CN116375034A - Preparation method of silicon carbide@carbon core-shell structure whisker and heat conduction wave-absorbing patch and corresponding product - Google Patents
Preparation method of silicon carbide@carbon core-shell structure whisker and heat conduction wave-absorbing patch and corresponding product Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 264
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 257
- 239000011258 core-shell material Substances 0.000 title claims abstract description 182
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 107
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 171
- 239000006185 dispersion Substances 0.000 claims abstract description 96
- 239000007788 liquid Substances 0.000 claims abstract description 86
- 239000008103 glucose Substances 0.000 claims abstract description 85
- 239000000843 powder Substances 0.000 claims abstract description 74
- 239000000243 solution Substances 0.000 claims abstract description 71
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000011259 mixed solution Substances 0.000 claims abstract description 33
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 32
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 31
- 239000012298 atmosphere Substances 0.000 claims abstract description 19
- 230000001681 protective effect Effects 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 230000003213 activating effect Effects 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 21
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 239000002033 PVDF binder Substances 0.000 claims description 17
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 238000007781 pre-processing Methods 0.000 claims description 7
- 238000010129 solution processing Methods 0.000 claims description 7
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 18
- 239000008204 material by function Substances 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 239000000945 filler Substances 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 7
- 239000011358 absorbing material Substances 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 239000012767 functional filler Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- VIXKTJNMLDPTGJ-UHFFFAOYSA-M [Co]O Chemical compound [Co]O VIXKTJNMLDPTGJ-UHFFFAOYSA-M 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the technical field of functional materials, and provides a preparation method of silicon carbide@carbon core-shell structure whiskers and a heat conduction wave-absorbing patch and a corresponding product, wherein the preparation method of the silicon carbide@carbon core-shell structure whiskers comprises the following steps: preparing a glucose solution to pretreat silicon carbide whiskers, activating the pretreated glucose and silicon carbide whisker mixed solution by adopting a hydrochloric acid solution, placing the prepared silicon carbide whisker dispersion liquid into a hydrothermal synthesis reaction kettle to perform hydrothermal reaction, centrifugally washing the prepared silicon carbide@glucose core-shell whisker dispersion liquid by adopting deionized water, drying the centrifugally washed silicon carbide@glucose core-shell whisker dispersion liquid, and placing the prepared silicon carbide@glucose core-shell whisker powder into a protective atmosphere to perform high-temperature sintering treatment to obtain the silicon carbide@carbon core-shell structure whisker powder. According to the invention, through the preparation of the silicon carbide@carbon core-shell structure whisker, the heat conduction and wave absorption performance of the heat conduction wave absorption patch can be improved.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a preparation method of silicon carbide@carbon core-shell structure whiskers and a heat conduction wave-absorbing patch and a corresponding product.
Background
The development thinking of the heat-conducting wave-absorbing material is to add functional filler into the polymer matrix to enable the material to have heat-conducting or wave-absorbing functions. The wave absorbing material is usually added with wave absorbing agents such as ferrite, hydroxy nickel, hydroxy cobalt, barium titanate, graphite, carbon fiber and the like in a matrix, so that the wave absorbing material has wave absorbing performance, and the heat conductivity coefficients of the filler and the matrix in the wave absorbing material are low. In the heat conductive material, an insulating filler such as alumina, magnesia, aluminum nitride, boron nitride, etc. is usually added to the base material, and none of the fillers in the heat conductive material has a wave absorbing function. Therefore, when preparing a material having both heat conduction and wave absorption, it is necessary to mix and add a conventional heat conductive filler and a wave absorber into a base material.
However, in actual manufacturing, because the total addition amount of the functional filler in the matrix material such as rubber has an upper limit, the addition amount of one functional filler is necessarily increased to reduce the addition amount of another functional filler, so that the heat conducting property and the wave absorbing property of the heat conducting wave absorbing material are contradicted, and synchronous improvement of the heat conducting property and the wave absorbing property of the material is difficult to realize. At present, the heat conduction and wave absorption properties of the filler can only be balanced by coordinating the proportion of the two fillers, and the requirements of the electronic device on the material with high heat conduction property and strong electromagnetic wave absorption can not be met.
Therefore, how to provide a method for preparing a filler with heat conduction and wave absorption functions, and to prepare a high-performance heat conduction wave absorption material based on the prepared filler is a technical problem to be solved.
Disclosure of Invention
In view of the above, the invention mainly provides a preparation method of silicon carbide@carbon core-shell structure whiskers and a heat-conducting wave-absorbing patch and a corresponding product, aiming at overcoming the defects in the prior art.
