CN113754454A - Preparation method and application of carbon fiber/silicon carbide directional porous framework - Google Patents
Preparation method and application of carbon fiber/silicon carbide directional porous framework Download PDFInfo
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- CN113754454A CN113754454A CN202111125847.9A CN202111125847A CN113754454A CN 113754454 A CN113754454 A CN 113754454A CN 202111125847 A CN202111125847 A CN 202111125847A CN 113754454 A CN113754454 A CN 113754454A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 73
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 73
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 68
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000013354 porous framework Substances 0.000 title abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000010703 silicon Substances 0.000 claims abstract description 45
- 238000007710 freezing Methods 0.000 claims abstract description 43
- 230000008014 freezing Effects 0.000 claims abstract description 43
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 42
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002131 composite material Substances 0.000 claims abstract description 26
- 239000011230 binding agent Substances 0.000 claims abstract description 22
- 238000005338 heat storage Methods 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000006722 reduction reaction Methods 0.000 claims abstract description 18
- 239000000945 filler Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000011232 storage material Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 38
- 239000002002 slurry Substances 0.000 claims description 36
- 239000000843 powder Substances 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- 230000009467 reduction Effects 0.000 claims description 13
- 239000012300 argon atmosphere Substances 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
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- 230000001070 adhesive effect Effects 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229920001661 Chitosan Polymers 0.000 claims description 2
- 239000002033 PVDF binder Substances 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 239000004809 Teflon Substances 0.000 claims description 2
- 229920006362 Teflon® Polymers 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000011268 mixed slurry Substances 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
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- 235000019698 starch Nutrition 0.000 claims description 2
- 238000009777 vacuum freeze-drying Methods 0.000 abstract description 9
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 30
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- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 16
- 239000012188 paraffin wax Substances 0.000 description 16
- 239000002245 particle Substances 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000004108 freeze drying Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- 239000011812 mixed powder Substances 0.000 description 8
- 239000011863 silicon-based powder Substances 0.000 description 8
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- 239000012520 frozen sample Substances 0.000 description 7
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- 229910052681 coesite Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- SICLLPHPVFCNTJ-UHFFFAOYSA-N 1,1,1',1'-tetramethyl-3,3'-spirobi[2h-indene]-5,5'-diol Chemical compound C12=CC(O)=CC=C2C(C)(C)CC11C2=CC(O)=CC=C2C(C)(C)C1 SICLLPHPVFCNTJ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
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- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229940057995 liquid paraffin Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- -1 silicon carbide compound Chemical class 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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Abstract
The invention discloses a preparation method and application of a carbon fiber/silicon carbide composite porous skeleton with directional heat conduction characteristics, and relates to the following steps: firstly, silicon and silicon dioxide powder raw materials are uniformly mixed, then the silicon source mixture and carbon fiber raw materials are uniformly dispersed in a binder solution, and a three-dimensional skeleton blank with an oriented porous structure is obtained through pre-freezing, freezing and forming and vacuum freeze drying treatment. And finally, carrying out high-temperature calcination treatment in an inert atmosphere, and utilizing carbothermic reduction reaction to generate silicon carbide to prepare the carbon fiber/silicon carbide composite porous skeleton with the directional heat conduction characteristic. The prepared composite porous framework body can be used as a heat-conducting filler to be applied to a phase-change heat storage material and a thermal interface material, so that the heat conductivity coefficient of the composite is improved, and the composite porous framework body has the characteristic of oriented heat conduction. The invention has simple preparation process, low cost and wide application.
Description
Technical Field
The invention relates to the field of phase change heat storage and electronic equipment heat management, in particular to a preparation method and application of a carbon fiber/silicon carbide directional porous heat conducting framework.
Background
The utilization efficiency of fossil energy is improved and carbon emission is reduced by realizing one of main ways of carbon emission reduction and carbon neutralization. The fossil energy is used to convert heat energy into energy in other forms by combustion, and in a power plant, the fossil energy releases heat by combustion to convert heat energy into electric energy as a final product. However, the amount of electricity used is not always matched with the amount of electricity generated, which results in waste of electric energy, but the cost of storing electric energy is too high, so that it is very urgent to find an economical and efficient way for storing thermal energy.
