208 petroleum Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 239000005543 nano-size silicon particle Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 150000003839 salts Chemical group 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000002344 surface layer Substances 0.000 claims description 2
- 239000012720 thermal barrier coating Substances 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 2
- 239000002585 base Substances 0.000 description 83
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 52
- 239000008367 deionised water Substances 0.000 description 39
- 229910021641 deionized water Inorganic materials 0.000 description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 26
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 26
- 239000000203 mixture Substances 0.000 description 26
- 238000005303 weighing Methods 0.000 description 26
- 229910052799 carbon Inorganic materials 0.000 description 18
- 239000000758 substrate Substances 0.000 description 16
- 238000012360 testing method Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 13
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 13
- 230000032683 aging Effects 0.000 description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 description 13
- 239000003638 chemical reducing agent Substances 0.000 description 13
- 238000005229 chemical vapour deposition Methods 0.000 description 13
- 229960003964 deoxycholic acid Drugs 0.000 description 13
- 238000009826 distribution Methods 0.000 description 13
- NASVITFAUKYCPM-UHFFFAOYSA-N ethanol;tetraethyl silicate Chemical compound CCO.CCO[Si](OCC)(OCC)OCC NASVITFAUKYCPM-UHFFFAOYSA-N 0.000 description 13
- 229910052739 hydrogen Inorganic materials 0.000 description 13
- 239000001257 hydrogen Substances 0.000 description 13
- 238000010298 pulverizing process Methods 0.000 description 13
- 239000002109 single walled nanotube Substances 0.000 description 13
- FHHPUSMSKHSNKW-SMOYURAASA-M sodium deoxycholate Chemical compound [Na+].C([C@H]1CC2)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC([O-])=O)C)[C@@]2(C)[C@@H](O)C1 FHHPUSMSKHSNKW-SMOYURAASA-M 0.000 description 13
- 238000001291 vacuum drying Methods 0.000 description 13
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 12
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 12
- 239000012975 dibutyltin dilaurate Substances 0.000 description 12
- OMAWWKIPXLIPDE-UHFFFAOYSA-N (ethyldiselanyl)ethane Chemical compound CC[Se][Se]CC OMAWWKIPXLIPDE-UHFFFAOYSA-N 0.000 description 9
- 239000004965 Silica aerogel Substances 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 239000004945 silicone rubber Substances 0.000 description 4
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 description 3
- 229920001558 organosilicon polymer Polymers 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Landscapes
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a double-component and a coating of a flexible electromagnetic shielding ablation-resistant heat-insulating coating and a preparation method thereof, and relates to the field of functional coatings. The coating prepared by the coating has lower comprehensive density, heat conductivity and excellent electromagnetic shielding performance, and can be used as a temperature-resistant heat-insulating electromagnetic shielding material for an aircraft.
Description
Technical Field
The invention relates to the field of functional coatings, in particular to a flexible electromagnetic shielding ablation-resistant heat-insulating coating bi-component, a coating and a preparation method thereof.
Background
Electromagnetic shielding is an important means of resisting electromagnetic drying. The development of the electromagnetic shielding coating is regarded as one of important paths of electromagnetic shielding and stealth technology development, the electromagnetic shielding effect can be realized only by coating the electromagnetic shielding coating on the surface of a substrate to be protected, and the electromagnetic shielding coating has wide application prospect in the fields of national defense, military industry, aerospace, communication, medical treatment and the like. The metal material is the most commonly used electromagnetic shielding material, has the characteristics of good shielding effect, wide application field and the like, but the material is generally heavy in quality, easy to oxidize and high in cost, and the carbon material is widely focused in the electromagnetic shielding field due to excellent conductivity, acid and alkali resistance and the like.
The carbon nano tube is structurally regarded as a one-dimensional tubular structure formed by curling graphene sheets, and the unique structure and the excellent electric conduction performance of the carbon nano tube enable the carbon nano tube to show good electromagnetic shielding performance. However, due to the inherent hydrophobic and oleophobic characteristics, the carbon nanotubes have poor compatibility with the organic polymer, extremely light density, and have the problems of difficult dispersion and unstable properties of a dispersion system, and the carbon nanotubes are scattered each other due to the use process of the coating, so that the conductivity is greatly reduced, the electromagnetic shielding performance is reduced and even fails, and the application of the carbon nanotubes in the field of electromagnetic shielding coatings is not facilitated. Meanwhile, when the aircraft flies in the air at a high speed, the aircraft faces a severe pneumatic heating environment, and the aircraft needs to be subjected to necessary thermal protection, namely, the aircraft coating has certain heat resistance and heat insulation performance besides a specific function. Therefore, the preparation of the light flexible heat-resistant and heat-insulating electromagnetic shielding coating has important significance for aerospace development.
Disclosure of Invention
The invention aims to provide a light flexible electromagnetic shielding ablation-resistant heat-insulating coating bi-component and a coating preparation method thereof, so as to solve the problems of high density, insufficient conductivity, poor high-temperature ablation resistance, limited heat-insulating performance and the like of the current electromagnetic shielding coating. The light flexible electromagnetic shielding ablation-resistant heat insulation coating takes self-made continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler as a bridging conductive group, and the discrete ultra-soft nano carbon light filler in the coating is connected to form a conductive network in a coating surface, so that the broadband electromagnetic shielding performance of the coating is improved, and the heat insulation coating is matched with the design of longitudinally overlapping coating heat insulation layers, so that the longitudinal heat conductivity of the prepared coating is reduced, and the heat insulation coating can be used as an aircraft heat insulation electromagnetic shielding material.
