CN114409954A - Preparation method of graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel - Google Patents
Preparation method of graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel Download PDFInfo
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 61
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 54
- 239000000919 ceramic Substances 0.000 title claims abstract description 53
- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 43
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 43
- 239000004964 aerogel Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 45
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000243 solution Substances 0.000 claims abstract description 43
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002243 precursor Substances 0.000 claims abstract description 34
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 239000002253 acid Substances 0.000 claims abstract description 23
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 18
- 238000004108 freeze drying Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 15
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000000197 pyrolysis Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000000835 fiber Substances 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000007710 freezing Methods 0.000 claims description 14
- 230000008014 freezing Effects 0.000 claims description 14
- 238000009987 spinning Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- -1 graphite alkene Chemical class 0.000 abstract description 3
- 229910002804 graphite Inorganic materials 0.000 abstract 1
- 239000010439 graphite Substances 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 6
- 230000001678 irradiating effect Effects 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 229920003257 polycarbosilane Polymers 0.000 description 4
- 239000004575 stone Substances 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000006250 one-dimensional material Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/0083—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive non-fibrous particles embedded in an electrically insulating supporting structure, e.g. powder, flakes, whiskers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The invention discloses a preparation method of graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel, which comprises the steps of adding a polymer precursor and polyvinylpyrrolidone powder into a mixed solution of tetrahydrofuran and absolute ethyl alcohol, and carrying out electrostatic spinning, heating and high-temperature pyrolysis on the mixed solution to obtain ceramic nanofiber; mixing glutaraldehyde, methanol, acetic acid, concentrated sulfuric acid and deionized water together, and magnetically stirring for 1h to obtain a glutaraldehyde acid solution; adding graphene oxide, polyvinyl alcohol and ceramic nano-fibers into an acid glutaraldehyde solution, and stirring to obtain a uniform solution; and (3) putting the uniform solution into a microwave oven for irradiation, taking out the uniform solution, performing directional freeze drying, and putting the uniform solution into the microwave oven in an argon atmosphere for microwave irradiation again to obtain the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel. The problem of current single component graphite alkene aerogel specific surface area is little, mechanical fragility is big and improper electric conductivity causes material impedance and unmatched with free space impedance is solved.
Description
Technical Field
The invention belongs to the technical field of electromagnetic wave-absorbing materials, and relates to a preparation method of graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel.
Background
Graphene-based aerogels are receiving attention from researchers due to their high porosity, large specific surface area and adjustable electrical conductivity, and these wonderful properties greatly expand their applications in the fields of supercapacitors, lithium ion batteries, sensors, electromagnetic wave absorption/shielding, environmental remediation, and the like. However, most reported graphene aerogels are generally brittle and easily damaged under mechanical deformation, and most of them are assembled by pi-pi stacking of graphene sheets, thereby greatly reducing the specific surface area and limiting the practical application thereof. Therefore, one-dimensional materials such as carbon nanotubes, metal oxide nanorods, or nanofibers are often considered to increase the specific surface area of graphene aerogels and provide functionality. For example, in an aerogel of reduced graphene oxide/titanium dioxide nanofibers designed for use in a supercapacitor, the nanofibers provide sufficient gaps as spacer layers, maintain a high surface area of graphene, and ensure accessibility of the reactants. In addition, similar spacing effect is also observed in the graphene aerogel intercalated with the carbon nano tubes, but research on the improvement of mechanical properties and wave absorption properties has not been reported.
The electrostatic spinning nanofiber with the diameter of 10-1000nm has the advantages of adjustable surface property, good flexibility, easiness in preparation and the like, so that the electrostatic spinning nanofiber has a wide prospect in construction of multifunctional aerogel. The combination of the one-dimensional electrostatic spinning nano-fiber, the two-dimensional graphene sheet and the organic polymer is the best choice for manufacturing the multifunctional mixed aerogel with high mechanical strength. However, nanofibers are often deposited densely in layered films and are difficult to incorporate into aerogels.
Disclosure of Invention
The invention aims to provide a preparation method of graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel, and solves the problem that the material impedance is not matched with the free space impedance due to small specific surface area, large mechanical brittleness and improper electrical conductivity of the existing single-component graphene aerogel.
The technical scheme adopted by the invention is that the preparation method of the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel is implemented according to the following steps:
and 4, placing the uniform solution obtained in the step 3 into a 500W microwave oven for irradiation for 1min, taking out, performing directional freeze drying, and placing into a 700W microwave oven under an argon atmosphere for microwave irradiation again for 30s to obtain the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel.