At present, the heat storage modes mainly comprise chemical reaction heat storage, sensible heat storage and latent heat storage. Although the heat storage density is high by utilizing the chemical reaction heat storage, the large-scale application of the heat storage is limited by the defects of complex reaction process and equipment, high technical difficulty, high cost and the like. Sensible heat storage is to store heat by the heat capacity of a sensible material, store and release heat as the temperature increases and decreases, but the storage density is low. Compared with sensible heat materials, latent heat materials have the advantages of high heat storage density, larger heat storage capacity and stable heat storage and release platforms when phase change occurs, but the problems of easy leakage, low heat storage and release speed and the like when the phase change occurs. Therefore, the filler with the leakage-proof and high-heat-conduction material is extremely important to find, and is compounded with the phase-change heat storage base body, so that the problems of low heat storage and release speed and leakage of the phase-change material can be effectively solved, and the filler is widely applied to the fields of waste heat recovery, heat management and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon fiber/silicon carbide composite porous skeleton with a directional heat conduction structure.
The invention also aims to provide the carbon fiber/silicon carbide composite porous skeleton composite phase change heat storage material with the oriented heat conduction structure prepared by the method.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a carbon fiber/silicon carbide composite heat conducting framework with a directional heat conducting structure comprises the following steps:
(1) uniformly mixing powder raw materials of silicon and silicon dioxide according to a certain proportion to prepare a silicon source mixture, and then dispersing the mixture and a carbon fiber raw material in a binder solution with a certain concentration according to a certain proportion to prepare uniformly mixed slurry; then pouring the slurry into a Teflon die with a copper bar at the bottom, and carrying out two-stage freezing treatment, namely 1) pre-freezing in a freezing chamber at the temperature of-30-0 ℃ for 10-25 min, and reducing the temperature of the slurry; 2) the bottom of the copper bar of the mould is placed in a cold trap at the temperature of-196 to-50 ℃ for freezing for 20min to 6 h; 3) and finally drying the mixture in a vacuum freeze dryer for 12-60 hours.
(2) Placing the dried sample obtained in the step (1) in an argon atmosphere to carry out the following two-stage sintering treatment: 1) Firstly, carrying out presintering treatment at a lower temperature to carbonize a binder; 2) and then, continuously carrying out high-temperature heat treatment under the argon atmosphere, generating silicon carbide by utilizing a carbothermic reduction reaction, and cooling to room temperature to obtain the carbon fiber/silicon carbide composite porous skeleton with the directional heat conduction characteristic. The reaction principle of carbothermic reduction to produce silicon carbide is as follows:
Si(s)+SiO2(s)＝2SiO(g) (1)
3SiO(g)+3C(s)＝2SiC(s)+SiO2(l)+CO(g) (2)
3SiO(g)+CO(g)＝SiC(s)+2SiO2(l) (3)
Si(s)+C(s)＝SiC(s) (4)
preferably, the molar ratio of the silicon to the silicon dioxide powder raw material in the step (1) is 1-2.
Preferably, the carbon/silicon molar ratio of the carbon fiber and the silicon source in the step (1) is 1-10.
Preferably, the binder in step (1) is selected from one or more of polyvinyl alcohol, polyethylene glycol, polyacrylic acid, sodium carboxymethyl cellulose, starch, polymethyl methacrylate, polyvinylidene fluoride and chitosan; the adhesive is prepared by dissolving the adhesive in a corresponding solvent, and the solution concentration of the adhesive is 0.5-5 wt%.
Preferably, the pretreatment temperature in the step (2) is 300-800 ℃, and the treatment time is 1-3 h; the carbothermic reduction temperature is 1200-1800 ℃, and the treatment time is 1-10 h.
On the other hand, the invention also provides application of the carbon fiber/silicon carbide composite heat-conducting framework with the oriented heat-conducting structure prepared by the method in improving the performance of the phase-change heat-storage material as a heat-conducting filler.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention utilizes the directional ice template method, can easily obtain a porous skeleton blank with a directional structure by controlling the growth direction of ice crystals during freezing, and then generates silicon carbide with high heat conductivity by using a carbothermic reduction reaction, thereby obtaining the excellent heat-conducting network structure of the silicon carbide crosslinked carbon fiber. Compared with the method of directly utilizing the heat-conducting powder filler, the porous framework body with the oriented structure can effectively improve the heat conductivity of the composite in a certain direction (vertical direction/horizontal direction), and can be used as a good high-heat-conducting filler framework to be applied to industries such as phase-change heat storage and thermal interface materials.
2. The preparation method is simple and convenient, the process cost is low, the obtained carbon fiber/silicon carbide and phase-change material composite has excellent thermal response speed and leakage prevention capability, and the industrial mass production is easy.
