CN115745652A - Light-weight bearing multifunctional SiC aerogel composite material and preparation method thereof - Google Patents
Light-weight bearing multifunctional SiC aerogel composite material and preparation method thereof Download PDFInfo
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- 239000004964 aerogel Substances 0.000 title claims abstract description 70
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 60
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 14
- 230000008878 coupling Effects 0.000 claims abstract description 8
- 238000010168 coupling process Methods 0.000 claims abstract description 8
- 238000005859 coupling reaction Methods 0.000 claims abstract description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 56
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000006260 foam Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 235000012239 silicon dioxide Nutrition 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 10
- 239000011148 porous material Substances 0.000 claims description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 9
- 238000007158 vacuum pyrolysis Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004965 Silica aerogel Substances 0.000 claims description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 235000019353 potassium silicate Nutrition 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 230000003014 reinforcing effect Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000011946 reduction process Methods 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 10
- 238000009413 insulation Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 238000007598 dipping method Methods 0.000 description 4
- 238000002679 ablation Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000004966 Carbon aerogel Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 description 1
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Abstract
The application discloses multi-functional SiC aerogel combined material is born to light and preparation method thereof, multi-functional SiC aerogel combined material is born to light includes carbon foam skeleton, sets up in the intensive coating on carbon foam skeleton surface and sets up the aerogel in carbon foam skeleton hole, carbon foam skeleton is three-dimensional open cell structure, the aerogel is carborundum aerogel to be three-dimensional network structure, be two network coupling nested structures between carbon foam skeleton and the aerogel. The light-weight load-bearing multifunctional SiC aerogel composite material has the advantages of small density, high strength, excellent heat insulation performance and capability of regulating and controlling the dielectric performance of the whole material and realizing incident absorption of electromagnetic waves, thereby realizing wave absorption and achieving the stealth effect.
Description
Technical Field
The application relates to the technical field of composite materials, in particular to a light-weight bearing multifunctional SiC aerogel composite material and a preparation method thereof.
Background
When the hypersonic aerocraft flies at high speed with the Mach number of 6-10, the temperature range of the wing leading edge can reach 700 ℃ or even more than 1000 ℃. Due to the extremely severe high-temperature thermal environment, the problem of the thermal strength of materials and structures of hypersonic flight vehicles becomes one of the important key problems of research success and failure. In addition, with the development of wireless detection technology and ultrahigh-speed precise guidance weapons, hypersonic aircrafts are urgently required to have excellent electromagnetic wave stealth characteristics, and in the fields of aerospace and new generation weapons, wave-absorbing materials are required to have multiple functions of light weight, high temperature resistance, multiple frequency bands, adjustability and the like.
Aerogels are superporous, high specific surface area (≧ 500 m) with a porosity of about 90% to 99.9% and a pore size in the range of 1nm to 100nm 2 The material is characterized by comprising the following components in parts by weight, namely,/g) and is a material with excellent properties such as ultra-light weight, ultra-heat insulation, ultra-low dielectric property and the like, and the materials are classified in a plurality of categories, but have single property, for example, silica aerogel is not high-temperature resistant, ablation resistant and can not be used in a high-temperature environment, the permeation of electromagnetic waves is mainly realized, and the wave absorbing property is basically absent; the silicon carbide nanowire aerogel is low in strength, easy to collapse in a network structure, easy to tangle and agglomerate among nanowires, unstable in performance, complex in preparation process and high in requirement on equipment investment; the carbon aerogel high-temperature aerobic environment cannot be used, has low structural strength, is easy to react with oxygen, mainly shields and reflects electromagnetic waves, has no wave-absorbing performance, and cannot meet the requirements of ablation resistance, heat insulation and wave-absorbing invisibility in the field of aerospace.
Disclosure of Invention
The invention aims to provide a light-weight load-bearing multifunctional SiC aerogel composite material and a preparation method thereof, which are used for overcoming the defects in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the application discloses multi-functional SiC aerogel combined material is born to light, include carbon foam skeleton, set up in the reinforced coating on carbon foam skeleton surface and set up the aerogel in carbon foam skeleton hole, carbon foam skeleton is three-dimensional open cell structure, the aerogel is carborundum aerogel to be three-dimensional network structure, be two network coupling nested structure between carbon foam skeleton and the aerogel.
Further, in the light-weight bearing multifunctional SiC aerogel composite material, the reinforced coating is a silicon carbide coating which is discontinuously distributed, and the thickness of the reinforced coating is 1.2-1.5 μm.
Further, in the light load-bearing multifunctional SiC aerogel composite material, the porosity of the carbon foam skeleton is 95.0-99.0%, and the pore size is 25.0-40.0 μm.