In order to achieve the above object, the present invention adopts the following technical scheme:
The invention provides a preparation method of a light flexible electromagnetic shielding ablation-resistant heat insulation coating, which comprises the following steps:
(1) Preparing mesoporous silica microspheres as a load matrix material, loading a catalyst on the mesoporous silica microspheres, wherein the catalyst loading amount is 0.02% -2% of the mass of the mesoporous silica microspheres, and then growing continuously lapped carbon nanotubes in a surface layer mesoporous structure and on the outer surface of the material, wherein the obtained carbon nanotube loading amount is 0.05% -5% of the mass of the mesoporous silica microspheres, the pipe diameter is less than or equal to 50nm, and the length is more than or equal to 10 mu m, so as to obtain self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler;
(2) Preparing an ultra-light nano carbon material, and then crushing the ultra-light nano carbon material into ultra-light nano carbon powder filler through oscillation treatment;
(3) Mixing a matrix film forming material, a reinforcing filler, ablation-resistant oxide powder and hollow microspheres according to the mass ratio of (90-120): (5-15): (15-80): (2-25) to obtain a coating base material A0 component;
(4) Mixing the coating base material A0 obtained in the step (3), the continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler obtained in the step (1) and the ultra-light nano carbon powder filler obtained in the step (2) according to the mass ratio of 100 (2-15) (10-40) to obtain a coating base material B0 component;
(5) Adding a curing agent into the coating base material A0 obtained in the step (3) for stirring and mixing uniformly, adding the curing agent into the coating base material B0 obtained in the step (4) for stirring and mixing uniformly, and preparing the component A and the component B of the light flexible electromagnetic shielding ablation-resistant heat insulation coating.
Preferably, the mesoporous silica microspheres have a size of 5-50 μm; the mesoporous silica supported catalyst is a salt containing one or more elements of iron, cobalt and nickel.
Preferably, the ultra-light flexible nano carbon material is an ultra-light elastic aerogel material composed of one or more of carbon nano tubes and graphene, the tube diameter of the carbon nano tubes is less than or equal to 50nm, the length of the carbon nano tubes is less than or equal to 50 mu m, the size of graphene sheets is less than or equal to 300 mu m, and the density of the ultra-light elastic aerogel material is 0.05-0.50mg/cm 3; more preferably, the density of the ultra-light elastic aerogel material is 0.05-0.20mg/cm 3; the size of the ultra-light nano carbon powder material is 50-200 mu m, and the specific surface area is more than or equal to 800m 2/g.
Preferably, the matrix film forming material is one or more of ablation-resistant modified organic silicon rubber and organic silicon resin, the reinforcing filler is one or more of nano silicon dioxide aerogel, nano aluminum oxide, mica powder and talcum powder, the ablation-resistant oxide powder is one or more of sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder, zinc oxide powder, manganese oxide powder and zirconium oxide powder, and the hollow microsphere is one or more of hollow glass microsphere and hollow ceramic microsphere.
Preferably, the granularity of the reinforcing filler is more than or equal to 100 meshes, the granularity of the ablation-resistant oxide powder is more than or equal to 200 meshes, and the outer diameter of the hollow microsphere is less than or equal to 200 mu m.
Preferably, the curing agent is one of organic tin and amine, the addition amount of the curing agent is 5-25% of the mass of the matrix film forming matter in the coating base material A0, and the addition amount of the curing agent is 5-25% of the mass of the matrix film forming matter in the coating base material B0; more preferably, the addition amount of the curing agent is 8% -15% of the mass of the matrix film forming matter in the coating base material A0, and the addition amount of the curing agent is 10% -18% of the mass of the matrix film forming matter in the coating base material B0; and selecting a curing agent corresponding to the components in the coating base material A0 or B0, adding and uniformly mixing the curing agent, and using the coating within 10-30h according to different curing systems.
Preferably, the mesoporous silica microsphere preparation in the step (1), the carbon nanotube growth, the ultra-soft nano carbon material preparation in the step (2), the oscillation treatment, the mixing in the steps (3) and (4) and the stirring in the step (5) are all carried out by adopting the conventional operation means in the field.
The invention provides a light flexible electromagnetic shielding ablation-resistant heat insulation coating double-component in a second aspect, which comprises a component A and a component B, and is prepared by the method in the first aspect.
The invention provides a preparation method of a light flexible electromagnetic shielding ablation-resistant thermal insulation coating in a third aspect, which comprises the following steps: the light flexible electromagnetic shielding ablation-resistant heat-insulating coating prepared by the method in the first aspect of the invention is diluted to the required viscosity by a diluent, the A component and the B component are overlapped and coated by adopting a proper brushing method, the whole brushing process is completed, and the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained after drying.
Preferably, the diluent is one or more of cyclohexane, ethyl acetate, butyl acetate, toluene, xylene, petroleum ether, no. 6 solvent oil and No. 120 solvent oil.
Preferably, the brushing method is spraying.
Preferably, the single-layer spraying thickness of the component A is 0.1-0.3mm, and the single-layer spraying thickness of the component B is 0.2-0.4mm.
Preferably, the spraying times of the component A are more than or equal to 2 times, and the spraying times of the component B are more than or equal to 3 times.
Preferably, the drying mode is room temperature and normal pressure drying, and the drying time is 4-7 days.
In a fourth aspect, the invention provides a lightweight flexible electromagnetic shielding ablation-resistant thermal barrier coating prepared by the method of the third aspect.
Compared with the prior art, the invention has the following beneficial effects:
(1) The ultra-light nano carbon powder filler used in the invention is a sponge structure composed of carbon nano tubes and/or graphene aerogel, has the characteristics of ultra-light weight, strong conductivity and the like, and shows excellent electromagnetic shielding performance; the coating has the characteristics of light weight and super elasticity, can be compounded with ablation-resistant organosilicon polymer for use, and can be matched with organosilicon polymer film forming matters in a shrinkage way, so that the density of the coating is greatly reduced, and the formed coating has flexibility and elasticity.
(2) The self-made continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler has a porous structure inside, and can play roles in light weight and heat isolation; the surface continuous carbon nano tube is used as a bridging conductive structure, and can connect the discrete ultra-soft nano carbon powder filler in the coating to form a continuous and huge conductive network in the coating surface, thereby greatly improving the conductive performance in the coating surface and further improving the broadband electromagnetic shielding performance of the coating.