Drawings
FIG. 1(a) is a side view of a sample of the oriented structure of silicon source and carbon fiber obtained after freeze-drying in example 1; FIG. 1(b) is a side view of a carbon fiber/silicon carbide composite thermal conductive skeleton with a directional thermal conductive structure, which is obtained after carbothermic reduction in example 1; FIG. 1(c) is a diagram of a sample of the paraffin phase change material-carbon fiber/silicon carbide composite prepared in example 1; FIG. 1(d) is a graph of a blank sample of paraffin wax prepared in example 1.
FIG. 2 is a graph showing the shape change of the paraffin phase change material-carbon fiber/silicon carbide composite and the paraffin blank sample when heated at 80 ℃ in example 1. (a) Paraffin blank sample, and (b) paraffin-carbon fiber/silicon carbide composite.
Fig. 3 is an SEM image of a carbon fiber/silicon carbide sample with directional thermal conductivity characteristics prepared in example 2.
Fig. 4 is an XRD pattern of a sample of the carbon fiber/silicon carbide structure with directional thermal conductivity characteristics prepared in example 2.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The invention is described in further detail below with reference to the figures and specific embodiments.
Example 1:
1. preparation of carbon fiber/silicon carbide porous skeleton body
(1) Preparing slurry: weighing 6g of silicon dioxide powder with the particle size of 500nm and 3.085g of silicon powder (the molar ratio of silicon to silicon dioxide is 1.1), uniformly mixing, drying and grinding for later use. A 1 wt% strength aqueous solution of CMC (0.101 g by mass of CMC binder, 10g by mass of deionized water) was prepared. 1.147g of the mixed powder and 0.636g of carbon fiber powder with the particle size of 13 mu m are added into the adhesive solution to be stirred and mixed (wherein the silicon source and the carbon fiber powder account for 15 wt% of the slurry, and the molar ratio of carbon to silicon is 2), and the slurry is prepared after bubbles are removed.
(2) Freezing and freeze-drying: pouring the slurry into a special mold, removing air bubbles, and pre-freezing the mold in a freezing chamber at-20 deg.C for 15 min. Then freezing in a cold trap at-65 deg.C for 3h, and finally vacuum freeze-drying on a drying rack for 24h to obtain a sample of the oriented silicon source and carbon fiber mixture, which is shown in FIG. 1 (a).
(3) And (3) heat treatment: carrying out two-stage heat treatment on the sample prepared in the step (2) in an argon atmosphere: pre-burning at 300 ℃ for 1h, then heating to 1500 ℃ for carbothermic reduction heat treatment for 2h, and naturally cooling to room temperature to obtain the carbon fiber/silicon carbide porous skeleton, wherein the substance is shown in figure 1 (b).
2. Preparation and leakage-proof experiment of paraffin phase-change material and carbon fiber/silicon carbide compound
60g of paraffin was put in a beaker and heated to 80 ℃ to completely dissolve the paraffin. And secondly, immersing the carbon fiber/silicon carbide porous skeleton filler into liquid paraffin to completely immerse the carbon fiber/silicon carbide porous skeleton filler into the paraffin, then keeping the constant temperature of 70 ℃ for 4 hours in a vacuum device, fishing out a sample, and cooling to the room temperature to obtain the paraffin-carbon fiber/silicon carbide composite. The sample object diagram is shown in FIG. 1 (c); FIG. 1(d) is a block pure paraffin comparative sample.
The paraffin complex (paraffin accounts for 80 wt%) and the pure paraffin sample are placed in a heating box at a constant temperature of 80 ℃, and then the change of the shape of the sample during heating is recorded by a digital camera every 10 min. Fig. 2 is a real diagram of two samples before and after heating, after heating at 80 ℃ for 50 minutes, pure paraffin samples are completely melted into liquid and spread on the whole container, the compound of paraffin and porous filler can keep an integral shape, and melted paraffin is absorbed in a porous structure without leakage.
Example 2:
1. preparation of carbon fiber/silicon carbide skeleton structure
(1) Preparing slurry: weighing 6g of silicon dioxide powder with the particle size of 500nm and 5.61g of silicon powder (the molar ratio of silicon to silicon dioxide is 2), uniformly mixing, drying and grinding for later use. Preparing 1.5 wt% CMC solution (the mass of the CMC binder is 0.152g, the mass of the deionized water is 10g), taking 1.106 g of the mixed powder and 0.685g of carbon fiber powder with the particle size of 13 mu m, adding the powder and the carbon fiber powder into the binder solution, stirring and mixing (wherein the silicon source and the carbon fiber powder account for 15 wt% of the slurry, and the molar ratio of carbon to silicon is 2), and removing bubbles to finish the preparation of the slurry.