In one aspect, the invention provides a method for preparing a silicon carbide@carbon core-shell structure whisker, which comprises the following steps:
step one, preparation of silicon carbide whisker dispersion liquid
Preparing a glucose solution, and preprocessing silicon carbide whiskers by adopting the prepared glucose solution to obtain a preprocessed glucose and silicon carbide whisker mixed solution;
activating the pretreated glucose and silicon carbide whisker mixed solution by adopting a hydrochloric acid solution to obtain a silicon carbide whisker dispersion liquid;
step two, preparing silicon carbide@glucose core-shell whisker dispersion liquid
Placing the silicon carbide whisker dispersion liquid prepared in the step one into a hydrothermal synthesis reaction kettle for hydrothermal reaction to obtain silicon carbide@glucose core-shell whisker dispersion liquid;
step three, preparation of silicon carbide@glucose core-shell whisker powder
Centrifugally washing the silicon carbide@glucose core-shell whisker dispersion liquid prepared in the second step by adopting deionized water, and drying the centrifugally washed silicon carbide@glucose core-shell whisker dispersion liquid to obtain silicon carbide@glucose core-shell whisker powder;
step four, preparing silicon carbide@carbon core-shell structure whisker powder
And (3) placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in a protective atmosphere for high-temperature sintering treatment to obtain the silicon carbide@carbon core-shell structure whisker powder.
In the first step, a glucose solution is prepared, and the prepared glucose solution is adopted to pretreat the silicon carbide whisker to obtain a pretreated glucose and silicon carbide whisker mixed solution, wherein the preparation method comprises the following steps: adding 0.594-1.782g of glucose into 50ml of deionized water, and stirring and mixing for 5-10min to obtain a uniformly mixed glucose solution; adding 0.3g of silicon carbide whisker into the glucose solution, and carrying out ultrasonic mixing for 15-30min to obtain the pretreated glucose and silicon carbide whisker mixed solution.
In the first step, hydrochloric acid solution is adopted to activate the pretreated glucose and silicon carbide whisker mixed solution to obtain silicon carbide whisker dispersion liquid, and the preparation method comprises the following steps: 5-7ml of 15% hydrochloric acid solution is added into the pretreated glucose and silicon carbide whisker mixed solution, and the pH value of the solution is adjusted to 3.0, so as to obtain silicon carbide whisker dispersion liquid.
In the second step, the temperature of the hydrothermal reaction is 150 ℃ and the time of the hydrothermal reaction is 20 hours.
In the third step, the centrifugally washed silicon carbide@glucose core-shell whisker dispersion liquid is dried to obtain silicon carbide@glucose core-shell whisker powder, which comprises the following steps: when the pH value of the washed silicon carbide@glucose core-shell whisker dispersion liquid reaches 7.0, the silicon carbide@glucose core-shell whisker dispersion liquid is dried for 12 hours at the temperature of 100 ℃ to obtain silicon carbide@glucose core-shell whisker powder.
In the fourth step, the silicon carbide@glucose core-shell whisker powder prepared in the third step is placed in a protective atmosphere for high-temperature sintering treatment, and the method comprises the following steps: and (3) placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in a protective atmosphere, heating to 1000 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 2 hours, cooling to 300 ℃ at a rate of 10 ℃/min, and naturally cooling to obtain the silicon carbide@carbon core-shell whisker powder.
In the fourth step, the protective atmosphere is argon atmosphere.
On the other hand, the invention provides a silicon carbide@carbon core-shell structure whisker, which is prepared by the method.
Furthermore, the invention also provides a preparation method of the heat conduction wave-absorbing patch based on the silicon carbide@carbon core-shell structure whisker, which comprises the following steps:
step one, preparation of polyvinylidene fluoride dispersion liquid
Adding 0.7-0.9g of polyvinylidene fluoride powder into 15ml of N, N-dimethylformamide solution, and magnetically stirring at 650rpm for 30min to obtain polyvinylidene fluoride dispersion;
step two, preparing silicon carbide@carbon core-shell structure whisker dispersion liquid
Adding 0.1-0.3g of silicon carbide@carbon core-shell structure whisker powder into 15ml of N, N-dimethylformamide solution, and carrying out ultrasonic mixing for 20min to obtain silicon carbide@carbon core-shell structure whisker dispersion liquid;
step three, preparation of heat conduction wave absorbing film based on silicon carbide@carbon core-shell structure whisker
Adding the silicon carbide@carbon core-shell structure whisker dispersion prepared in the second step into the polyvinylidene fluoride dispersion prepared in the first step according to the proportion of 1g of the total mass of the silicon carbide@carbon core-shell structure whisker powder and the polyvinylidene fluoride powder, magnetically stirring for 8 hours, and drying at 60 ℃ for 12 hours to obtain the heat-conducting wave-absorbing film based on the silicon carbide@carbon core-shell structure whisker;
step four, preparation of heat conduction wave absorbing patch based on silicon carbide@carbon core-shell structure whisker
And (3) performing hot press forming on the film prepared in the step (III) in a heat-conducting sheet forming die, wherein the temperature of the hot press forming is 200 ℃, the film is pressurized to 3MPa at a pressurizing rate of 0.1-0.2MPa/s, and the pressure is maintained for 20min, so that the heat-conducting wave-absorbing patch based on the silicon carbide@carbon core-shell structure whisker is obtained.
Finally, the invention also provides a heat-conducting wave-absorbing patch based on the silicon carbide@carbon core-shell structure whisker, which is prepared according to the preparation method of the heat-conducting wave-absorbing patch based on the silicon carbide@carbon core-shell structure whisker.