The application also discloses a method for preparing the light-weight load-bearing multifunctional SiC aerogel composite material, which comprises the following steps:
1) Preparing a carbon foam framework: placing the light porous melamine foam in a vacuum pyrolysis furnace, and pyrolyzing the light porous melamine foam in a nitrogen protection gradient heating mode to prepare a carbon foam framework;
2) Reinforcing the carbon foam framework: preparing a silicon carbide coating on the inner walls of the pores of the carbon foam framework by a chemical vapor deposition process to obtain carbon/silicon carbide foam;
3) And gel: preparing silica aerogel in the gaps of the carbon/silicon carbide foam by a freeze-drying process;
4) And preparing the aerogel: and pyrolyzing the silicon dioxide aerogel into silicon carbide aerogel through a carbothermic reduction process to obtain the silicon carbide aerogel composite material.
Further, in the above preparation method of the light-weight load-bearing multifunctional SiC aerogel composite, step 3) includes the following steps:
31 Preparation of sol): preparing silica sol by using water glass as a precursor;
32 Dipping, dipping: impregnating a carbon/silicon carbide foam in a silica sol;
33 And aging: repeatedly leaching the carbon/silicon carbide foam impregnated with the silica sol by using ethanol for 2-3 times, and aging in a water bath environment at 50-60 ℃ for 2-5 days;
34 Freeze-drying: and (3) putting the silicon dioxide aerogel into a refrigerator, freezing the silicon dioxide aerogel for 2 to 3 days at the temperature of minus 30 ℃, and then vacuumizing and drying the silicon dioxide aerogel for 2 to 3 days at the temperature of 25 to 40 ℃, namely preparing the silicon dioxide aerogel in the gaps of the carbon/silicon carbide foam.
Further, in the preparation method of the light-weight load-bearing multifunctional SiC aerogel composite material, the carbothermic reduction method in the step 4) is carried out in a vacuum pyrolysis furnace, 50ml/min of inert gas is introduced, the carbothermic reduction method is heated to 1200-1500 ℃ at the heating rate of 15-25 ℃/min, and the temperature is kept for 2-4 h.
Compared with the prior art, the invention has the advantages that: the silicon carbide aerogel composite material prepared by the preparation method disclosed by the invention is small in density and high in strength, the pore structure of the double-network coupling nested structure inhibits air convection conduction, the heat insulation performance is excellent, the silicon carbide coating and the silicon carbide aerogel material have excellent high-temperature-resistant and oxidation-resistant performances, the dielectric performance of the whole material can be regulated and controlled by the double-network coupling nested structure formed by the carbon foam framework and the silicon carbide aerogel, electromagnetic wave incident absorption can be realized, the wave absorption is realized, the stealth effect is achieved, and the performance requirements of the aerospace field on ablation resistance, heat insulation and wave absorption stealth are met.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural diagram of a light-weight load-bearing multifunctional SiC aerogel composite according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described in detail below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Referring to fig. 1, a preparation method of a light-weight load-bearing multifunctional SiC aerogel composite material comprises the following steps:
1) Preparing a carbon foam framework 1: placing the light porous melamine foam in a vacuum pyrolysis furnace, controlling the temperature rise rate of the vacuum pyrolysis furnace to rise from normal temperature to 350 ℃ at 7.0 ℃/min, rising from 350 ℃ to 450 ℃ at 2.0 ℃/min, rising from 450 ℃ to 1100 ℃ at 5.7 ℃/min, preserving heat at 1100 ℃ for 2 hours, and cooling along with the furnace, wherein in the whole pyrolysis process, nitrogen is always introduced into the vacuum pyrolysis furnace at the flow rate of 50ml/min, so that a carbon foam framework with the porosity of 95.0-99.0% and the pore size of 25.0-40.0 mu m is obtained, and the carbon foam framework has a three-dimensional porous structure, and is beneficial to the subsequent deposition of a silicon carbide reinforced coating and the preparation of silicon carbide (chemical formula: siC) aerogel;
2) Reinforcing the carbon foam framework: placing the carbon foam framework into a chemical vapor deposition furnace, checking the airtightness of the chemical vapor deposition furnace, vacuumizing, introducing trichloromethylsilane, argon and hydrogen with a gas flow ratio of 1; the carbon foam framework with the improved mechanical property is used as a reinforced framework of the aerogel particles, so that the stability of the whole structure can be kept in the preparation process of the silicon carbide aerogel;
3) And gel: preparing a silica aerogel within the voids of the carbon/silicon carbide foam by a freeze-drying process;
31 Preparation of sol): the water glass is used as a precursor to prepare the silica sol, the specific formula and the process are both in the prior art, and the water glass has wide raw material sources and is suitable for industrial large-scale production;
32 Dipping, dipping: impregnating a carbon/silicon carbide foam in a silica sol;
33 And aging): repeatedly leaching the carbon/silicon carbide foam impregnated with the silica sol by using ethanol for 2-3 times, aging for 2-5 days in a water bath environment at 50-60 ℃, dissolving the uneven aerogel particles and performing polycondensation again to increase the aerogel particle linkage, thereby being beneficial to forming a reticular aerogel framework;
34 Freeze-drying: putting the mixture into a refrigerator, freezing the mixture for 2 to 3 days at the temperature of minus 30 ℃, and then vacuumizing and drying the mixture for 2 to 3 days at the temperature of 25 to 40 ℃ to prepare the silicon dioxide aerogel in gaps of the carbon/silicon carbide foam;
4) And preparing the aerogel: placing carbon/silicon carbide foam embedded with silicon dioxide aerogel in a vacuum pyrolysis furnace, introducing 50ml/min of inert gas, heating to 1200-1500 ℃ at the heating rate of 15-25 ℃/min, preserving heat for 2-4 h, and preparing the silicon dioxide aerogel into silicon carbide aerogel 2 to obtain the silicon carbide aerogel composite material, wherein the silicon carbide aerogel is in a three-dimensional net structure and is in a double-network coupling nested structure with a carbon foam framework, the mechanical property is coordinately enhanced, gaps are divided, the transmission of heat is inhibited, the heat insulation and heat prevention performance of the whole material can be improved, and each component forms a complex interface polarization relaxation phenomenon due to the difference of electromagnetic properties, so that the back-and-forth reflection, absorption and dissipation of electromagnetic waves in the material are promoted, the dissipation and absorption of the electromagnetic waves are further increased, and the functions of low heat conduction and strong wave absorption are realized.