The present invention is also characterized in that,
in the step 1, the molecular weight of the polymer precursor is 1000-1600, and the molecular weight of polyvinylpyrrolidone is 1100000-1500000.
In the step 1, the mass ratio of the polymer precursor to the polyvinylpyrrolidone to the tetrahydrofuran to the absolute ethyl alcohol is 0.5-1: 0.5-1: 6: 4.
in the step 1, the spinning voltage of electrostatic spinning is 12-18 kV, the material pushing speed is 0.001-0.005 mm/s, the spinning distance is 15cm, the heating temperature is 200 ℃, the heating time is 2h, and the high-temperature pyrolysis temperature is 1200-1400 ℃.
In the step 2, the mass ratio of glutaraldehyde with the mass concentration of 25%, methanol, acetic acid, concentrated sulfuric acid and deionized water is 5-10: 10-20: 10-20: 1-2: 100.
in the step 3, the mass ratio of the graphene oxide to the polyvinyl alcohol to the ceramic nanofiber to the glutaraldehyde acid solution is 5-10: 3: 10-20: 5 to 7.
And 4, performing directional freeze drying by adopting liquid nitrogen auxiliary freezing equipment, wherein the freezing rate is 1-100 mm/min, and the drying vacuum degree is 0.01-10 Pa.
The beneficial effect of the invention is that,
(1) the aerogel prepared by the method has a three-dimensional porous structure, can provide more multiple reflection and scattering effects, effectively consumes electromagnetic waves emitted into the material, enhances the conductivity of a graphene network, further enhances the conductivity loss of the aerogel and improves the absorption performance of the electromagnetic waves;
(2) the aerogel prepared by the method has typical low density, superelasticity, good heat-insulating property and excellent minimum reflection loss, the wave-absorbing property reaches more than-60 dB, and the effective absorption bandwidth is more than 7 GHz;
(3) the aerogel prepared by the method has the characteristics of light weight, elasticity, heat insulation and high-efficiency wave absorption performance, and is suitable for the field of aviation.
Drawings
Fig. 1 is a scanning electron micrograph of graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of ceramic nanofibers according to example 1 of the present invention;
fig. 3 is a picture of the electromagnetic wave absorption performance of the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a preparation method of graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel, which is implemented according to the following steps:
the molecular weight of the polymer precursor is 1000-1600, and the molecular weight of the polyvinylpyrrolidone is 1100000-1500000;
the mass ratio of the polymer precursor to the polyvinylpyrrolidone to the tetrahydrofuran to the absolute ethyl alcohol is 0.5-1: 0.5-1: 6: 4;
spinning voltage of electrostatic spinning is 12-18 kV, material pushing speed is 0.001-0.005 mm/s, spinning distance is 15cm, heating temperature is 200 ℃, heating time is 2h, and high-temperature pyrolysis temperature is 1200-1400 ℃;
the mass ratio of glutaraldehyde with the mass concentration of 25%, methanol, acetic acid, concentrated sulfuric acid and deionized water is 5-10: 10-20: 10-20: 1-2: 100, respectively;
the mass ratio of the graphene oxide to the polyvinyl alcohol to the ceramic nanofiber to the glutaraldehyde acid solution is 5-10: 3: 10-20: 5-7;
the directional freeze drying is carried out by adopting liquid nitrogen auxiliary freezing equipment, the freezing speed is 1-100 mm/min, and the drying vacuum degree is 0.01-10 Pa.
Example 1
the mass ratio of polycarbosilane to polyvinylpyrrolidone to tetrahydrofuran to absolute ethyl alcohol is 0.5: 0.5: 6: 4;
the spinning voltage of electrostatic spinning is 16kV, the material pushing speed is 0.001mm/s, the spinning distance is 15cm, the heating temperature is 200 ℃, the heating time is 2h, and the high-temperature pyrolysis temperature is 1400 ℃;
the mass ratio of glutaraldehyde with the mass concentration of 25%, methanol, acetic acid, concentrated sulfuric acid and deionized water is 6: 12: 12: 1: 100, respectively;
the mass ratio of the graphene oxide to the polyvinyl alcohol to the ceramic nanofiber to the glutaraldehyde acid solution is 7: 3: 15: 5;
and 4, putting the uniform solution obtained in the step 3 into a 500W microwave oven, irradiating for 1min (water is put in the microwave oven to protect a magnetron), taking out, performing directional freeze drying by adopting liquid nitrogen auxiliary freezing equipment, wherein the freezing rate is 6mm/min, the drying vacuum degree is 4Pa, and after the directional freeze drying is finished, putting the obtained product into a 700W microwave oven in an argon atmosphere, and performing microwave irradiation again for 30s to obtain the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel.
