CN115058885B - Carbon fiber cloth surface orientation SiC nanowire array and preparation method thereof - Google Patents
Carbon fiber cloth surface orientation SiC nanowire array and preparation method thereof Download PDFInfo
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 98
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 98
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000004744 fabric Substances 0.000 title claims abstract description 67
- 239000002070 nanowire Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title abstract description 18
- 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 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000011065 in-situ storage Methods 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims description 45
- 238000005245 sintering Methods 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 229910002804 graphite Inorganic materials 0.000 claims description 18
- 239000010439 graphite Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 15
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 3
- 229940044175 cobalt sulfate Drugs 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 55
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 53
- 230000000694 effects Effects 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 8
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 5
- 238000005406 washing Methods 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000009827 uniform distribution Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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Abstract
The invention relates to a carbon fiber cloth surface directional SiC nanowire array and a preparation method thereof, which adopt low-cost raw materials and utilize a catalyst-assisted chemical vapor deposition process to realize in-situ directional growth of the SiC nanowire array on the carbon fiber cloth surface. The SiC nanowire has smooth surface and uniform size, and the large-area directional SiC nanowire array is obtained by using the preparation method. The technical scheme provided by the invention has the advantages of low raw material cost, simple and controllable process and equipment, strong universality and good repeatability. Because the SiC nanowire prepared by the method is different from the random orientation silicon carbide nanowire prepared by the prior art, the SiC nanowire prepared by the method has strong bonding force with a matrix, and is expected to achieve a satisfactory toughening effect. The SiC nanowires prepared by the method are uniformly distributed on the whole carbon fiber cloth, and the whole orientation on a single carbon fiber is obvious; the effect of large-area and repeatable in-situ directional growth of the SiC nanowire array is realized.
Description
Technical Field
The invention belongs to a preparation method of SiC nanowires, and relates to a carbon fiber cloth surface orientation SiC nanowire array and a preparation method thereof.
Background
SiC nanowires, because of their low density, good thermal and chemical stability, excellent mechanical strength, and greater aspect ratio than SiC nanoparticles and whiskers, are often incorporated into materials as reinforcing phases to improve their mechanical properties, document 1"Shen QL,Li HJ,Li L,et al.SiC nanowire reinforced carbon/carbon composites with improved interlaminar strength [ J ]. Materials Science and Engineering: a,2016,651:583-589," incorporation of toothed SiC nanowires into C/C composites by chemical vapor deposition, siC nanowires form a mechanical interlock with the matrix, improving load transfer efficiency, resulting in improved interlaminar strength of the material, but the reinforced interface results in reduced toughness of the composite. In addition, the SiC nanowires prepared by most of the current processes are paved on the surface of a matrix, so that the interface binding force between the SiC nanowires is weak, and further, poor load transfer effect is caused, and the toughening effect of the SiC nanowires is greatly limited. Meanwhile, the orientation of the SiC nanowire is also important to the exertion of the toughening effect of the SiC nanowire. The silicon carbide nano wire grown in situ and oriented has strong binding force with the matrix, even orientation distribution and hopeful realization of satisfactory toughening effect.
Aiming at the directional growth of the silicon carbide nanowires, the current preparation technology mainly comprises a template method and a polymer precursor pyrolysis method. Document 2 et al, "Pan ZW, lai HL, au FCK, et al, oriented silicon carbide nanowires: synthesis and field emission properties [ J ]. Advanced Materials,2000,12 (16): 1186-1190," prepared directionally grown SiC nanowires with orientation and dimensions highly similar to carbon nanotube templates using a carbon nanotube template method. However, the use of the template method to prepare the SiC nanowire directional array creates the problem that the subsequent template is difficult to remove, and the nanowire size and orientation are limited by the template, and the steps are complex and the cost is high. In patent 1 (CN 200910160766.5), single crystal SiC nanowires were grown by SiC single-wafer induction, resulting in large-area directionally grown SiC nanowires. Document 3"Liu WN,Li XX,Li WJ,et al.High-performance supercapacitors based on free-standing SiC@PEDOT nanowires with robust cycling stability [ J ]. Journal of Energy Chemistry,2022, 66:30-37" "SiC nanowires are grown on carbon fibers by thermal depolymerization of silazane. But further applications are limited due to the higher cost of the polymer precursor.