(3) According to the preparation method of the coating, which is used by the invention, the component A and the component B are overlapped to form the layer, the conductivity limit of the coating can be within the layer B, the overlapping coating design of the layer A and the layer B can realize insulation in the thickness direction of the coating, heat transfer is blocked, and the longitudinal heat conductivity coefficient of the coating is not improved while the electromagnetic shielding performance of the coating is improved; meanwhile, the components A and B are identical except the difference of electromagnetic shielding components, so that the compatibility and the thermal expansion coefficient of the components are consistent, the bonding strength of the coating and the stability and the reliability of the use can be ensured, and the conductive network formed in the coating B has excellent heat conduction performance, so that heat conduction can be realized in the coating B, the property change of the coating caused by local overheating is avoided, and the electromagnetic shielding performance is damaged.
(4) The ablation-resistant oxide powder used in the invention can ensure the ablation dimension of the coating in the whole temperature range under the use condition and ensure the ablation stability of the coating by reasonably compounding the oxide powder with different melting points and heat conductivity coefficients.
(5) The invention adopts the ablation-resistant organosilicon polymer as a matrix film forming matter, does not form carbon in the service environment, can ensure that the electromagnetic shielding performance of the coating is not influenced, and keeps the stability of the electromagnetic shielding effect in the use process of the coating.
(6) The density of the light flexible electromagnetic shielding ablation-resistant heat insulation coating prepared by the invention is less than or equal to 0.40g/cm 3, the room temperature heat conductivity is less than or equal to 0.10W/(m.K), the average electromagnetic shielding efficiency is greater than 50dB in the frequency range of 1.5-18GHz, the high-temperature examination at 800-1200 ℃ can be resisted, the outer surface of the coating is kept complete and is not cracked after the examination, the electromagnetic shielding performance does not generate obvious attenuation, the coating can be dried and cured at room temperature for forming, the coating process is simple, and the coating has wide application prospect in the field of aircraft heat protection and electromagnetic shielding.
Detailed Description
In order to make the technical features and advantages or technical effects of the above technical solution of the present invention more obvious and understandable, the following detailed description is given with reference to the embodiments.
Example 1:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,10 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 5-45 mu m are obtained through vacuum drying;
(2) Loading cobalt tungstate with the weight of 0.02% on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the mesoporous silica microspheres through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading amount is 0.05% of the mass of the mesoporous silica microspheres, so that the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler is prepared;
(3) Weighing 5g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 5g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (5% of deionized water solution of N-methylpyrrolidone), and carrying out ultrasonic crushing by virtue of stirring to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying are carried out on the nano carbon sol system to obtain an ultra-light flexible nano carbon material, the material is stirred and oscillated and smashed into ultra-light flexible nano carbon powder filler, the powder size is 50-150 mu m after pulverization, and the density is 0.05mg/cm 3;
(4) 90g of ablation-resistant silicon rubber, 2.5g of nano aluminum oxide (with granularity not less than 100 meshes), 2.5g of mica powder (with granularity not less than 100 meshes), 15g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2), 2g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(5) 100 Parts by mass of coating base material A0, 2 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 10 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 4.1g and 2.0g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
the prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by No. 120 solvent oil respectively, then the B component (the thickness of a single layer is 0.2 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.1 mm) and the B component are overlapped and coated, the A component is coated for 2 times, the B component is coated for 3 times, and the room temperature is dried for 6 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.35g/cm 3, the room temperature thermal conductivity is 0.051W/(m.K), the average electromagnetic shielding effectiveness is 62dB in the range of 1.5-18GHz frequency band, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Example 2:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,10 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 5-45 mu m are obtained through vacuum drying;
(2) Loading 2% of cobalt tungstate on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the mesoporous silica microspheres through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading is 5% of the mass of the mesoporous silica microspheres, so that the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler is prepared;
(3) Weighing 5g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 10g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (deionized water solution of 5% N-methylpyrrolidone), and carrying out stirring and ultrasonic crushing to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying the nano carbon sol system to obtain an ultra-light flexible nano carbon material, stirring and oscillating the material, crushing the material into ultra-light flexible nano carbon powder filler, and pulverizing to obtain powder with a size of 50-150 mu m and a density of 0.3mg/cm 3;
(4) 90g of ablation-resistant silicon rubber, 2.5g of nano aluminum oxide (with granularity not less than 100 meshes), 2.5g of mica powder (with granularity not less than 100 meshes), 15g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2), 2g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(5) 100 Parts by mass of coating base material A0, 2 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 10 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 4.1g and 2.0g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
the prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by No. 120 solvent oil respectively, then the B component (the thickness of a single layer is 0.2 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.1 mm) and the B component are overlapped and coated, the A component is coated for 2 times, the B component is coated for 3 times, and the room temperature is dried for 6 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.36g/cm 3, the room temperature thermal conductivity is 0.055W/(m.K), the average electromagnetic shielding effectiveness is 78dB in the frequency range of 1.5-18GHz, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Example 3:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,10 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 5-45 mu m are obtained through vacuum drying;
(2) Loading 2% of cobalt tungstate on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the mesoporous silica microspheres through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading is 5% of the mass of the mesoporous silica microspheres, so that the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler is prepared;
(3) Weighing 5g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 10g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (deionized water solution of 5% N-methylpyrrolidone), and carrying out stirring and ultrasonic crushing to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying the nano carbon sol system to obtain an ultra-light flexible nano carbon material, stirring and oscillating the material, crushing the material into ultra-light flexible nano carbon powder filler, and pulverizing to obtain powder with a size of 50-150 mu m and a density of 0.3mg/cm 3;
(4) 90g of ablation-resistant silicon rubber, 2.5g of nano alumina (with granularity not less than 100 meshes), 5g of nano silica aerogel (with granularity not less than 100 meshes), 80g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2:2), 25g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(5) 100 Parts by mass of coating base material A0, 2 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 10 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 3.5g and 4.0g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
the prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by No. 120 solvent oil respectively, then the B component (the thickness of a single layer is 0.2 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.1 mm) and the B component are overlapped and coated, the A component is coated for 2 times, the B component is coated for 3 times, and the room temperature is dried for 6 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.38g/cm 3, the room temperature thermal conductivity is 0.072W/(m.K), the average electromagnetic shielding efficiency is 75dB in the frequency range of 1.5-18GHz, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Example 4:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,10 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 5-45 mu m are obtained through vacuum drying;