In this embodiment, the polyvinyl alcohol and the glutaraldehyde are used to interconnect the graphene oxide and the ceramic nanofibers through covalent crosslinking and a hydrogen bond, and the technical indexes are as follows: the density is 9.85mg/cm3, the elasticity is 60% reversible compressibility, and the wave-absorbing efficiency is as follows: 61.02dB, and the effective wave-absorbing bandwidth is 7.04 GHz;
as can be seen from FIG. 2, the ceramic nanofibers have a long fiber structure with a diameter of 200-500 nm and a length of 50 μm.
As can be seen from FIG. 1, the ceramic nanofibers penetrate through the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel, the thickness of the graphene oxide nanosheet layer is 50-200 nanometers, and the size of the inter-lamellar hole is 30-80 micrometers.
As can be seen from fig. 3, the wave absorbing performance of the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel is as follows: 61.02dB, and the effective wave-absorbing bandwidth is 7.04 GHz.
Example 2
the mass ratio of polycarbozirconane to polyvinylpyrrolidone to tetrahydrofuran to absolute ethyl alcohol is 0.7: 0.7: 6: 4;
the spinning voltage of electrostatic spinning is 18kV, the material pushing speed is 0.002mm/s, the spinning distance is 15cm, the heating temperature is 200 ℃, the heating time is 2h, and the high-temperature pyrolysis temperature is 1300 ℃;
the mass ratio of glutaraldehyde with the mass concentration of 25%, methanol, acetic acid, concentrated sulfuric acid and deionized water is 7: 15: 15: 2: 100, respectively;
the mass ratio of the graphene oxide to the polyvinyl alcohol to the ceramic nanofiber to the glutaraldehyde acid solution is 8: 3: 15: 6;
and 4, putting the uniform solution obtained in the step 3 into a 500W microwave oven, irradiating for 1min (water is put in the microwave oven to protect a magnetron), taking out, performing directional freeze drying by adopting liquid nitrogen auxiliary freezing equipment, wherein the freezing rate is 6mm/min, the drying vacuum degree is 4Pa, and after the directional freeze drying is finished, putting the obtained product into a 700W microwave oven in an argon atmosphere, and performing microwave irradiation again for 30s to obtain the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel.
In the embodiment, the polyvinyl alcohol and the glutaraldehyde are used for interconnecting the graphene oxide and the ZrC nanofibers through covalent crosslinking and hydrogen bonding, and the technical indexes are as follows: the density is 11.63mg/cm3, the elasticity is 68% reversible compressibility, and the wave-absorbing efficiency is as follows: 65.36dB, and the effective wave-absorbing bandwidth is 7.39 GHz.
Example 3
the mass ratio of polycarbozirconane to polyvinylpyrrolidone to tetrahydrofuran to absolute ethyl alcohol is 1: 1: 6: 4;
the spinning voltage of electrostatic spinning is 12kV, the material pushing speed is 0.005mm/s, the spinning distance is 15cm, the heating temperature is 200 ℃, the heating time is 2h, and the high-temperature pyrolysis temperature is 1200 ℃;
the mass ratio of glutaraldehyde with the mass concentration of 25%, methanol, acetic acid, concentrated sulfuric acid and deionized water is 5: 10: 10: 1.5: 100, respectively;
the mass ratio of the graphene oxide to the polyvinyl alcohol to the ceramic nanofiber to the glutaraldehyde acid solution is 5: 3: 10: 7;
and 4, putting the uniform solution obtained in the step 3 into a 500W microwave oven, irradiating for 1min (water is put in the microwave oven to protect a magnetron), taking out, performing directional freeze drying by adopting liquid nitrogen auxiliary freezing equipment, wherein the freezing rate is 1mm/min, the drying vacuum degree is 0.01Pa, and after the directional freeze drying is finished, putting the obtained product into a 700W microwave oven in an argon atmosphere, and performing microwave irradiation for 30s again to obtain the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel.