The invention realizes the uniform distribution of SiC nanowires on the whole carbon fiber cloth and the in-situ uniform directional growth of SiC nanowires on single carbon fiber by a catalyst-assisted chemical vapor deposition method to obtain a large-area directional SiC nanowire array; the method effectively solves the problems of complex process, high cost and the like, and provides a novel technology and method for preparing the SiC nanowire for toughening.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a carbon fiber cloth surface orientation SiC nanowire array and a preparation method thereof.
Technical proposal
The directional SiC nanowire array is characterized in that the SiC nanowires are smooth in surface and uniform in size, are uniformly distributed on the whole carbon fiber cloth and uniformly and directionally grow on single carbon fiber in situ.
The preparation method of the carbon fiber cloth surface orientation SiC nanowire array is characterized by comprising the following steps:
step 1, carbon fiber cloth treatment: placing the pretreated carbon fibers in a metal salt catalyst solution for soaking for 1-10 hours, taking out, and placing in a 60-100 ℃ oven for drying for 5-24 hours;
step 2, mixing powder: siO is made of 2 Mixing Si and C powder according to the mass ratio of 1:0.1-0.5:0.3-0.7, putting into a planetary ball mill for grinding for 12-24 hours at 150-200 rpm to obtain mixed uniform powder, taking out and putting into a baking oven at 60-100 ℃ for 5-12 hours for baking;
step 3, directional synthesis of SiC nanowires on the surface of the carbon fiber cloth: placing the powder obtained in the step 2 into a graphite crucible, arranging the dried carbon fiber impregnated with metal salt at the top of the graphite crucible and 1-5 cm away from the bottom of the crucible, placing into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1-0.4 Pa; argon is filled into the atmosphere sintering furnace at the flow rate of 10-200 mL/min; and then heating the atmosphere sintering furnace to 1300-1800 ℃ at a heating rate of 5-20 ℃/min, preserving heat at the temperature for 1-10 h, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally growing on the surface of the carbon fiber cloth.
The pretreatment of the carbon fiber cloth is to clean the carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, and dry the carbon fiber cloth in an oven at 60-100 ℃ for 8-24 hours.
The metal salt solutions include, but are not limited to: ferric nitrate, cobalt nitrate, nickel nitrate, ferrous sulfate, cobalt sulfate, nickel sulfate, ferric chloride, cobalt chloride or nickel chloride.
Advantageous effects
According to the carbon fiber cloth surface directional SiC nanowire array and the preparation method, the SiC nanowire array is directionally grown on the carbon fiber cloth surface in situ by adopting low-cost raw materials and utilizing a catalyst-assisted chemical vapor deposition process. The SiC nanowire has smooth surface, uniform size, uniform distribution on the whole carbon fiber cloth, uniform directional growth in situ on single carbon fiber, and obvious directional effect. The preparation method provided by the invention is used for obtaining the large-area directional SiC nanowire array. The technical scheme provided by the invention has the advantages of low raw material cost, simple and controllable process and equipment, strong universality and good repeatability. Because the SiC nanowire prepared by the method is different from the random orientation silicon carbide nanowire prepared by the prior art, the SiC nanowire prepared by the method has strong bonding force with a matrix, and is expected to achieve a satisfactory toughening effect. The SiC nanowires prepared by the method are uniformly distributed on the whole carbon fiber cloth, and the whole orientation on a single carbon fiber is obvious; the effect of large-area and repeatable in-situ directional growth of the SiC nanowire array is realized.
The invention adopts low-cost raw material, namely SiO 2 The Si and C mixed powder and the catalyst-assisted chemical vapor deposition process are utilized, and the reaction mechanism is a catalyst-assisted gas-liquid-solid (VLS) mechanism, so that the effect of in-situ directional growth of the SiC nanowire array on the surface of the carbon fiber cloth is achieved. SiC nanowires grown in situ oriented on the substrate surface are believed to have a more excellent toughening effect than SiC nanowires randomly oriented and tiled on the substrate surface. The SiC nanowires prepared by the method are uniformly distributed on the whole carbon fiber cloth and uniformly and directionally grow on single carbon fiber in situ, the directional effect is obvious, and the large-area directional SiC nanowire array is obtained. The technical scheme has the advantages of simple operation, controllable process, low raw material cost, good repeatability and strong universality, and has wide application prospect.