(2) Freezing and freeze drying, pouring the slurry into a special mold, removing air bubbles, and pre-freezing the mold in a freezing chamber at-20 deg.C for 15 min. Then placing the pre-frozen sample in a cold trap at the temperature of-65 ℃ for freezing for 3h, and finally carrying out vacuum freeze drying on a drying rack for 24h to obtain a sample of the oriented silicon source and carbon fiber mixture
(3) And (3) heat treatment: the sample is subjected to two-stage heat treatment under argon atmosphere: and (3) presintering at 300 ℃ for 1h, then heating to 1550 ℃ for carbothermic reduction heat treatment for 2h, and naturally cooling to room temperature to obtain the carbon fiber/silicon carbide porous framework.
2. Structure and component analysis of carbon fiber/silicon carbide porous framework material
The morphology of the sample is observed by using a Scanning Electron Microscope (SEM), as shown in figure 3, the skeleton structure of the prepared sample has certain orientation, and the SiC nanowires generated by the carbothermic reduction reaction are crosslinked with carbon fibers to form a good heat conducting network, so that the heat conductivity of the compound can be obviously improved. The composition of the sample was analyzed by X-ray diffractometry (XRD), and as shown in fig. 4, the prepared sample was a composite of carbon and β -SiC.
Example 3:
(1) preparing slurry: weighing 6g of silicon dioxide powder with the particle size of 500nm and 2.806g of silicon powder (the molar ratio of silicon to silicon dioxide is 1), uniformly mixing, drying and grinding for later use. Preparing 0.5 wt% CMC solution (the mass of CMC binder is 0.051g, the mass of deionized water is 10g), taking 1.394g of the mixed powder and 0.380g of carbon fiber powder with the particle size of 13 mu m, adding the mixture into the binder solution, stirring and mixing (wherein the silicon source and the carbon fiber powder account for 15 wt% of the slurry, and the molar ratio of carbon to silicon is 1), and removing bubbles to finish the preparation of the slurry.
(2) Freezing and freeze-drying: pouring the slurry into a special mold, removing air bubbles, and pre-freezing the mold in a freezing chamber at-20 deg.C for 15 min. And then placing the pre-frozen sample in a cold trap at the temperature of-65 ℃ for freezing for 20min, and finally carrying out vacuum freeze drying on a drying rack for 60h to obtain a sample of the oriented silicon source and carbon fiber mixture.
(3) And (3) heat treatment: the sample is subjected to two-stage heat treatment under argon atmosphere: pre-burning at 300 ℃ for 1h, then heating to 1200 ℃ for carbothermic reduction heat treatment for 10h, and naturally cooling to room temperature to obtain the carbon fiber/silicon carbide porous framework.
Example 4:
(1) preparing slurry: weighing 6g of silicon dioxide powder with the particle size of 500nm and 2.806g of silicon powder (the molar ratio of silicon to silicon dioxide is 1), uniformly mixing, drying and grinding for later use. Preparing 0.5 wt% CMC solution (the mass of CMC binder is 0.051g, the mass of deionized water is 10g), taking 1.394g of the mixed powder and 0.380g of carbon fiber powder with the particle size of 13 mu m, adding the mixture into the binder solution, stirring and mixing (wherein the silicon source and the carbon fiber powder account for 15 wt% of the slurry, and the molar ratio of carbon to silicon is 1), and removing bubbles to finish the preparation of the slurry.
(2) Freezing and freeze-drying: pouring the slurry into a special mold, removing air bubbles, and pre-freezing the mold in a freezing chamber at-20 deg.C for 15 min. And then placing the pre-frozen sample in a cold trap at the temperature of-65 ℃ for freezing for 20min, and finally carrying out vacuum freeze drying on a drying rack for 12h to obtain a sample of the oriented silicon source and carbon fiber mixture.
(3) And (3) heat treatment: the sample is subjected to two-stage heat treatment under argon atmosphere: pre-burning at 300 ℃ for 1h, then heating to 1800 ℃ for carbothermic reduction heat treatment for 1h, and naturally cooling to room temperature to obtain the carbon fiber/silicon carbide porous framework.