Example 4
the mass ratio of polycarbosilane to polyvinylpyrrolidone to tetrahydrofuran to absolute ethyl alcohol is 0.7: 0.7: 6: 4;
the spinning voltage of electrostatic spinning is 18kV, the material pushing speed is 0.002mm/s, the spinning distance is 15cm, the heating temperature is 200 ℃, the heating time is 2h, and the high-temperature pyrolysis temperature is 1400 ℃;
the mass ratio of glutaraldehyde with the mass concentration of 25%, methanol, acetic acid, concentrated sulfuric acid and deionized water is 10: 20: 20: 2: 100, respectively;
the mass ratio of the graphene oxide to the polyvinyl alcohol to the ceramic nanofiber to the glutaraldehyde acid solution is 10: 3: 20: 6;
and 4, putting the uniform solution obtained in the step 3 into a 500W microwave oven, irradiating for 1min (300 ml of water is put into the microwave oven to protect a magnetron), taking out, performing directional freeze drying by adopting liquid nitrogen auxiliary freezing equipment, wherein the freezing rate is 100mm/min, the drying vacuum degree is 10Pa, and after the directional freeze drying is finished, putting the obtained product into a 700W microwave oven in an argon atmosphere, and performing microwave irradiation again for 30s to obtain the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel.
Claims (7)
1. The preparation method of the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel is characterized by comprising the following steps:
step 1, adding a polymer precursor and polyvinylpyrrolidone powder into a mixed solution of tetrahydrofuran and absolute ethyl alcohol for electrostatic spinning to obtain precursor fibers, and heating and pyrolyzing the precursor fibers at high temperature to obtain ceramic nanofibers;
step 2, mixing glutaraldehyde with the mass concentration of 25%, methanol, acetic acid, concentrated sulfuric acid and deionized water together, and magnetically stirring for 1h to obtain a glutaraldehyde acid solution;
step 3, adding graphene oxide, polyvinyl alcohol and the ceramic nanofiber obtained in the step 1 into the glutaraldehyde acid solution obtained in the step 2, and stirring to obtain a uniform solution;
and 4, placing the uniform solution obtained in the step 3 into a 500W microwave oven for irradiation for 1min, taking out, performing directional freeze drying, and placing into a 700W microwave oven under an argon atmosphere for microwave irradiation again for 30s to obtain the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel.
2. The preparation method of the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel according to claim 1, wherein the molecular weight of the polymer precursor in the step 1 is 1000-1600, and the molecular weight of the polyvinylpyrrolidone is 1100000-1500000.
3. The preparation method of the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel according to claim 1, wherein the mass ratio of the polymer precursor, polyvinylpyrrolidone, tetrahydrofuran and absolute ethyl alcohol in the step 1 is 0.5-1: 0.5-1: 6: 4.
4. the preparation method of the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel according to claim 1, wherein the spinning voltage of the electrostatic spinning in the step 1 is 12-18 kV, the material pushing speed is 0.001-0.005 mm/s, the spinning distance is 15cm, the heating temperature is 200 ℃, the heating time is 2h, and the high-temperature pyrolysis temperature is 1200-1400 ℃.
5. The preparation method of the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel according to claim 1, wherein the mass ratio of 25% glutaraldehyde, methanol, acetic acid, concentrated sulfuric acid and deionized water in the step 2 is 5-10: 10-20: 10-20: 1-2: 100.
6. the preparation method of the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel according to claim 1, wherein the mass ratio of the graphene oxide to the polyvinyl alcohol to the ceramic nanofiber to the glutaraldehyde acid solution in the step 3 is 5-10: 3: 10-20: 5 to 7.
7. The preparation method of the graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel according to claim 1, wherein directional freeze drying in the step 4 is performed by using liquid nitrogen-assisted freezing equipment, the freezing rate is 1-100 mm/min, and the drying vacuum degree is 0.01-10 Pa.
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| CN115057686A (en) * | 2022-06-29 | 2022-09-16 | 航天特种材料及工艺技术研究所 | High-strength high-temperature-resistant ceramic fiber elastomer heat-insulating material and preparation method and application thereof |
| CN115124363A (en) * | 2022-06-29 | 2022-09-30 | 航天特种材料及工艺技术研究所 | High-temperature-resistant ultra-light ceramic fiber porous elastomer material and preparation method and application thereof |
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