(2) Loading 2% of cobalt tungstate on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the mesoporous silica microspheres through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading is 5% of the mass of the mesoporous silica microspheres, so that the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler is prepared;
(3) Weighing 5g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 10g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (deionized water solution of 5% N-methylpyrrolidone), and carrying out stirring and ultrasonic crushing to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying the nano carbon sol system to obtain an ultra-light flexible nano carbon material, stirring and oscillating the material, crushing the material into ultra-light flexible nano carbon powder filler, and pulverizing to obtain powder with a size of 50-150 mu m and a density of 0.3mg/cm 3;
(4) 90g of ablation-resistant silicon rubber, 2.5g of nano alumina (with granularity not less than 100 meshes), 5g of nano silica aerogel (with granularity not less than 100 meshes), 80g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2:2), 25g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(5) 100 Parts by mass of coating base material A0, 15 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 40 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 3.5g and 4.8g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
the prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by No. 120 solvent oil respectively, then the B component (the thickness of a single layer is 0.2 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.1 mm) and the B component are overlapped and coated, the A component is coated for 2 times, the B component is coated for 3 times, and the room temperature is dried for 6 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.40g/cm 3, the room temperature thermal conductivity is 0.081W/(m.K), the average electromagnetic shielding effectiveness is 78dB in the frequency range of 1.5-18GHz, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Example 5:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,10 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 5-45 mu m are obtained through vacuum drying;
(2) Loading 2% of cobalt tungstate on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the mesoporous silica microspheres through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading is 5% of the mass of the mesoporous silica microspheres, so that the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler is prepared;
(3) Weighing 5g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 10g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (deionized water solution of 5% N-methylpyrrolidone), and carrying out stirring and ultrasonic crushing to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying the nano carbon sol system to obtain an ultra-light flexible nano carbon material, stirring and oscillating the material, crushing the material into ultra-light flexible nano carbon powder filler, and pulverizing to obtain powder with a size of 50-150 mu m and a density of 0.3mg/cm 3;
(4) 90g of ablation-resistant silicon rubber, 2.5g of nano alumina (with granularity not less than 100 meshes), 5g of nano silica aerogel (with granularity not less than 100 meshes), 80g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2:2), 25g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(5) 100 Parts by mass of coating base material A0, 15 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 40 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 3.5g and 4.8g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
The prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is prepared by respectively diluting the two components (A and B) with petroleum ether, then coating the B component (the thickness of a single layer is 0.2 mm) on the surface of a substrate, and then overlapping and coating the A component (the thickness of the single layer is 0.1 mm) and the B component, coating the A component for 4 times, coating the B component for 5 times, and drying at room temperature for 6 days.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.40g/cm 3, the room temperature thermal conductivity is 0.080W/(m.K), the average electromagnetic shielding effectiveness is 85dB in the range of 1.5-18GHz frequency band, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Example 6:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,10 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 5-45 mu m are obtained through vacuum drying;
(2) Loading 2% of cobalt tungstate on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the mesoporous silica microspheres through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading is 5% of the mass of the mesoporous silica microspheres, so that the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler is prepared;
(3) Weighing 5g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 10g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (deionized water solution of 5% N-methylpyrrolidone), and carrying out stirring and ultrasonic crushing to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying the nano carbon sol system to obtain an ultra-light flexible nano carbon material, stirring and oscillating the material, crushing the material into ultra-light flexible nano carbon powder filler, and pulverizing to obtain powder with a size of 50-150 mu m and a density of 0.3mg/cm 3;
(4) 90g of ablation-resistant silicon rubber, 2.5g of nano alumina (with granularity not less than 100 meshes), 5g of nano silica aerogel (with granularity not less than 100 meshes), 80g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2:2), 25g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(5) 100 Parts by mass of coating base material A0, 15 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 40 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 6.0g and 6.5g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
The prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is prepared by respectively diluting the two components (A and B) with petroleum ether, then coating the B component (the thickness of a single layer is 0.2 mm) on the surface of a substrate, and then overlapping and coating the A component (the thickness of the single layer is 0.1 mm) and the B component, coating the A component for 4 times, coating the B component for 5 times, and drying at room temperature for 4 days.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.39g/cm 3, the room temperature thermal conductivity is 0.066W/(m.K), the average electromagnetic shielding efficiency is 87dB in the frequency range of 1.5-18GHz, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Example 7:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,12 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 10-45 mu m are obtained through vacuum drying;
(2) Loading 1% of cobalt tungstate on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the mesoporous silica microspheres through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading is 3% of the mass of the mesoporous silica microspheres, so as to prepare the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler;
(3) Weighing 8g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 10g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (deionized water solution of 5% N-methylpyrrolidone), and carrying out stirring and ultrasonic crushing to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying the nano carbon sol system to obtain an ultra-light flexible nano carbon material, stirring and oscillating the material, crushing the material into ultra-light flexible nano carbon powder filler, and pulverizing to obtain powder with a size of 50-150 mu m and a density of 0.5mg/cm 3;
(4) 110g of ablation-resistant silicon rubber, 7g of nano alumina (with granularity not less than 100 meshes), 8g of nano silica aerogel (with granularity not less than 100 meshes), 60g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2:2), 20g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(5) 100 Parts by mass of coating base material A0, 10 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 30 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 5.4g and 7.0g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
The prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by 120 # solvent oil respectively, then the B component (the thickness of a single layer is 0.2 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.1 mm) and the B component are coated in an overlapping manner, the A component is coated for 4 times, the B component is coated for 5 times, and the room temperature drying is carried out for 6 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.40g/cm 3, the room temperature thermal conductivity is 0.072W/(m.K), the average electromagnetic shielding efficiency is 83dB in the frequency range of 1.5-18GHz, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Example 8:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,12 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 10-45 mu m are obtained through vacuum drying;
(2) Loading 1% nickel nitrate on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the mesoporous silica microspheres through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading amount is 4% of the mass of the mesoporous silica microspheres, so as to prepare the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler;