Fig. 1 is an XRD pattern of an oriented SiC nanowire array on the surface of a carbon fiber cloth prepared according to the present invention, and it can be known from XRD of fig. 1 that the main component of the SiC nanowire prepared according to the present invention is β -SiC. Fig. 2 is a low-power SEM characterization diagram of an oriented SiC nanowire array on the surface of the carbon fiber cloth prepared by the present invention, and as can be seen from the low-power scanning electron microscope photograph of fig. 2, the SiC nanowires prepared by the present invention uniformly grow on the carbon fiber cloth, and have uniform morphology. FIG. 3 is an SEM characterization diagram of an in-situ growth of an oriented SiC nanowire array prepared by the invention on a single carbon fiber, and the scanning electron microscope photograph of FIG. 3 shows that the SiC nanowire prepared by the invention is in-situ oriented on the carbon fiber, the surface of the nanowire is smooth, the diameter is 0.5-1.5 mu m, and the length is 10-30 mu m. Moreover, the presence of a spherical cap catalyst was observed at the top of the SiC nanowires, indicating that the growth mechanism of the SiC nanowires is a catalyst-assisted gas-liquid-solid (VLS) mechanism. In summary, the technical scheme provided by the invention realizes the uniform distribution of SiC nanowires on the whole carbon fiber cloth, and the in-situ uniform directional growth on single carbon fiber to obtain a large-area directional SiC nanowire array; the technical scheme has the advantages of low raw material cost, simple and controllable process and equipment, strong universality and good repeatability. The invention provides a novel technology and a novel method for preparing the SiC nanowire directional array.
Drawings
Fig. 1: XRD patterns of the directional SiC nanowire arrays on the surfaces of the carbon fiber cloth prepared by the invention;
fig. 2: the invention provides a low-power SEM characterization graph of a carbon fiber cloth surface orientation SiC nanowire array;
fig. 3: SEM characterization graph of directional SiC nanowire array in-situ grown on single carbon fiber.
Detailed Description
The invention will now be further described with reference to examples, figures:
example 1:
1. carbon fiber cloth treatment: washing carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, drying in a 70 ℃ oven for 12 hours, arranging the dried carbon fiber in a 1mol/L ferric nitrate solution for soaking for 1 hour, taking out, and drying in the 70 ℃ oven for 12 hours;
2. powder mixing: siO is made of 2 Mixing Si and C powder according to the mass ratio of 1:0.4:0.5, putting into a planetary ball mill, grinding for 12h at 200 r/min to obtain mixed uniform powder, taking out, and putting into a 70 ℃ oven for drying for 8 h;
3. the SiC nanowires are directionally synthesized on the surface of the carbon fiber cloth:
weighing 1g of the powder obtained in the second step, putting the powder into a graphite crucible, arranging the dried carbon fiber impregnated with the metal salt at the top of the graphite crucible and 2cm away from the bottom of the crucible, putting the powder into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1Pa; argon is filled into the atmosphere sintering furnace at the flow rate of 10 mL/min; and then heating the atmosphere sintering furnace to 1500 ℃ at a heating rate of 5 ℃/min, preserving heat at the temperature for 4 hours, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally growing on the surface of the carbon fiber cloth, thereby completing the preparation.
Example 2:
1. carbon fiber cloth treatment: washing carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, drying in a 70 ℃ oven for 12 hours, arranging the dried carbon fiber in a 1mol/L ferric nitrate solution for soaking for 1 hour, taking out, and drying in the 70 ℃ oven for 12 hours;
2. powder mixing: siO is made of 2 Mixing Si and C powder according to the mass ratio of 1:0.4:0.5, putting into a planetary ball mill, grinding for 12h at 200 r/min to obtain mixed uniform powder, taking out, and putting into a 70 ℃ oven for drying for 8 h;
3. the SiC nanowires are directionally synthesized on the surface of the carbon fiber cloth:
2g of the powder obtained in the second step is weighed and placed into a graphite crucible, the dried carbon fiber impregnated with the metal salt is arranged at the top of the graphite crucible and is 2cm away from the bottom of the crucible, the powder is placed into an atmosphere sintering furnace, and the vacuum degree of the atmosphere sintering furnace is controlled to be 0.1Pa; argon is filled into the atmosphere sintering furnace at the flow rate of 100 mL/min; and then heating the atmosphere sintering furnace to 1500 ℃ at a heating rate of 5 ℃/min, preserving heat at the temperature for 6 hours, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally growing on the surface of the carbon fiber cloth, thereby completing the preparation.