The invention has the following beneficial effects:
1. according to the preparation method, the silicon carbide whisker is activated by glucose pretreatment and hydrochloric acid solution, glucose is used as a carbon source, and the surface of the silicon carbide whisker is coated with glucose derived carbon with a heterostructure by a hydrothermal method and high-temperature sintering, so that the thickness of a carbon shell is 2-5nm. The pretreatment of the glucose can enable the glucose to be coated on the silicon carbide whisker more uniformly when the glucose is hydrothermal, the hydrochloric acid solution can remove impurity ions on the surface of the silicon carbide while being activated, so that the dispersibility of the glucose is improved, the glucose-derived carbon has high conductivity, the glucose-derived carbon is converted into heat energy when microwaves enter a sample, and the interface between the graphite carbon and the silicon carbide enhances the multi-scale scattering of the microwaves, so that the glucose-derived carbon has excellent electromagnetic wave absorption performance.
2. The film is pressed into a tablet by a hot pressing method, the film is pressurized to 3MPa at the temperature of 200 ℃ at the pressurizing rate of 0.1-0.2MPa/s, the pressure is maintained for 20min, and the film can be pressed into a flat patch. Under a certain pressurizing rate, bubbles between the filler and the matrix can be orderly discharged, gaps between the filler and the matrix are reduced, and higher density is obtained, so that a continuous heat conduction path is formed.
3. According to the invention, silicon carbide@carbon core-shell whisker is used as a filler, and polyvinylidene fluoride is used as a polymer matrix, and the length of the whisker is different, so that a heat conduction network is more easily built in the patch, and compared with other types of polymers, the whisker can be uniformly dispersed in polyvinylidene fluoride solution, and film formation is easier.
4. The mass ratio of glucose to silicon carbide whisker in the invention can reach 5.72GHz at the maximum effective absorption bandwidth (RL < -10 dB) under the conditions of 15wt% of filler ratio and thickness of 1.875mm, and the thermal conductivity is 0.422W/mk. It has an effective absorption bandwidth (RL < -10 dB) of 3.64GHz with a filler ratio of 30wt% and a thickness of 1.3mm, and a thermal conductivity of at most 0.673W/mk. The heat-conducting wave-absorbing patch prepared by the invention realizes excellent performance under a thinner thickness, so that the problems of slow heat dissipation and strong electromagnetic wave radiation of electronic devices can be solved in a very small space.
5. The preparation method is simple in preparation operation, convenient in equipment and capable of being popularized in industrialization.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an X-ray diffraction analysis chart of the silicon carbide @ carbon core-shell structure whiskers prepared in example 1, example 2, example 4 and example 5 of the present invention.
FIG. 2 is a scanning electron micrograph of a whisker having a silicon carbide @ carbon core-shell structure prepared in example 3 of the present invention.
Fig. 3 is a transmission electron microscope image of a silicon carbide @ carbon core-shell structured whisker prepared in example 3 of the present invention.
Fig. 4 is a transmission electron microscope image of a silicon carbide @ carbon core-shell structured whisker prepared in example 3 of the present invention.
Fig. 5 is a reflection loss diagram of a heat conduction wave absorption patch sample based on silicon carbide@carbon core-shell structure whiskers, which is prepared in example 6 of the present invention and is numbered a.
Fig. 6 is a reflection loss diagram of a sample of a heat conducting and wave absorbing patch based on silicon carbide @ carbon core-shell structure whiskers, prepared in example 6 of the present invention, with the number b.
Fig. 7 is a reflection loss diagram of a sample of a heat conducting and wave absorbing patch based on silicon carbide @ carbon core-shell structure whiskers, numbered c, prepared in example 6 of the present invention.
Fig. 8 is a graph of thermal conductivity coefficients of thermal conductive wave-absorbing patch samples based on silicon carbide @ carbon core-shell structure whiskers, prepared in example 6 of the present invention, numbered a, b, and c.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
It should be noted that, without conflict, the following embodiments and features in the embodiments may be combined with each other; and, based on the embodiments in this disclosure, all other embodiments that may be made by one of ordinary skill in the art without inventive effort are within the scope of the present disclosure.
It is noted that various aspects of the embodiments are described below within the scope of the following claims. It should be apparent that the aspects described herein may be embodied in a wide variety of forms and that any specific structure and/or function described herein is merely illustrative. Based on the present disclosure, one skilled in the art will appreciate that one aspect described herein may be implemented independently of any other aspect, and that two or more of these aspects may be combined in various ways. For example, an apparatus may be implemented and/or a method practiced using any number of the aspects set forth herein. In addition, such apparatus may be implemented and/or such methods practiced using other structure and/or functionality in addition to one or more of the aspects set forth herein.
Example 1
Preparation of silicon carbide@carbon core-shell structure whiskers:
step one, preparation of silicon carbide whisker dispersion liquid
Preparing a glucose solution, and preprocessing silicon carbide whiskers by adopting the prepared glucose solution to obtain a preprocessed glucose and silicon carbide whisker mixed solution; specifically, adding 0.594g of glucose into 50ml of deionized water, and stirring and mixing for 5min to obtain a uniformly mixed glucose solution; adding 0.3g of silicon carbide whisker into the glucose solution, and carrying out ultrasonic mixing for 15min to obtain a pretreated glucose and silicon carbide whisker mixed solution;
activating the pretreated glucose and silicon carbide whisker mixed solution by adopting a hydrochloric acid solution to obtain a silicon carbide whisker dispersion liquid; specifically, 5ml of 15% hydrochloric acid solution is added into the pretreated glucose and silicon carbide whisker mixed solution, and the pH value of the solution is adjusted to 3.0, so as to obtain silicon carbide whisker dispersion liquid;
step two, preparing silicon carbide@glucose core-shell whisker dispersion liquid
Placing the silicon carbide whisker dispersion liquid prepared in the step one into a hydrothermal synthesis reaction kettle for hydrothermal reaction to obtain silicon carbide@glucose core-shell whisker dispersion liquid; the temperature of the hydrothermal reaction is 150 ℃, and the time of the hydrothermal reaction is 20 hours;
step three, preparation of silicon carbide@glucose core-shell whisker powder
Centrifugally washing the silicon carbide@glucose core-shell whisker dispersion liquid prepared in the second step by adopting deionized water, and drying the centrifugally washed silicon carbide@glucose core-shell whisker dispersion liquid to obtain silicon carbide@glucose core-shell whisker powder; specifically, when the pH value of the washed silicon carbide@glucose core-shell whisker dispersion liquid reaches 7.0, drying the silicon carbide@glucose core-shell whisker dispersion liquid at the temperature of 100 ℃ for 12 hours to obtain silicon carbide@glucose core-shell whisker powder;
step four, preparing silicon carbide@carbon core-shell structure whisker powder
And (3) placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in a protective atmosphere for high-temperature sintering treatment to obtain the silicon carbide@carbon core-shell whisker powder, specifically, placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in an argon protective atmosphere, heating to 1000 ℃ at a heating rate of 5 ℃/min, preserving heat for 2 hours, cooling to 300 ℃ at a rate of 10 ℃/min, and naturally cooling to obtain the silicon carbide@carbon core-shell whisker powder.
Example 2
Preparation of silicon carbide@carbon core-shell structure whiskers:
step one, preparation of silicon carbide whisker dispersion liquid
Preparing a glucose solution, and preprocessing silicon carbide whiskers by adopting the prepared glucose solution to obtain a preprocessed glucose and silicon carbide whisker mixed solution; specifically, adding 0.732g of glucose into 50ml of deionized water, and stirring and mixing for 10min to obtain a uniformly mixed glucose solution; adding 0.3g of silicon carbide whisker into the glucose solution, and carrying out ultrasonic mixing for 20min to obtain a pretreated glucose and silicon carbide whisker mixed solution;
activating the pretreated glucose and silicon carbide whisker mixed solution by adopting a hydrochloric acid solution to obtain a silicon carbide whisker dispersion liquid; specifically, 5ml of 15% hydrochloric acid solution is added into the pretreated glucose and silicon carbide whisker mixed solution, and the pH value of the solution is adjusted to 3.0, so as to obtain silicon carbide whisker dispersion liquid;
step two, preparing silicon carbide@glucose core-shell whisker dispersion liquid
Placing the silicon carbide whisker dispersion liquid prepared in the step one into a hydrothermal synthesis reaction kettle for hydrothermal reaction to obtain silicon carbide@glucose core-shell whisker dispersion liquid; the temperature of the hydrothermal reaction is 150 ℃, and the time of the hydrothermal reaction is 20 hours;
step three, preparation of silicon carbide@glucose core-shell whisker powder
Centrifugally washing the silicon carbide@glucose core-shell whisker dispersion liquid prepared in the second step by adopting deionized water, and drying the centrifugally washed silicon carbide@glucose core-shell whisker dispersion liquid to obtain silicon carbide@glucose core-shell whisker powder; specifically, when the pH value of the washed silicon carbide@glucose core-shell whisker dispersion liquid reaches 7.0, drying the silicon carbide@glucose core-shell whisker dispersion liquid at the temperature of 100 ℃ for 12 hours to obtain silicon carbide@glucose core-shell whisker powder;
step four, preparing silicon carbide@carbon core-shell structure whisker powder
And (3) placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in a protective atmosphere for high-temperature sintering treatment to obtain the silicon carbide@carbon core-shell whisker powder, specifically, placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in an argon protective atmosphere, heating to 1000 ℃ at a heating rate of 8 ℃/min, preserving heat for 2 hours, cooling to 300 ℃ at a rate of 10 ℃/min, and naturally cooling to obtain the silicon carbide@carbon core-shell whisker powder.
Example 3
Preparation of silicon carbide@carbon core-shell structure whiskers:
step one, preparation of silicon carbide whisker dispersion liquid
Preparing a glucose solution, and preprocessing silicon carbide whiskers by adopting the prepared glucose solution to obtain a preprocessed glucose and silicon carbide whisker mixed solution; specifically, adding 0.809g of glucose into 50ml of deionized water, and stirring and mixing for 10min to obtain a uniformly mixed glucose solution; adding 0.3g of silicon carbide whisker into the glucose solution, and carrying out ultrasonic mixing for 30min to obtain a pretreated glucose and silicon carbide whisker mixed solution;
activating the pretreated glucose and silicon carbide whisker mixed solution by adopting a hydrochloric acid solution to obtain a silicon carbide whisker dispersion liquid; specifically, adding 6ml of 15% hydrochloric acid solution into the pretreated glucose and silicon carbide whisker mixed solution, and adjusting the pH value of the solution to 3.0 to obtain silicon carbide whisker dispersion liquid;
step two, preparing silicon carbide@glucose core-shell whisker dispersion liquid
Placing the silicon carbide whisker dispersion liquid prepared in the step one into a hydrothermal synthesis reaction kettle for hydrothermal reaction to obtain silicon carbide@glucose core-shell whisker dispersion liquid; the temperature of the hydrothermal reaction is 150 ℃, and the time of the hydrothermal reaction is 20 hours;
step three, preparation of silicon carbide@glucose core-shell whisker powder
Centrifugally washing the silicon carbide@glucose core-shell whisker dispersion liquid prepared in the second step by adopting deionized water, and drying the centrifugally washed silicon carbide@glucose core-shell whisker dispersion liquid to obtain silicon carbide@glucose core-shell whisker powder; specifically, when the pH value of the washed silicon carbide@glucose core-shell whisker dispersion liquid reaches 7.0, drying the silicon carbide@glucose core-shell whisker dispersion liquid at the temperature of 100 ℃ for 12 hours to obtain silicon carbide@glucose core-shell whisker powder;
step four, preparing silicon carbide@carbon core-shell structure whisker powder
And (3) placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in a protective atmosphere for high-temperature sintering treatment to obtain the silicon carbide@carbon core-shell whisker powder, specifically, placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in an argon protective atmosphere, heating to 1000 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, cooling to 300 ℃ at a rate of 10 ℃/min, and naturally cooling to obtain the silicon carbide@carbon core-shell whisker powder.
Example 4
Preparation of silicon carbide@carbon core-shell structure whiskers:
step one, preparation of silicon carbide whisker dispersion liquid
Preparing a glucose solution, and preprocessing silicon carbide whiskers by adopting the prepared glucose solution to obtain a preprocessed glucose and silicon carbide whisker mixed solution; specifically, 1.436g of glucose is added into 50ml of deionized water, and the mixture is stirred and mixed for 10min to obtain a uniformly mixed glucose solution; adding 0.3g of silicon carbide whisker into the glucose solution, and carrying out ultrasonic mixing for 30min to obtain a pretreated glucose and silicon carbide whisker mixed solution;
activating the pretreated glucose and silicon carbide whisker mixed solution by adopting a hydrochloric acid solution to obtain a silicon carbide whisker dispersion liquid; specifically, 7ml of 15% hydrochloric acid solution is added into the pretreated glucose and silicon carbide whisker mixed solution, and the pH value of the solution is adjusted to 3.0, so as to obtain silicon carbide whisker dispersion liquid;
step two, preparing silicon carbide@glucose core-shell whisker dispersion liquid
Placing the silicon carbide whisker dispersion liquid prepared in the step one into a hydrothermal synthesis reaction kettle for hydrothermal reaction to obtain silicon carbide@glucose core-shell whisker dispersion liquid; the temperature of the hydrothermal reaction is 150 ℃, and the time of the hydrothermal reaction is 20 hours;
step three, preparation of silicon carbide@glucose core-shell whisker powder
Centrifugally washing the silicon carbide@glucose core-shell whisker dispersion liquid prepared in the second step by adopting deionized water, and drying the centrifugally washed silicon carbide@glucose core-shell whisker dispersion liquid to obtain silicon carbide@glucose core-shell whisker powder; specifically, when the pH value of the washed silicon carbide@glucose core-shell whisker dispersion liquid reaches 7.0, drying the silicon carbide@glucose core-shell whisker dispersion liquid at the temperature of 100 ℃ for 12 hours to obtain silicon carbide@glucose core-shell whisker powder;
step four, preparing silicon carbide@carbon core-shell structure whisker powder
And (3) placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in a protective atmosphere for high-temperature sintering treatment to obtain the silicon carbide@carbon core-shell whisker powder, specifically, placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in an argon protective atmosphere, heating to 1000 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, cooling to 300 ℃ at a rate of 10 ℃/min, and naturally cooling to obtain the silicon carbide@carbon core-shell whisker powder.
Example 5
Preparation of silicon carbide@carbon core-shell structure whiskers:
step one, preparation of silicon carbide whisker dispersion liquid
Preparing a glucose solution, and preprocessing silicon carbide whiskers by adopting the prepared glucose solution to obtain a preprocessed glucose and silicon carbide whisker mixed solution; specifically, adding 1.782g of glucose into 50ml of deionized water, and stirring and mixing for 10min to obtain a uniformly mixed glucose solution; adding 0.3g of silicon carbide whisker into the glucose solution, and carrying out ultrasonic mixing for 30min to obtain a pretreated glucose and silicon carbide whisker mixed solution;
activating the pretreated glucose and silicon carbide whisker mixed solution by adopting a hydrochloric acid solution to obtain a silicon carbide whisker dispersion liquid; specifically, 7ml of 15% hydrochloric acid solution is added into the pretreated glucose and silicon carbide whisker mixed solution, and the pH value of the solution is adjusted to 3.0, so as to obtain silicon carbide whisker dispersion liquid;
step two, preparing silicon carbide@glucose core-shell whisker dispersion liquid
Placing the silicon carbide whisker dispersion liquid prepared in the step one into a hydrothermal synthesis reaction kettle for hydrothermal reaction to obtain silicon carbide@glucose core-shell whisker dispersion liquid; the temperature of the hydrothermal reaction is 150 ℃, and the time of the hydrothermal reaction is 20 hours;
step three, preparation of silicon carbide@glucose core-shell whisker powder
Centrifugally washing the silicon carbide@glucose core-shell whisker dispersion liquid prepared in the second step by adopting deionized water, and drying the centrifugally washed silicon carbide@glucose core-shell whisker dispersion liquid to obtain silicon carbide@glucose core-shell whisker powder; specifically, when the pH value of the washed silicon carbide@glucose core-shell whisker dispersion liquid reaches 7.0, drying the silicon carbide@glucose core-shell whisker dispersion liquid at the temperature of 100 ℃ for 12 hours to obtain silicon carbide@glucose core-shell whisker powder;
step four, preparing silicon carbide@carbon core-shell structure whisker powder
And (3) placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in a protective atmosphere for high-temperature sintering treatment to obtain the silicon carbide@carbon core-shell whisker powder, specifically, placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in an argon protective atmosphere, heating to 1000 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, cooling to 300 ℃ at a rate of 10 ℃/min, and naturally cooling to obtain the silicon carbide@carbon core-shell whisker powder.
Example 6
Preparation of a heat conduction wave-absorbing patch based on silicon carbide@carbon core-shell structure whiskers:
step one, preparation of polyvinylidene fluoride dispersion liquid
Adding 0.7-0.9g of polyvinylidene fluoride powder into 15ml of N, N-dimethylformamide solution, and magnetically stirring at 650rpm for 30min to obtain polyvinylidene fluoride dispersion;
step two, preparing silicon carbide@carbon core-shell structure whisker dispersion liquid
Adding 0.1-0.3g of silicon carbide@carbon core-shell structure whisker powder prepared in example 3 into 15ml of N, N-dimethylformamide solution, and carrying out ultrasonic mixing for 20min to obtain silicon carbide@carbon core-shell structure whisker dispersion liquid;
step three, preparation of heat conduction wave absorbing film based on silicon carbide@carbon core-shell structure whisker
Adding the silicon carbide@carbon core-shell structure whisker dispersion prepared in the second step into the polyvinylidene fluoride dispersion prepared in the first step according to the proportion of 1g of the total mass of the silicon carbide@carbon core-shell structure whisker powder and the polyvinylidene fluoride powder, magnetically stirring for 8 hours, and drying at 60 ℃ for 12 hours to obtain the heat-conducting wave-absorbing film based on the silicon carbide@carbon core-shell structure whisker;
step four, preparation of heat conduction wave absorbing patch based on silicon carbide@carbon core-shell structure whisker
And (3) performing hot press forming on the film prepared in the step (III) in a heat-conducting sheet forming die, wherein the hot press forming temperature is 200 ℃, the film is pressurized to 3MPa at a pressurizing rate of 0.1-0.2MPa/s, and the pressure is maintained for 20min, so that three heat-conducting wave-absorbing patch samples based on silicon carbide@carbon core-shell structure whiskers with the numbers of a, b and c are obtained. The specific process parameter settings for the samples numbered a, b, c are shown in table 1.
TABLE 1
Example 7
The phase composition of the silicon carbide @ carbon core-shell structure whiskers prepared in example 1, example 2, example 4 and example 5 was analyzed by means of an X-ray diffractometer (XRD) with model X' Pert PRO MPD; the powdered sample is poured into a slide well (1.5X 1.5 cm), preferably just filling the well, and then placed into an X-ray diffractometer. The radiation source is Cu K alpha (lambda= 0.15406 nm), the scanning range is 10-90 degrees, the scanning speed is 5 degrees/min, the tube voltage is 20-60kV, the tube current is 10-300mA, and the test result is shown in figure 1.
As shown in fig. 1, six characteristic peaks at 34.1 °, 35.7 °, 41.5 °, 60.1 °, 71.9 °, 75.6 ° respectively exist in XRD patterns of the silicon carbide @ carbon core-shell structure whiskers prepared in example 1, example 2, example 4, and example 5, respectively, corresponding to (101), (102), (104), (110), (116), and (0 1 12) crystal faces of β -SiC crystals, respectively, the increase of glucose does not shift the diffraction peak of SiC, and the figure has no diffraction peak of carbon shell because of the small carbon content in the sample.
Observing the microstructure of the silicon carbide@carbon core-shell structure whisker prepared in example 3 by using a cold field emission Scanning Electron Microscope (SEM) with the model of Hitachi, SU 8020; taking 0.1g of powdery sample, adding 2ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 20min to obtain a solution system with uniform dispersion, then dripping the solution on a silicon wafer, naturally air-drying, sticking the silicon wafer on a sample table by using conductive adhesive, and observing by using an instrument, wherein the accelerating voltage is 5kV or 15kV. The microstructure of the silicon carbide @ carbon core-shell structured whisker prepared in example 3 is shown in fig. 2.
As shown in FIG. 2, the length of the silicon carbide whisker of the silicon carbide@carbon core-shell structure whisker prepared in the embodiment 3 is not more than 3.5 μm, the diameter is 0.26-0.45 μm, and the length and the diameter are different, so that the silicon carbide whisker can more effectively construct a heat conduction and intercommunication network.
Observing the microstructure of the silicon carbide@carbon core-shell structure whisker prepared in the example 3 by adopting a field emission transmission electron microscope with the model JEM-2100F; taking 0.1g of powdery sample, adding 2ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 20min to obtain a uniformly dispersed solution system, then dripping the solution system on a copper foil, placing the copper foil on a sample table, and observing by using an instrument, wherein the test result is shown in figures 3 and 4.
As shown in fig. 3, the graphite carbon shell on the whisker surface of the silicon carbide @ carbon core-shell structure prepared in the embodiment 3 is uniformly coated, and the structure is reasonable.
As shown in FIG. 4, the thickness of the graphite carbon shell on the surface of the silicon carbide@carbon core-shell structure whisker prepared in example 3 is 2-5nm.
The reflection loss performance of the sample a, sample b and sample c prepared in example 6 was tested by using a vector network analyzer of model Agilent Technologies N5247A; the specimen sample is clamped between test fixtures for measurement. The testing method is a coaxial method, the tested wave band is a 2-18GHz wave band, the number of scanning points is 401 points, and the testing results of the sample a, the sample b and the sample c are respectively shown in fig. 5, fig. 6 and fig. 7.
As shown in FIG. 5, the reflection loss test was performed on the sample pressed by sample a in example 6 by a vector network analyzer, so that the wave absorbing properties of the sample at different thicknesses (401 thicknesses are taken at intervals of 0-10mm by 0.025 mm) were obtained, and the minimum reflection loss RL at 12.84GHZ was found to be 2.85mm min At-21.5 dB, its effective absorption bandwidth (RL) is 3.15mm thick<-10 dB) at 5.28GHz (effective absorption bandwidth frequency range: 9.36-14.64 GHz).
As shown in FIG. 6, the sample pressed by sample b in example 6 was reflected by a vector network analyzerThe loss test can obtain the wave absorption performance of the sample under different thicknesses (the interval of 0-10mm is 0.025mm, and 401 thicknesses are taken), and the minimum reflection loss RL at 15.4GHZ is the minimum reflection loss RL when the thickness is 1.575mm min Is-46.0 dB, its effective absorption bandwidth (RL<-10 dB) at 5.72GHz (effective absorption bandwidth frequency range: 12.2-17.92 GHz).
As shown in FIG. 7, the reflection loss test was performed on the sample pressed by sample c in example 6 by a vector network analyzer, and the wave absorbing properties of the sample at different thicknesses (401 thicknesses are taken at 0-10mm intervals of 0.025 mm) were obtained, and the minimum reflection loss RL at 15.4GHZ was found to be 1.175mm min Is-12.3 dB, and has an effective absorption bandwidth (RL<-10 dB) at 3.64GHz (effective absorption bandwidth frequency range: 14.24-17.88 GHz).
The thermal conductivities of sample a, sample b and sample c in example 6 were tested using a laser thermal conductivity meter model LFA 457; the test was performed at 25℃using normal temperature detection, with the specific heat standard being the copper, and the test results were shown in FIG. 8.
As shown in FIG. 8, in the thermal conductivity images of sample a, sample b and sample c in example 6, the thermal conductivities of sample a and sample b were 0.369W/mk and 0.422W/mk, respectively, and the thermal conductivity of sample c was the highest, which was 0.673W/mk.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be included in the present invention. Therefore, the protection scope of the invention is subject to the protection scope of the claims.
Claims (10)
1. The preparation method of the silicon carbide@carbon core-shell structure whisker is characterized by comprising the following steps of:
step one, preparation of silicon carbide whisker dispersion liquid
Preparing a glucose solution, and preprocessing silicon carbide whiskers by adopting the prepared glucose solution to obtain a preprocessed glucose and silicon carbide whisker mixed solution;
activating the pretreated glucose and silicon carbide whisker mixed solution by adopting a hydrochloric acid solution to obtain a silicon carbide whisker dispersion liquid;
step two, preparing silicon carbide@glucose core-shell whisker dispersion liquid
Placing the silicon carbide whisker dispersion liquid prepared in the step one into a hydrothermal synthesis reaction kettle for hydrothermal reaction to obtain silicon carbide@glucose core-shell whisker dispersion liquid;
step three, preparation of silicon carbide@glucose core-shell whisker powder
Centrifugally washing the silicon carbide@glucose core-shell whisker dispersion liquid prepared in the second step by adopting deionized water, and drying the centrifugally washed silicon carbide@glucose core-shell whisker dispersion liquid to obtain silicon carbide@glucose core-shell whisker powder;
step four, preparing silicon carbide@carbon core-shell structure whisker powder
And (3) placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in a protective atmosphere for high-temperature sintering treatment to obtain the silicon carbide@carbon core-shell structure whisker powder.
2. The method for preparing silicon carbide@carbon core-shell structure whiskers according to claim 1, wherein in the first step, a glucose solution is prepared, the prepared glucose solution is adopted to pretreat the silicon carbide whiskers, and a pretreated glucose/silicon carbide whisker mixed solution is obtained, and the method comprises the following steps: adding 0.594-1.782g of glucose into 50ml of deionized water, and stirring and mixing for 5-10min to obtain a uniformly mixed glucose solution; adding 0.3g of silicon carbide whisker into the glucose solution, and carrying out ultrasonic mixing for 15-30min to obtain the pretreated glucose and silicon carbide whisker mixed solution.
3. The method for preparing silicon carbide@carbon core-shell structure whiskers according to claim 1, wherein in the first step, a hydrochloric acid solution is adopted to perform activation treatment on a pretreated glucose and silicon carbide whisker mixed solution to obtain a silicon carbide whisker dispersion liquid, and the method comprises the following steps: 5-7ml of hydrochloric acid solution with the volume fraction of 15% is added into the pretreated glucose and silicon carbide whisker mixed solution, and the pH value of the solution is adjusted to 3.0, so that the silicon carbide whisker dispersion liquid is obtained.
4. The method for preparing silicon carbide@carbon core-shell structure whiskers according to claim 1, wherein in the second step, the temperature of the hydrothermal reaction is 150 ℃, and the time of the hydrothermal reaction is 20 hours.
5. The method for preparing silicon carbide@carbon core-shell structure whiskers according to claim 1, wherein in the third step, drying the centrifugally washed silicon carbide@glucose core-shell whisker dispersion liquid to obtain silicon carbide@glucose core-shell whisker powder, the method comprises the following steps: when the pH value of the washed silicon carbide@glucose core-shell whisker dispersion liquid reaches 7.0, the silicon carbide@glucose core-shell whisker dispersion liquid is dried for 12 hours at the temperature of 100 ℃ to obtain silicon carbide@glucose core-shell whisker powder.
6. The method for preparing the silicon carbide@carbon core-shell structure whisker according to claim 1, wherein in the fourth step, the silicon carbide@glucose core-shell whisker powder prepared in the third step is placed in a protective atmosphere for high-temperature sintering treatment, and the method comprises the following steps: and (3) placing the silicon carbide@glucose core-shell whisker powder prepared in the step (III) in a protective atmosphere, heating to 1000 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 2 hours, cooling to 300 ℃ at a rate of 10 ℃/min, and naturally cooling to obtain the silicon carbide@carbon core-shell whisker powder.
7. The method for preparing silicon carbide@carbon core-shell structure whiskers according to claim 1, wherein in the fourth step, the protective atmosphere is an argon atmosphere.
8. A silicon carbide @ carbon core-shell structure whisker, wherein the silicon carbide @ carbon core-shell structure whisker is produced according to the method of any one of claims 1 to 7.
9. The preparation method of the heat conduction wave-absorbing patch based on the silicon carbide@carbon core-shell structure whisker is characterized by comprising the following steps of:
step one, preparation of polyvinylidene fluoride dispersion liquid
Adding 0.7-0.9g of polyvinylidene fluoride powder into 15ml of N, N-dimethylformamide solution, and magnetically stirring at 650rpm for 30min to obtain polyvinylidene fluoride dispersion;
step two, preparing silicon carbide@carbon core-shell structure whisker dispersion liquid
Adding 0.1-0.3g of silicon carbide@carbon core-shell structure whisker powder into 15ml of N, N-dimethylformamide solution, and carrying out ultrasonic mixing for 20min to obtain silicon carbide@carbon core-shell structure whisker dispersion liquid;
step three, preparation of heat conduction wave absorbing film based on silicon carbide@carbon core-shell structure whisker
Adding the silicon carbide@carbon core-shell structure whisker dispersion prepared in the second step into the polyvinylidene fluoride dispersion prepared in the first step according to the proportion of 1g of the total mass of the silicon carbide@carbon core-shell structure whisker powder and the polyvinylidene fluoride powder, magnetically stirring for 8 hours, and drying at 60 ℃ for 12 hours to obtain the heat-conducting wave-absorbing film based on the silicon carbide@carbon core-shell structure whisker;
step four, preparation of heat conduction wave absorbing patch based on silicon carbide@carbon core-shell structure whisker
And (3) performing hot press forming on the film prepared in the step (III) in a heat-conducting sheet forming die, wherein the temperature of the hot press forming is 200 ℃, the film is pressurized to 3MPa at a pressurizing rate of 0.1-0.2MPa/s, and the pressure is maintained for 20min, so that the heat-conducting wave-absorbing patch based on the silicon carbide@carbon core-shell structure whisker is obtained.
10. A thermally conductive wave-absorbing patch based on silicon carbide @ carbon core-shell structure whiskers, characterized in that the thermally conductive wave-absorbing patch based on silicon carbide @ carbon core-shell structure whiskers is produced according to the method of claim 9.
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