(3) Weighing 8g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 10g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (deionized water solution of 5% N-methylpyrrolidone), and carrying out stirring and ultrasonic crushing to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying the nano carbon sol system to obtain an ultra-light flexible nano carbon material, stirring and oscillating the material, crushing the material into ultra-light flexible nano carbon powder filler, and pulverizing to obtain powder with a size of 50-150 mu m and a density of 0.5mg/cm 3;
(4) 110g of room temperature vulcanized silicone rubber, 7g of nano alumina (with granularity not less than 100 meshes), 8g of nano silica aerogel (with granularity not less than 100 meshes), 60g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2:2), 20g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(5) 100 Parts by mass of coating base material A0, 10 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 30 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 5.0g and 6.5g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
The prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by 120 # solvent oil respectively, then the B component (the thickness of a single layer is 0.2 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.1 mm) and the B component are coated in an overlapping manner, the A component is coated for 4 times, the B component is coated for 5 times, and the room temperature drying is carried out for 6 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.37g/cm 3, the room temperature thermal conductivity is 0.075W/(m.K), the average electromagnetic shielding effectiveness is 85dB in the frequency range of 1.5-18GHz, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Example 9:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,12 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 10-45 mu m are obtained through vacuum drying;
(2) Loading 1% of cobalt tetraoxide on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the carbon source through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading amount is 5% of the mass of the mesoporous silica microspheres, so that the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler is prepared;
(3) Weighing 8g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 10g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (deionized water solution of 5% N-methylpyrrolidone), and carrying out stirring and ultrasonic crushing to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying the nano carbon sol system to obtain an ultra-light flexible nano carbon material, stirring and oscillating the material, crushing the material into ultra-light flexible nano carbon powder filler, and pulverizing to obtain powder with a size of 50-150 mu m and a density of 0.5mg/cm 3;
(4) 110g of methyl phenyl silicone resin and room temperature vulcanized silicone rubber compound system (compound according to the mass ratio of 5:4), 7g of nano alumina (granularity is more than or equal to 100 meshes), 8g of nano silica aerogel (granularity is more than or equal to 100 meshes), 60g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compound according to the mass ratio of 1.2:1:1.5:2:2), 20g of hollow ceramic microspheres (with the external diameter of less than or equal to 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the paint base A0.
(5) 100 Parts by mass of coating base material A0, 10 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 30 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 6.0g and 5.5g of curing agent (the curing agent is tetraethylene tetramine) and uniformly mixed to respectively obtain a double-component A component and a double-component B component of the flexible electromagnetic shielding ablation-resistant heat insulation coating.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
The prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by 120 # solvent oil respectively, then the B component (the thickness of a single layer is 0.2 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.1 mm) and the B component are coated in an overlapping manner, the A component is coated for 4 times, the B component is coated for 5 times, and the room temperature drying is carried out for 6 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.37g/cm 3, the room temperature thermal conductivity is 0.069W/(m.K), the average electromagnetic shielding efficiency is 86dB in the frequency range of 1.5-18GHz, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Example 10:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,15 ml of 5wt% tetraethyl orthosilicate ethanol solution is dropwise added into the mixture, after the mixture is reacted for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 30-50 mu m are obtained through vacuum drying;
(2) Loading 1% of cobalt tetraoxide on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the carbon source through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading amount is 5% of the mass of the mesoporous silica microspheres, so that the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler is prepared;
(3) Weighing 8g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 10g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (deionized water solution of 5% N-methylpyrrolidone), and carrying out stirring and ultrasonic crushing to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying the nano carbon sol system to obtain an ultra-light flexible nano carbon material, stirring and oscillating the material, crushing the material into ultra-light flexible nano carbon powder filler, and pulverizing to obtain powder with a size of 50-150 mu m and a density of 0.5mg/cm 3;
(4) 110g of methyl phenyl silicone resin and room temperature vulcanized silicone rubber compound system (compound according to the mass ratio of 5:4), 7g of nano alumina (granularity is more than or equal to 100 meshes), 8g of nano silica aerogel (granularity is more than or equal to 100 meshes), 60g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compound according to the mass ratio of 1.2:1:1.5:2:2), 20g of hollow ceramic microspheres (with the external diameter of less than or equal to 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the paint base A0.
(5) 100 Parts by mass of coating base material A0, 10 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 30 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 6.0g and 5.5g of curing agent (the curing agent is tetraethylene tetramine) and uniformly mixed to respectively obtain a double-component A component and a double-component B component of the flexible electromagnetic shielding ablation-resistant heat insulation coating.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
The prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by 120 # solvent oil respectively, then the B component (the thickness of a single layer is 0.4 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.3 mm) and the B component are coated in an overlapping manner, the A component is coated for 4 times, the B component is coated for 5 times, and the room temperature drying is carried out for 7 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.36g/cm 3, the room temperature thermal conductivity is 0.070W/(m.K), the average electromagnetic shielding effectiveness is 74dB in the frequency range of 1.5-18GHz, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Example 11:
The embodiment particularly discloses a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,15 ml of 5wt% tetraethyl orthosilicate ethanol solution is dropwise added into the mixture, after the mixture is reacted for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 30-50 mu m are obtained through vacuum drying;
(2) Loading 1% of cobalt tetraoxide on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the carbon source through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading amount is 5% of the mass of the mesoporous silica microspheres, so that the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler is prepared;
(3) Weighing 8g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 10g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (deionized water solution of 5% N-methylpyrrolidone), and carrying out stirring and ultrasonic crushing to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying are carried out on the nano carbon sol system to obtain an ultra-light flexible nano carbon material, the material is stirred and oscillated and smashed into ultra-light flexible nano carbon powder filler, the size of the powder after pulverization is 50-200 mu m, and the density is 0.5mg/cm 3;
(4) 120g of methyl phenyl silicone resin and room temperature vulcanized silicone rubber compound system (compound according to the mass ratio of 5:4), 7g of nano alumina (with the granularity of more than or equal to 100 meshes), 8g of nano silica aerogel (with the granularity of more than or equal to 100 meshes), 60g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder, zinc oxide powder, manganese oxide powder and zirconium oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2:2.1:1.5:1, the granularity of more than or equal to 200 meshes) and 20g of hollow glass microspheres (with the external diameter of less than or equal to 200 mu m), and then a small amount of butyl acetate is selectively added and uniformly mixed to prepare the paint base A0.