Example 3:
1. carbon fiber cloth treatment: washing carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, drying in a 70 ℃ oven for 12 hours, arranging the dried carbon fiber in a 1mol/L ferric nitrate solution for soaking for 1 hour, taking out, and drying in the 70 ℃ oven for 12 hours;
2. powder mixing: siO is made of 2 Mixing Si and C powder according to the mass ratio of 1:0.4:0.5, putting into a planetary ball mill, grinding for 12h at 200 r/min to obtain mixed uniform powder, taking out, and putting into a 70 ℃ oven for drying for 8 h;
3. the SiC nanowires are directionally synthesized on the surface of the carbon fiber cloth:
weighing 1g of the powder obtained in the second step, putting the powder into a graphite crucible, arranging the dried carbon fiber impregnated with the metal salt at the top of the graphite crucible and 2cm away from the bottom of the crucible, putting the powder into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1Pa; argon is filled into the atmosphere sintering furnace at the flow rate of 50 mL/min; and then heating the atmosphere sintering furnace to 1600 ℃ at a heating rate of 5 ℃/min, preserving heat at the temperature for 2 hours, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally growing on the surface of the carbon fiber cloth, thereby completing the preparation.
Example 4:
1. carbon fiber cloth treatment: washing carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, drying in a 70 ℃ oven for 12 hours, arranging the dried carbon fiber in 0.5mol/L ferric nitrate solution for soaking for 1 hour, taking out, and drying in the 70 ℃ oven for 12 hours;
2. powder mixing: siO is made of 2 Mixing Si and C powder according to the mass ratio of 1:0.4:0.5, putting into a planetary ball mill, grinding for 12h at 200 r/min to obtain mixed uniform powder, taking out, and putting into a 70 ℃ oven for drying for 8 h;
3. the SiC nanowires are directionally synthesized on the surface of the carbon fiber cloth:
weighing 4g of the powder obtained in the second step, putting the powder into a graphite crucible, arranging the dried carbon fiber impregnated with the metal salt at the top of the graphite crucible and 2cm away from the bottom of the crucible, putting the powder into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1Pa; argon is filled into the atmosphere sintering furnace at the flow rate of 10 mL/min; and then heating the atmosphere sintering furnace to 1500 ℃ at a heating rate of 5 ℃/min, preserving heat at the temperature for 2 hours, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally growing on the surface of the carbon fiber cloth, thereby completing the preparation.
Example 5:
1. carbon fiber cloth treatment: washing carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, drying in a 70 ℃ oven for 12 hours, arranging the dried carbon fiber in a 1mol/L cobalt nitrate solution for soaking for 1 hour, taking out, and drying in the 70 ℃ oven for 12 hours;
2. powder mixing: siO is made of 2 Mixing Si and C powder according to the mass ratio of 1:0.4:0.5, putting into a planetary ball mill, grinding for 12h at 200 r/min to obtain mixed uniform powder, taking out, and putting into a 70 ℃ oven for drying for 8 h;
3. the SiC nanowires are directionally synthesized on the surface of the carbon fiber cloth:
2g of the powder obtained in the second step is weighed and placed into a graphite crucible, the dried carbon fiber impregnated with the metal salt is arranged at the top of the graphite crucible and is 2cm away from the bottom of the crucible, the powder is placed into an atmosphere sintering furnace, and the vacuum degree of the atmosphere sintering furnace is controlled to be 0.1Pa; argon is filled into the atmosphere sintering furnace at the flow rate of 10 mL/min; and then heating the atmosphere sintering furnace to 1500 ℃ at a heating rate of 5 ℃/min, preserving heat at the temperature for 4 hours, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally growing on the surface of the carbon fiber cloth, thereby completing the preparation.
Example 6:
1. carbon fiber cloth treatment: washing carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, drying in a 70 ℃ oven for 12 hours, arranging the dried carbon fiber in a 1mol/L cobalt nitrate solution for soaking for 1 hour, taking out, and drying in the 70 ℃ oven for 12 hours;
2. powder mixing: siO is made of 2 Mixing Si and C powder according to the mass ratio of 1:0.4:0.5, putting into a planetary ball mill, grinding for 12h at 200 r/min to obtain mixed uniform powder, taking out, and putting into a 70 ℃ oven for drying for 8 h;
3. the SiC nanowires are directionally synthesized on the surface of the carbon fiber cloth:
2g of the powder obtained in the second step is weighed and placed into a graphite crucible, the dried carbon fiber impregnated with the metal salt is arranged at the top of the graphite crucible and is 2cm away from the bottom of the crucible, the powder is placed into an atmosphere sintering furnace, and the vacuum degree of the atmosphere sintering furnace is controlled to be 0.1Pa; argon is filled into the atmosphere sintering furnace at the flow rate of 10 mL/min; and then heating the atmosphere sintering furnace to 1600 ℃ at a heating rate of 5 ℃/min, preserving heat at the temperature for 2 hours, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally growing on the surface of the carbon fiber cloth, thereby completing the preparation.