Example 5:
(1) preparing slurry: weighing 6g of silicon dioxide powder with the particle size of 500nm and 2.806g of silicon powder (the molar ratio of silicon to silicon dioxide is 1), uniformly mixing, drying and grinding for later use. Preparing 0.5 wt% CMC solution (the mass of CMC binder is 0.051g, the mass of deionized water is 10g), taking 0.477g of the mixed powder and 1.297g of carbon fiber powder with the particle size of 13 mu m, adding the mixture into the binder solution, stirring and mixing (wherein the silicon source and the carbon fiber powder account for 15 wt% of the slurry, and the molar ratio of carbon to silicon is 10), and removing air bubbles to finish the preparation of the slurry.
(2) Freezing and freeze-drying: pouring the slurry into a special mold, removing air bubbles, and pre-freezing the mold in a freezing chamber at-20 deg.C for 15 min. And then placing the pre-frozen sample in a cold trap at the temperature of-65 ℃ for freezing for 20min, and finally carrying out vacuum freeze drying on a drying rack for 24h to obtain a sample of the oriented silicon source and carbon fiber mixture.
(3) And (3) heat treatment: the sample is subjected to two-stage heat treatment under argon atmosphere: pre-burning at 300 ℃ for 1h, then heating to 1800 ℃ for carbothermic reduction heat treatment for 2h, and naturally cooling to room temperature to obtain the carbon fiber/silicon carbide porous framework.
Example 6:
(1) preparing slurry: weighing 6g of silicon dioxide powder with the particle size of 500nm and 2.806g of silicon powder (the molar ratio of silicon to silicon dioxide is 1), uniformly mixing, drying and grinding for later use. Preparing 5 wt% CMC solution (the mass of the CMC binder is 0.526g, the mass of the deionized water is 10g), adding 1.460g of the mixed powder and 0.398g of carbon fiber powder with the particle size of 13 mu m into the binder solution, stirring and mixing, (wherein the silicon source and the carbon fiber powder account for 15 wt% of the slurry, and the molar ratio of carbon to silicon is 1), and removing air bubbles to finish the preparation of the slurry.
(2) Freezing and freeze-drying: pouring the slurry into a special mold, removing air bubbles, and pre-freezing the mold in a freezing chamber at-20 deg.C for 15 min. And then placing the pre-frozen sample in a cold trap at the temperature of-65 ℃ for freezing for 20min, and finally carrying out vacuum freeze drying on a drying rack for 24h to obtain a sample of the oriented silicon source and carbon fiber mixture.
(3) And (3) heat treatment: the sample is subjected to two-stage heat treatment under argon atmosphere: pre-burning at 300 ℃ for 1h, then heating to 1200 ℃ for carbothermic reduction heat treatment for 2h, and naturally cooling to room temperature to obtain the carbon fiber/silicon carbide porous framework.
Example 7:
(1) preparing slurry: weighing 6g of silicon dioxide powder with the particle size of 500nm and 5.61g of silicon powder (the molar ratio of silicon to silicon dioxide is 2), uniformly mixing, drying and grinding for later use. Preparing a 5 wt% CMC solution (the mass of the CMC binder is 0.526g, and the mass of the deionized water is 10g), adding 1.418g of the mixed powder and 0.440g of carbon fiber powder with the particle size of 13 mu m into the binder solution, stirring and mixing (wherein the silicon source and the carbon fiber powder account for 15 wt% of the slurry, and the molar ratio of carbon to silicon is 1), and removing bubbles to finish the preparation of the slurry.
(2) Freezing and freeze-drying: pouring the slurry into a special mold, removing air bubbles, and pre-freezing the mold in a freezing chamber at-20 deg.C for 15 min. And then placing the pre-frozen sample in a cold trap at the temperature of-65 ℃ for freezing for 20min, and finally carrying out vacuum freeze drying on a drying rack for 24h to obtain a sample of the oriented silicon source and carbon fiber mixture.
(3) And (3) heat treatment: the sample is subjected to two-stage heat treatment under argon atmosphere: pre-burning at 300 ℃ for 1h, then heating to 1200 ℃ for carbothermic reduction heat treatment for 2h, and naturally cooling to room temperature to obtain the carbon fiber/silicon carbide porous framework.
Example 8:
(1) preparing slurry: weighing 6g of silicon dioxide powder with the particle size of 500nm and 5.61g of silicon powder (the molar ratio of silicon to silicon dioxide is 2), uniformly mixing, drying and grinding for later use. Preparing 5 wt% CMC solution (the mass of the CMC binder is 0.526g, the mass of the deionized water is 10g), taking 0.423 g of the mixed powder and 0.131g of carbon fiber powder with the particle size of 13 mu m, adding the powder and the carbon fiber powder into the binder solution, stirring and mixing (wherein the silicon source and the carbon fiber powder account for 5 wt% of the slurry, and the molar ratio of carbon to silicon is 1), and removing bubbles to finish the preparation of the slurry.
(2) Freezing and freeze-drying: pouring the slurry into a special mold, removing air bubbles, and pre-freezing the mold in a freezing chamber at-20 deg.C for 15 min. And then placing the pre-frozen sample in a cold trap at the temperature of-65 ℃ for freezing for 20min, and finally carrying out vacuum freeze drying on a drying rack for 24h to obtain a sample of the oriented silicon source and carbon fiber mixture.
(3) And (3) heat treatment: the sample is subjected to two-stage heat treatment under argon atmosphere: pre-burning at 300 ℃ for 1h, then heating to 1200 ℃ for carbothermic reduction heat treatment for 2h, and naturally cooling to room temperature to obtain the carbon fiber/silicon carbide porous framework.
Claims (6)
1. A preparation method of a carbon fiber/silicon carbide composite porous skeleton with directional heat conduction characteristics is characterized by comprising the following steps:
(1) uniformly mixing powder raw materials of silicon and silicon dioxide according to a certain proportion to prepare a silicon source mixture, and then dispersing the mixture and a carbon fiber raw material in a binder solution with a certain concentration according to a certain proportion to prepare uniformly mixed slurry; then pouring the slurry into a Teflon die with a copper bar at the bottom, and carrying out two-stage freezing treatment, namely 1) pre-freezing in a freezing chamber at the temperature of-30-0 ℃ for 10-25 min, and reducing the temperature of the slurry; 2) the bottom of the copper bar of the mould is placed in a cold trap at the temperature of-196 to-50 ℃ for freezing for 20min to 6 h; 3) and finally drying in a vacuum freeze dryer for 12-60 h.
(2) Placing the dried sample obtained in the step (1) in an argon atmosphere to carry out the following two-stage sintering treatment: 1) firstly, carrying out presintering treatment at a lower temperature to carbonize a binder; 2) and then, continuously carrying out high-temperature heat treatment in an argon atmosphere, generating silicon carbide by using a carbothermic reduction reaction, and cooling to room temperature to obtain the carbon fiber/silicon carbide composite porous skeleton with the directional heat conduction characteristic.
2. The method for preparing the carbon fiber/silicon carbide composite porous skeleton with the oriented heat conduction characteristic according to claim 1 is characterized in that the molar ratio of silicon to the silicon dioxide powder raw material in the step (1) is 1-2.
3. The method for preparing the carbon fiber/silicon carbide composite porous skeleton with the directional heat conduction characteristic according to claim 1, wherein the carbon/silicon molar ratio of the carbon fiber to the silicon source in the step (1) is 1-10.
4. The method for preparing the carbon fiber/silicon carbide composite porous skeleton with the oriented heat conduction characteristic according to claim 1, wherein the binder in the step (1) is selected from one or more of polyvinyl alcohol, polyethylene glycol, polyacrylic acid, sodium carboxymethyl cellulose, starch, polymethyl methacrylate, polyvinylidene fluoride and chitosan; the adhesive is prepared by dissolving the adhesive in a corresponding solvent, and the solution concentration of the adhesive is 0.5-5 wt%.
5. The preparation method of the carbon fiber/silicon carbide composite porous skeleton with the directional heat conduction characteristic according to claim 1, wherein the pretreatment temperature in the step (2) is 300-800 ℃, and the treatment time is 1-3 h; the carbothermic reduction temperature is 1200-1800 ℃, and the treatment time is 1-10 h.
6. The use of the carbon fiber/silicon carbide composite heat conducting skeleton with the oriented heat conducting structure prepared by the preparation method as a heat conducting filler in phase change heat storage materials and thermal interface materials according to any one of claims 1 to 5.
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| CN114214040A (en) * | 2022-01-26 | 2022-03-22 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Preparation method of organic phase-change composite material and prepared phase-change composite material |
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| CN115255350A (en) * | 2022-09-02 | 2022-11-01 | 中国矿业大学 | Wood powder and silicon dioxide composite nanoparticle packed bed porous heat-insulating material and preparation method thereof |
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