(5) 100 Parts by mass of coating base material A0, 10 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 30 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 10.0g and 8.0g of curing agent (the curing agent is tetraethylene tetramine) and uniformly mixed to respectively obtain a double-component A component and a double-component B component of the flexible electromagnetic shielding ablation-resistant heat insulation coating.
The embodiment also specifically discloses a preparation method of the flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
The prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by No. 120 solvent oil respectively, then the B component (the thickness of a single layer is 0.3 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.2 mm) and the B component are coated in an overlapping manner, the A component is coated for 4 times, the B component is coated for 5 times, and the room temperature is dried for 4 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.39g/cm 3, the room temperature thermal conductivity is 0.068W/(m.K), the average electromagnetic shielding efficiency is 76dB in the frequency range of 1.5-18GHz, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Comparative example 1:
The comparative example adopts a preparation method of a flexible ablation-resistant heat-insulating coating, which comprises the following steps:
(1) 90g of ablation-resistant silicon rubber, 2.5g of nano aluminum oxide (with granularity not less than 100 meshes), 2.5g of mica powder (with granularity not less than 100 meshes), 15g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2), 2g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material.
(2) And adding 4.1g of curing agent (the curing agent is prepared by mixing ethyl orthosilicate and dibutyltin dilaurate with the ratio of 18:1) into 100g of coating base material, and uniformly mixing to obtain the flexible electromagnetic shielding ablation-resistant heat-insulating coating wet coating.
The comparative example adopts a preparation method of a flexible ablation-resistant thermal insulation coating, which comprises the following steps:
diluting the prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating with No. 120 solvent oil, then brushing 0.7mm on a substrate, and drying at room temperature for 6 days to obtain the light flexible electromagnetic shielding ablation-resistant heat-insulating coating.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.32g/cm 3, the room temperature thermal conductivity is 0.045W/(m.K), the electromagnetic shielding effect is almost absent, and the external surface of the coating cracks after the thermal examination of 600s at 1200 ℃.
Comparative example 2:
The comparative example adopts a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 5g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 5g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (5% of deionized water solution of N-methylpyrrolidone), and carrying out ultrasonic crushing by virtue of stirring to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying are carried out on the nano carbon sol system to obtain an ultra-light flexible nano carbon material, the material is stirred and oscillated and smashed into ultra-light flexible nano carbon powder filler, the powder size is 50-150 mu m after pulverization, and the density is 0.1mg/cm 3;
(2) 90g of ablation-resistant silicon rubber, 2.5g of nano aluminum oxide (with granularity not less than 100 meshes), 2.5g of mica powder (with granularity not less than 100 meshes), 15g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2), 2g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(3) And uniformly mixing 100 parts by mass of coating base material A0 and 10 parts by mass of ultra-soft nano carbon powder filler to prepare coating base material B0.
(4) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 4.1g and 1.8g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The comparative example adopts a preparation method of a flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
the prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by No. 120 solvent oil respectively, then the B component (the thickness of a single layer is 0.2 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.1 mm) and the B component are overlapped and coated, the A component is coated for 2 times, the B component is coated for 3 times, and the room temperature is dried for 6 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.37g/cm 3, the room temperature thermal conductivity is 0.050W/(m.K), the average electromagnetic shielding efficiency is 31dB in the frequency range of 1.5-18GHz, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Comparative example 3:
The comparative example adopts a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,10 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 5-45 mu m are obtained through vacuum drying;
(2) Loading cobalt tungstate with the weight of 0.02% on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the mesoporous silica microspheres through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading amount is 0.1% of the mass of the mesoporous silica microspheres, so as to prepare the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler;
(3) 90g of ablation-resistant silicon rubber, 2.5g of nano aluminum oxide (with granularity not less than 100 meshes), 2.5g of mica powder (with granularity not less than 100 meshes), 15g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2), 2g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(4) 100 Parts by mass of coating base material A0 and 2 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler are uniformly mixed to prepare coating base material B0.
(5) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 4.1g and 2.8g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The comparative example adopts a preparation method of a flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
the prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by No. 120 solvent oil respectively, then the B component (the thickness of a single layer is 0.2 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.1 mm) and the B component are overlapped and coated, the A component is coated for 2 times, the B component is coated for 3 times, and the room temperature is dried for 6 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.38g/cm 3, the room temperature thermal conductivity is 0.046W/(m.K), the average electromagnetic shielding efficiency is 39dB in the range of 1.5-18GHz frequency band, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
Comparative example 4:
The comparative example adopts a preparation method of a flexible electromagnetic shielding ablation-resistant heat-insulating coating double component, which comprises the following steps:
(1) Weighing 0.03gKCl, 10ml deionized water, 90ml absolute ethyl alcohol and a proper amount of ammonia water in a three-neck flask, and uniformly stirring; under the condition of stirring in a water bath at 30 ℃,10 ml of 5wt% tetraethyl orthosilicate ethanol solution is added dropwise into the mixture, after the mixture reacts for 6 hours, the reaction is stopped, the obtained silicon dioxide microspheres are respectively washed 3 times by absolute ethanol and deionized water, and the monodisperse mesoporous silicon dioxide microspheres with the size distribution of 5-45 mu m are obtained through vacuum drying;
(2) Loading cobalt tungstate with the weight of 0.02% on the mesoporous silica microspheres, then taking methane as a carbon source, taking hydrogen as a reducing agent, and growing continuously lapped carbon nanotubes on the mesoporous silica microspheres through chemical vapor deposition, wherein the diameter of the obtained carbon nanotubes is less than or equal to 50nm, the length is more than or equal to 10 mu m, and the loading amount is 0.1% of the mass of the mesoporous silica microspheres, so as to prepare the self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler;
(3) Weighing 5g of graphene oxide (the sheet size is less than or equal to 300 mu m) and 5g of single-walled carbon nanotubes (the length is less than or equal to 50 mu m and the diameter of a tube bundle is less than or equal to 50 nm), sequentially adding 0.1wt% of sodium deoxycholate solution (5% of deionized water solution of N-methylpyrrolidone), and carrying out ultrasonic crushing by virtue of stirring to obtain a uniformly mixed nano carbon sol system; ageing, solvent replacement and drying are carried out on the nano carbon sol system to obtain an ultra-light flexible nano carbon material, the material is stirred and oscillated and smashed into ultra-light flexible nano carbon powder filler, the powder size is 50-150 mu m after pulverization, and the density is 0.1mg/cm 3;
(4) 90g of ablation-resistant silicon rubber, 2.5g of nano aluminum oxide (with granularity not less than 100 meshes), 2.5g of mica powder (with granularity not less than 100 meshes), 15g of ablation-resistant oxide powder (sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder and zinc oxide powder are compounded according to the mass ratio of 1.2:1:1.5:2), 2g of hollow ceramic microspheres (with external diameter not more than 200 mu m), and a small amount of butyl acetate is selectively added and uniformly mixed to prepare the coating base material A0.