In conclusion, the silicon carbide aerogel composite material prepared by the preparation method disclosed by the invention is small in density and high in strength, the pore structure of the double-network coupling nested structure inhibits air convection conduction, the heat insulation performance is excellent, the silicon carbide coating and the silicon carbide aerogel material have excellent high-temperature-resistant and oxidation-resistant performances, and the double-network coupling nested structure formed by the carbon foam framework and the silicon carbide aerogel can regulate and control the dielectric performance of the whole material and realize electromagnetic wave incident absorption, so that wave absorption is realized, and the stealth effect is achieved.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising one of 8230; \8230;" 8230; "does not exclude the presence of additional like elements in a process, method, article, or apparatus that comprises the element.
The foregoing is illustrative of the present disclosure and it will be appreciated by those skilled in the art that changes may be made in this embodiment without departing from the principles of the disclosure, the scope of which is defined by the appended claims.
Claims (6)
1. The utility model provides a multi-functional SiC aerogel combined material is born to light which characterized in that: including carbon foam skeleton, set up in the intensive coating on carbon foam skeleton surface and set up the aerogel in carbon foam skeleton pore space, carbon foam skeleton is three-dimensional open cell structure, the aerogel is silicon carbide aerogel to be three-dimensional network structure, be double network coupling nested structure between carbon foam skeleton and the aerogel.
2. The lightweight load-bearing multifunctional SiC aerogel composite of claim 1, characterized in that: the reinforced coating is a silicon carbide coating which is discontinuously distributed, and the thickness of the reinforced coating is 1.2-1.5 mu m.
3. The light weight, load-bearing, multifunctional SiC aerogel composite of claim 1, characterized in that: the porosity of the carbon foam skeleton is 95.0-99.0%, and the pore size is 25.0-40.0 μm.
4. A method for producing a light-weight, load-bearing multifunctional SiC aerogel composite according to any of claims 1 to 3, characterized in that it comprises the following steps:
1) Preparing a carbon foam framework: putting the light porous melamine foam into a vacuum pyrolysis furnace, and pyrolyzing the light porous melamine foam in a gradient heating mode under the protection of nitrogen to prepare a carbon foam framework;
2) Reinforcing a carbon foam framework: preparing a silicon carbide coating on the inner walls of the pores of the carbon foam framework by a chemical vapor deposition process to obtain carbon/silicon carbide foam;
3) And gel: preparing a silica aerogel within the voids of the carbon/silicon carbide foam by a freeze-drying process;
4) And (3) preparing the aerogel: and pyrolyzing the silicon dioxide aerogel into silicon carbide aerogel through a carbothermic reduction process to obtain the silicon carbide aerogel composite material.
5. The preparation method of the light-weight load-bearing multifunctional SiC aerogel composite material according to claim 4, wherein the step 3) comprises the following steps:
31 Preparation of sol): preparing silica sol by using water glass as a precursor;
32 ) and impregnation: impregnating carbon/silicon carbide foam in silica sol;
33 And aging: repeatedly leaching the carbon/silicon carbide foam impregnated with the silica sol by using ethanol for 2-3 times, and aging for 2-5 days in a water bath environment at 50-60 ℃;
34 And freeze-drying: and (3) putting the silicon dioxide aerogel into a refrigerator, freezing the silicon dioxide aerogel for 2 to 3 days at the temperature of minus 30 ℃, and then vacuumizing and drying the silicon dioxide aerogel for 2 to 3 days at the temperature of 25 to 40 ℃, namely preparing the silicon dioxide aerogel in the gaps of the carbon/silicon carbide foam.
6. The preparation method of the light-weight load-bearing multifunctional SiC aerogel composite material according to claim 4, wherein the preparation method comprises the following steps: the carbothermic reduction method in the step 4) is carried out in a vacuum pyrolysis furnace, 50ml/min of inert gas is introduced, the carbothermic reduction method is heated to 1200-1500 ℃ at the heating rate of 15-25 ℃/min, and the temperature is kept for 2-4 h.
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