The invention provides a preparation method of a carbon fiber cloth surface orientation SiC nanowire array. According to the technical scheme provided by the invention, the SiC nanowires are uniformly distributed on the whole carbon fiber cloth and uniformly and directionally grow on the single carbon fiber in situ, and the large-area directional SiC nanowire array is obtained. The technical scheme has the advantages of low raw material cost, simple and controllable process and equipment, strong universality and good repeatability. The invention provides a novel technology and a novel method for preparing the SiC nanowire directional array.
The technical scheme of the invention is not limited to the specific embodiments listed above, and various changes can be made. I.e. all other embodiments obtained according to the claims and the description of the present application, are within the scope of the present invention.
Claims (3)
1. The directional SiC nanowire array on the surface of the carbon fiber cloth is characterized in that the SiC nanowires are smooth in surface and uniform in size, are uniformly distributed on the whole carbon fiber cloth and uniformly grow in an in-situ and directional manner on single carbon fiber;
the carbon fiber cloth surface orientation SiC nanowire array is prepared according to the following steps:
step 1, carbon fiber cloth treatment: placing the pretreated carbon fibers in a metal salt catalyst solution for soaking for 1-10 hours, taking out, and placing in a 60-100 ℃ oven for drying for 5-24 hours;
step 2, mixing powder: siO is made of 2 Mixing Si and C powder according to the mass ratio of 1:0.1-0.5:0.3-0.7, putting into a planetary ball mill for grinding for 12-24 hours at 150-200 rpm to obtain mixed uniform powder, taking out and putting into a baking oven at 60-100 ℃ for 5-12 hours for baking;
step 3, directional synthesis of SiC nanowires on the surface of the carbon fiber cloth: placing the powder obtained in the step 2 into a graphite crucible, arranging the dried carbon fiber impregnated with metal salt at the top of the graphite crucible and 1-5 cm away from the bottom of the crucible, placing into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1-0.4 Pa; argon is filled into the atmosphere sintering furnace at the flow rate of 10-200 mL/min; then heating the atmosphere sintering furnace to 1300-1800 ℃ at a heating rate of 5-20 ℃/min, preserving heat at the temperature for 1-10 h, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally growing on the surface of the carbon fiber cloth;
the metal salt solution comprises: ferric nitrate, cobalt nitrate, nickel nitrate, ferrous sulfate, cobalt sulfate, nickel sulfate, ferric chloride, cobalt chloride or nickel chloride.
2. A method for preparing the carbon fiber cloth surface orientation SiC nanowire array of claim 1, which is characterized by comprising the following steps:
step 1, carbon fiber cloth treatment: placing the pretreated carbon fibers in a metal salt catalyst solution for soaking for 1-10 hours, taking out, and placing in a 60-100 ℃ oven for drying for 5-24 hours;
step 2, mixing powder: siO is made of 2 Mixing Si and C powder according to the mass ratio of 1:0.1-0.5:0.3-0.7, putting into a planetary ball mill for grinding for 12-24 hours at 150-200 rpm to obtain mixed uniform powder, taking out and putting into a baking oven at 60-100 ℃ for 5-12 hours for baking;
step 3, directional synthesis of SiC nanowires on the surface of the carbon fiber cloth: placing the powder obtained in the step 2 into a graphite crucible, arranging the dried carbon fiber impregnated with metal salt at the top of the graphite crucible and 1-5 cm away from the bottom of the crucible, placing into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1-0.4 Pa; argon is filled into the atmosphere sintering furnace at the flow rate of 10-200 mL/min; then heating the atmosphere sintering furnace to 1300-1800 ℃ at a heating rate of 5-20 ℃/min, preserving heat at the temperature for 1-10 h, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally growing on the surface of the carbon fiber cloth;
the metal salt solution comprises: ferric nitrate, cobalt nitrate, nickel nitrate, ferrous sulfate, cobalt sulfate, nickel sulfate, ferric chloride, cobalt chloride or nickel chloride.
3. The method according to claim 2, characterized in that: the pretreatment of the carbon fiber cloth is to clean the carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, and dry the carbon fiber cloth in an oven at 60-100 ℃ for 8-24 hours.
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