(5) 100 Parts by mass of coating base material A0, 2 parts by mass of continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler and 10 parts by mass of ultra-soft nano carbon powder filler are uniformly mixed to prepare coating base material B0.
(6) 100G of coating base material A0 and 100g of coating base material B0 are respectively added with 4.1g and 2.0g of curing agent (the curing agent is prepared by mixing tetraethoxysilane and dibutyltin dilaurate with the ratio of 18:1), and the components A and B of the flexible electromagnetic shielding ablation-resistant heat insulation coating are respectively obtained.
The comparative example adopts a preparation method of a flexible electromagnetic shielding ablation-resistant thermal insulation coating, which comprises the following steps:
The prepared light flexible electromagnetic shielding ablation-resistant heat-insulating coating is diluted by 120 # solvent oil respectively, then the B component (the thickness of a single layer is 0.2 mm) is coated on the surface of a substrate, then the A component (the thickness of the single layer is 0.1 mm) and the B component are coated in an overlapping manner, the A component is coated for 1 time, the B component is coated for 2 times, and the room temperature drying is carried out for 6 days, so that the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is obtained.
And (3) testing the performance of the coating product: the density of the prepared light flexible electromagnetic shielding ablation-resistant thermal insulation coating is 0.34g/cm 3, the room temperature thermal conductivity is 0.055W/(m.K), the average electromagnetic shielding effectiveness is 45dB in the range of 1.5-18GHz frequency band, the thermal examination at 1200 ℃ can be carried out for 600s, and the outer surface of the coating is kept complete after the examination.
As can be seen from the above examples 1 to 11 and comparative examples 1 to 4, in the examples, compared with the comparative examples, since the self-made continuous lap joint carbon nanotube-supported silica mesoporous microsphere light heat insulation filler and the ultra-soft nano carbon powder light filler were prepared through the first 3 steps, the above two fillers exhibited excellent electromagnetic shielding effectiveness through lap joint, the fillers were mixed with the coating base material, and the two-component overlapping coating layering process was combined, and after the finally prepared coating was prepared into a coating product, the flexible electromagnetic shielding property and the ablation-resistant heat insulation property of the coating were remarkably increased on the basis of not damaging the original properties.
Although the present invention has been described with reference to the above embodiments, it should be understood that the invention is not limited thereto, and that modifications and equivalents may be made thereto by those skilled in the art, which modifications and equivalents are intended to be included within the scope of the present invention as defined by the appended claims.
Claims (10)
1. The preparation method of the light flexible electromagnetic shielding ablation-resistant heat-insulating coating is characterized by comprising the following steps of:
(1) Preparing mesoporous silica microspheres as a load matrix material, loading a catalyst on the mesoporous silica microspheres, wherein the catalyst loading amount is 0.02% -2% of the mass of the mesoporous silica microspheres, and then growing continuously lapped carbon nanotubes in a surface layer mesoporous structure and on the outer surface of the material, wherein the obtained carbon nanotube loading amount is 0.05% -5% of the mass of the mesoporous silica microspheres, the pipe diameter is less than or equal to 50nm, and the length is more than or equal to 10 mu m, so as to obtain self-made continuously lapped carbon nanotube loaded silica mesoporous microsphere light heat insulation filler;
(2) Preparing an ultra-light nano carbon material, and then crushing the ultra-light nano carbon material into ultra-light nano carbon powder filler through oscillation treatment;
(3) Mixing a matrix film forming material, a reinforcing filler, ablation-resistant oxide powder and hollow microspheres according to the mass ratio of (90-120): (5-15): (15-80): (2-25) to obtain a coating base material A0 component;
(4) Mixing the coating base material A0 obtained in the step (3), the continuous lap joint carbon nano tube loaded silicon dioxide mesoporous microsphere light heat insulation filler obtained in the step (1) and the ultra-light nano carbon powder filler obtained in the step (2) according to the mass ratio of 100 (2-15) (10-40) to obtain a coating base material B0 component;
(5) Adding a curing agent into the coating base material A0 obtained in the step (3) for stirring and mixing uniformly, adding the curing agent into the coating base material B0 obtained in the step (4) for stirring and mixing uniformly, and preparing the component A and the component B of the light flexible electromagnetic shielding ablation-resistant heat insulation coating.
2. The method of claim 1, wherein the mesoporous silica microspheres have a size of 5-50 μm; the mesoporous silica supported catalyst is a salt containing one or more elements of iron, cobalt and nickel.
3. The preparation method of claim 1, wherein the ultra-light nano carbon material is an ultra-light elastic aerogel material composed of one or more of carbon nano tubes and graphene, the tube diameter of the carbon nano tubes is less than or equal to 50nm, the length of the carbon nano tubes is less than or equal to 50 μm, the size of graphene sheets is less than or equal to 300 μm, and the density of the ultra-light elastic aerogel material is 0.05-0.50mg/cm 3; the size of the ultra-light nano carbon powder material is 50-200 mu m, and the specific surface area is more than or equal to 800m 2/g.
4. The preparation method of claim 1, wherein the matrix film forming material is one or more of ablation-resistant modified organic silicon rubber and organic silicon resin, the reinforcing filler is one or more of nano silicon dioxide aerogel, nano aluminum oxide, mica powder and talcum powder, the ablation-resistant oxide powder is one or more of sodium oxide powder, potassium oxide powder, boron oxide powder, ferric oxide powder, phosphorus oxide powder, zinc oxide powder, manganese oxide powder and zirconium oxide powder, and the hollow microsphere is one or more of hollow glass microsphere and hollow ceramic microsphere.
5. The method according to claim 1 or 4, wherein the particle size of the reinforcing filler is not less than 100 meshes, the particle size of the ablation-resistant oxide powder is not less than 200 meshes, and the outer diameter of the hollow microspheres is not more than 200 μm.
6. The preparation method of claim 1, wherein the curing agent is one of organotin and amine, the adding amount of the curing agent is 5% -25% of the mass of the matrix film forming matter in the coating base material A0, and the adding amount of the curing agent is 5% -25% of the mass of the matrix film forming matter in the coating base material B0; the corresponding curing agent is selected according to the components used in the coating base A0 or B0.
7. A light flexible electromagnetic shielding ablation-resistant heat insulation coating double-component comprising a component A and a component B, which is characterized by being prepared by the preparation method of any one of claims 1-6.
8. The preparation method of the light flexible electromagnetic shielding ablation-resistant thermal insulation coating is characterized by comprising the following steps of: the light flexible electromagnetic shielding ablation-resistant heat insulation coating prepared by the preparation method of any one of claims 1-6 is prepared by diluting a two-component A and a two-component B with a diluent to required viscosity, overlapping and coating the two-component A and the two-component B by a brushing method, completing the whole brushing process, and drying to obtain the light flexible electromagnetic shielding ablation-resistant heat insulation coating.
9. The preparation method of claim 8, wherein the diluent is one or more of cyclohexane, ethyl acetate, butyl acetate, toluene, xylene, petroleum ether, no. 6 solvent oil, no. 120 solvent oil; the brushing method is spraying; the single-layer spraying thickness of the component A is 0.1-0.3mm, and the single-layer spraying thickness of the component B is 0.2-0.4mm; the spraying times of the component A are more than or equal to 2 times, and the spraying times of the component B are more than or equal to 3 times; the drying mode is that the drying is carried out at room temperature and normal pressure, and the time is 4-7 days.
10. A lightweight flexible electromagnetic shielding ablation-resistant thermal barrier coating prepared by the preparation method of claim 8 or 9.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311720735.7A CN117925089A (en) | 2023-12-14 | 2023-12-14 | Flexible electromagnetic shielding ablation-resistant heat insulation coating double-component and coating and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311720735.7A CN117925089A (en) | 2023-12-14 | 2023-12-14 | Flexible electromagnetic shielding ablation-resistant heat insulation coating double-component and coating and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN117925089A true CN117925089A (en) | 2024-04-26 |
Family
ID=90749819
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202311720735.7A Pending CN117925089A (en) | 2023-12-14 | 2023-12-14 | Flexible electromagnetic shielding ablation-resistant heat insulation coating double-component and coating and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN117925089A (en) |
-
2023
- 2023-12-14 CN CN202311720735.7A patent/CN117925089A/en active Pending
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Xu et al. | Heteroatoms-doped carbon nanocages with enhanced dipolar and defective polarization toward light-weight microwave absorbers | |
US11235560B2 (en) | Electromagnetic wave absorption material and electromagnetic wave absorber | |
WO2019109726A1 (en) | Electromagnetic shielding filler, electromagnetic shielding coating comprising same, preparation method and application thereof | |
Shah et al. | Microwave absorption and flexural properties of Fe nanoparticle/carbon fiber/epoxy resin composite plates | |
Ren et al. | Preparation and electromagnetic wave absorption properties of carbon nanotubes loaded Fe3O4 composites | |
Uddin et al. | Enhanced microwave absorption from the magnetic-dielectric interface: a hybrid rGO@ Ni-doped-MoS2 | |
CN105950112B (en) | A kind of nano combined absorbing material and preparation method thereof | |
CN113185898A (en) | Method for preparing super-hydrophobic dual-functional coating by adopting spraying method | |
CN109852344A (en) | A kind of composite wave-suction material and preparation method thereof | |
CN111517831A (en) | Metal-carbon nanotube foam composite material and preparation method and application thereof | |
CN110003657A (en) | Silicon rubber nano composite material and preparation method thereof with isolation structure | |
Li et al. | Constructing 3D Tent-Like frameworks in melamine hybrid foam for superior microwave absorption and thermal insulation | |
CN102532889B (en) | Carbon nanotube-doped poly-Schiff base/ferrite composite stealth material | |
CN114479639A (en) | Preparation method and application of radiation heat-dissipation coating | |
CN117925089A (en) | Flexible electromagnetic shielding ablation-resistant heat insulation coating double-component and coating and preparation method thereof | |
You et al. | Fabrication of high-performance electromagnetic wave absorbing SiC composites reinforced by 3D printed carbon-based nanonetwork with Fe3O4 nanoparticles | |
WO2023050316A1 (en) | Bio-based microencapsulated mfapp flame retardant, and preparation method therefor and use thereof | |
Zhang et al. | A finite oxidation strategy for customizing heterogeneous interfaces to enhance magnetic loss ability and microwave absorption of Fe-cored carbon microcapsules | |
CN110669257A (en) | Coated modified alumina, preparation method thereof and epoxy composite insulating material | |
CN114350156A (en) | High-temperature-resistant heat-conducting wave-absorbing composite material and preparation method thereof | |
Tang et al. | Lightweight zirconium modified carbon–carbon composites with excellent microwave absorption and mechanical properties | |
CN111732871B (en) | Light high-heat-resistance coating and preparation method thereof | |
CN112940457B (en) | Flame-retardant epoxy electromagnetic shielding material and preparation method thereof | |
CN114716828B (en) | Rubber for low-resistance flame-retardant fuel cell transmission pipeline | |
CN111254718B (en) | Self-cleaning graphene carbon fiber non-woven fabric and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |