CN115058885A - Carbon fiber cloth surface oriented SiC nanowire array and preparation method thereof - Google Patents
Carbon fiber cloth surface oriented SiC nanowire array and preparation method thereof Download PDFInfo
- Publication number
- CN115058885A CN115058885A CN202210661138.0A CN202210661138A CN115058885A CN 115058885 A CN115058885 A CN 115058885A CN 202210661138 A CN202210661138 A CN 202210661138A CN 115058885 A CN115058885 A CN 115058885A
- Authority
- CN
- China
- Prior art keywords
- carbon fiber
- fiber cloth
- sic
- powder
- sic nanowire
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 113
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 113
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000004744 fabric Substances 0.000 title claims abstract description 88
- 239000002070 nanowire Substances 0.000 title claims abstract description 52
- 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 30
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000011065 in-situ storage Methods 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 59
- 238000005245 sintering Methods 0.000 claims description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 229910002804 graphite Inorganic materials 0.000 claims description 24
- 239000010439 graphite Substances 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 13
- 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 12
- 239000002184 metal Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 150000003839 salts Chemical class 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 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
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 230000002194 synthesizing effect Effects 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 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 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 2
- 239000012266 salt solution Substances 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 54
- 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
- 239000011159 matrix material Substances 0.000 abstract description 6
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 5
- 238000004140 cleaning Methods 0.000 description 6
- 239000011863 silicon-based powder Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 238000009827 uniform distribution Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002105 nanoparticle Substances 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
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 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
- 239000011812 mixed powder Substances 0.000 description 1
- 235000012149 noodles Nutrition 0.000 description 1
- 229920001709 polysilazane Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
Abstract
The invention relates to a carbon fiber cloth surface oriented SiC nanowire array and a preparation method thereof, which adopts low-cost raw materials and utilizes a catalyst to assist a chemical vapor deposition process to realize in-situ oriented growth of the SiC nanowire array on the surface of the carbon fiber cloth. 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. The SiC nanowire prepared by the invention has strong binding force with a matrix and is expected to achieve satisfactory toughening effect because of being different from the randomly oriented silicon carbide nanowire prepared by the predecessor. 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 oriented 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 larger aspect ratio than SiC nanoparticles and whiskers, are often introduced as a reinforcing phase into Materials to improve their mechanical properties, as described in document 1, "ShenQL, Li HJ, Li L, et al, SiC nanowire recycled carbon/carbon composites with improved interlaminar strength [ J ]. Materials Science and Engineering: A,2016,651:583 ″" by chemical vapor deposition to introduce the toothed SiC nanowires into C/C composites, the SiC nanowires form mechanical interlocks with the matrix, increasing the load transfer efficiency, increasing the interlaminar strength of the Materials, but the reinforced interface leads to a decrease in the toughness of the composites. In addition, most of the SiC nanowires prepared by the prior art are paved on the surface of a matrix, so that the interface bonding force between the SiC nanowires and the matrix is weak, the load transfer effect is poor, and the toughening effect of the SiC nanowires is greatly limited. Meanwhile, the orientation of the SiC nanowires is also important for the toughening effect of the SiC nanowires. The silicon carbide nanowires grown in the in-situ orientation mode have strong binding force with a matrix and uniform orientation distribution, and are expected to achieve satisfactory toughening effect.
Aiming at the directional growth of the silicon carbide nanowire, the current preparation technology mainly comprises a template method and a polymer precursor pyrolysis method. Reference 2 et al, "Pan ZW, Lai HL, Au FCK, et al. organic silicon carbide nanoparticles: synthesis and field emission properties [ J ]. Advanced Materials,2000,12(16): 1186-. However, the problem that the subsequent template is difficult to remove is caused when the SiC nanowire directional array is prepared by using the template method, the size and the orientation of the nanowire are limited by the template, the steps are complex, and the cost is high. In patent 1(CN200910160766.5), a single crystal SiC nanowire is induced to grow through a single crystal SiC wafer, and a large area directionally grown SiC nanowire is obtained. Document 3 "Liu WN, Li XX, Li WJ, et al, high-performance supercapacitors based on free-standing SiC @ PEDOT nanowinds with robust cycling stability [ J ]. Journal of Energy Chemistry,2022,66: 30-37" SiC nanowires are grown on carbon fibers by thermal depolymerization of polysilazane. But limit its further applications due to the high cost of the polymer precursors.
According to the invention, the uniform distribution of SiC nanowires on the whole carbon fiber cloth and the in-situ uniform and directional growth on a single carbon fiber are realized by a catalyst-assisted chemical vapor deposition method, so that a large-area directional SiC nanowire array is obtained; the method effectively avoids the problems of complex process, high cost and the like, and provides a new technology and a new 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 oriented SiC nanowire array and a preparation method thereof.
Technical scheme
A surface-oriented SiC nanowire array of carbon fiber cloth is characterized in that SiC nanowires are smooth in surface and uniform in size, are uniformly distributed on the whole carbon fiber cloth and uniformly grow on single carbon fibers in an in-situ and oriented manner.
A preparation method of the carbon fiber cloth surface oriented SiC nanowire array is characterized by comprising the following steps:
step 3, directionally synthesizing the SiC nanowires on the surface of the carbon fiber cloth: putting the powder obtained in the step (2) into a graphite crucible, arranging the dried carbon fiber impregnated with metal salt on the top of the graphite crucible, wherein the distance between the dried carbon fiber and the bottom of the crucible is 1-5 cm, putting the graphite crucible into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1-0.4 Pa; then filling argon 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 the heating rate of 5-20 ℃/min, preserving the heat at the temperature for 1-10 h, then stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally grown on the surface of the carbon fiber cloth.
The carbon fiber cloth pretreatment is to wash the carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, and to dry the carbon fiber cloth in an oven at 60-100 ℃ for 8-24 hours.
The metal salt solution includes but is not limited to: ferric nitrate, cobalt nitrate, nickel nitrate, ferrous sulfate, cobalt sulfate, nickel sulfate, ferric chloride, cobalt chloride or nickel chloride.
Advantageous effects
The invention provides a carbon fiber cloth surface oriented SiC nanowire array and a preparation method thereof, which adopt low-cost raw materials and utilize a catalyst to assist a chemical vapor deposition process, and realize in-situ oriented growth of the SiC nanowire array on the surface of the carbon fiber cloth. The SiC nanowires have smooth surfaces and uniform sizes, are uniformly distributed on the whole carbon fiber cloth and uniformly grow on single carbon fibers in an in-situ and directional manner, and have obvious directional effect. The preparation method 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. The SiC nanowire prepared by the invention has strong binding force with a matrix and is expected to achieve satisfactory toughening effect because of being different from the randomly oriented silicon carbide nanowire prepared by the predecessor. 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 is prepared by a catalyst-assisted chemical vapor deposition process, 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. Compared to SiC nanowires that are randomly oriented and tiled on the surface of the substrate, SiC nanowires that are directionally grown in situ on the surface of the substrate are considered to have a superior toughening effect. The SiC nano prepared by the inventionThe rice noodles are uniformly distributed on the whole carbon fiber cloth and uniformly grow on the single carbon fiber in an in-situ and directional manner, 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, strong universality and wide application prospect.
Fig. 1 is an XRD spectrum of the carbon fiber cloth surface oriented SiC nanowire array prepared by the present invention, and as can be seen from the XRD of fig. 1, the main component of the SiC nanowire prepared by the present invention is β -SiC. FIG. 2 is a low-power SEM representation of the oriented SiC nanowire array on the surface of the carbon fiber cloth prepared by the invention, and as can be seen from the low-power SEM photograph in FIG. 2, the SiC nanowires prepared by the invention uniformly grow on the carbon fiber cloth and have uniform morphology. FIG. 3 is an SEM representation of the in-situ growth of the oriented SiC nanowire array prepared by the present invention on a single carbon fiber, and as can be seen from the SEM photograph of FIG. 3, the SiC nanowire prepared by the present invention has the advantages of in-situ oriented growth on the carbon fiber, smooth surface, diameter of 0.5-1.5 μm, and length of 10-30 μm. Moreover, the presence of a spherical crown catalyst was observed at the tip of the SiC nanowire, suggesting that the growth mechanism of the SiC nanowire is a catalyst-assisted gas-liquid-solid (VLS) mechanism. In conclusion, 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 of the SiC nanowires on a single carbon fiber, so that a 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 new technology and a method for preparing the SiC nanowire directional array.
Drawings
FIG. 1: the XRD pattern of the directional SiC nanowire array on the surface of the carbon fiber cloth prepared by the invention;
FIG. 2: the invention discloses a low-power SEM representation of a directional SiC nanowire array on the surface of carbon fiber cloth;
FIG. 3: the directional SiC nanowire array prepared by the invention grows on a single carbon fiber in situ in an SEM representation picture.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1:
firstly, carbon fiber cloth treatment: cleaning carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, placing the carbon fiber cloth in a 70 ℃ oven for drying for 12h, placing the dried carbon fiber cloth in a 1mol/L ferric nitrate solution for soaking for 1h, taking out the carbon fiber cloth, and placing the carbon fiber cloth in the 70 ℃ oven for drying for 12 h;
secondly, mixing powder: mixing SiO 2 Mixing the Si powder and the C powder according to the mass ratio of 1:0.4:0.5, putting the mixture into a planetary ball mill, grinding the mixture for 12 hours at 200 revolutions per minute to obtain mixed uniform powder, taking the powder out, and putting the powder into a 70 ℃ oven to dry the powder for 8 hours;
thirdly, directionally synthesizing the SiC nanowires on the surface of the carbon fiber cloth:
weighing 1g of the powder obtained in the second step, placing the powder into a graphite crucible, placing the dried carbon fiber impregnated with metal salt on the top of the graphite crucible, placing the graphite crucible 2cm away from the bottom of the crucible into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1 Pa; then filling argon into the atmosphere sintering furnace at the flow rate of 10 mL/min; and then heating the atmosphere sintering furnace to 1500 ℃ at the heating rate of 5 ℃/min, preserving heat for 4h at the temperature, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally grown on the surface of the carbon fiber cloth, thereby completing the preparation.
Example 2:
firstly, carbon fiber cloth treatment: cleaning carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, placing the carbon fiber cloth in a 70 ℃ oven for drying for 12h, placing the dried carbon fiber cloth in a 1mol/L ferric nitrate solution for soaking for 1h, taking out the carbon fiber cloth, and placing the carbon fiber cloth in the 70 ℃ oven for drying for 12 h;
secondly, mixing powder: mixing SiO 2 Mixing Si powder and C powder according to the mass ratio of 1:0.4:0.5, grinding the mixture in a planetary ball mill for 12 hours at 200 revolutions per minute to obtain mixed uniform powder, taking out the mixed uniform powder, and placing the mixed uniform powder in a 70 ℃ oven for drying for 8 hours;
thirdly, directionally synthesizing the SiC nanowires on the surface of the carbon fiber cloth:
weighing 2g of the powder obtained in the second step, placing the powder into a graphite crucible, placing the dried carbon fiber impregnated with metal salt on the top of the graphite crucible, placing the graphite crucible 2cm away from the bottom of the crucible into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1 Pa; then filling argon into the atmosphere sintering furnace at the flow rate of 100 mL/min; and then heating the atmosphere sintering furnace to 1500 ℃ at the heating rate of 5 ℃/min, preserving heat for 6h at the temperature, stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally grown on the surface of the carbon fiber cloth, thus completing the preparation.
Example 3:
firstly, carbon fiber cloth treatment: cleaning carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, placing the carbon fiber cloth in a 70 ℃ oven for drying for 12h, placing the dried carbon fiber cloth in a 1mol/L ferric nitrate solution for soaking for 1h, taking out the carbon fiber cloth, and placing the carbon fiber cloth in the 70 ℃ oven for drying for 12 h;
secondly, mixing powder: mixing SiO 2 Mixing the Si powder and the C powder according to the mass ratio of 1:0.4:0.5, putting the mixture into a planetary ball mill, grinding the mixture for 12 hours at 200 revolutions per minute to obtain mixed uniform powder, taking the powder out, and putting the powder into a 70 ℃ oven to dry the powder for 8 hours;
thirdly, directionally synthesizing the SiC nanowires on the surface of the carbon fiber cloth:
weighing 1g of the powder obtained in the second step, placing the powder into a graphite crucible, placing the dried carbon fiber impregnated with metal salt on the top of the graphite crucible, placing the graphite crucible 2cm away from the bottom of the crucible into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1 Pa; then filling argon into the atmosphere sintering furnace at the flow rate of 50 mL/min; and then heating the atmosphere sintering furnace to 1600 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h at the temperature, then stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally grown on the surface of the carbon fiber cloth, thus completing the preparation.
Example 4:
firstly, carbon fiber cloth treatment: cleaning carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, placing the carbon fiber cloth in a 70 ℃ oven for drying for 12h, placing the dried carbon fiber cloth in a 0.5mol/L ferric nitrate solution for soaking for 1h, taking out the carbon fiber cloth, and placing the carbon fiber cloth in the 70 ℃ oven for drying for 12 h;
secondly, mixing powder: mixing SiO 2 Mixing the Si powder and the C powder according to the mass ratio of 1:0.4:0.5, putting the mixture into a planetary ball mill, grinding the mixture for 12 hours at 200 revolutions per minute to obtain mixed uniform powder, taking the powder out, and putting the powder into a 70 ℃ oven to dry the powder for 8 hours;
thirdly, directionally synthesizing the SiC nanowires on the surface of the carbon fiber cloth:
weighing 4g of the powder obtained in the second step, placing the powder into a graphite crucible, placing the dried carbon fiber impregnated with metal salt on the top of the graphite crucible, placing the graphite crucible 2cm away from the bottom of the crucible into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1 Pa; then filling argon into the atmosphere sintering furnace at the flow rate of 10 mL/min; and then heating the atmosphere sintering furnace to 1500 ℃ at the heating rate of 5 ℃/min, preserving heat for 2 hours at the temperature, then stopping heating, cooling to room temperature along with the furnace, opening the furnace to obtain the SiC nanowire array which directionally grows on the surface of the carbon fiber cloth, and completing the preparation.
Example 5:
firstly, carbon fiber cloth treatment: cleaning carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, placing the carbon fiber cloth in an oven at 70 ℃ for drying for 12h, placing the dried carbon fiber cloth in a 1mol/L cobalt nitrate solution for soaking for 1h, taking out the carbon fiber cloth, and placing the carbon fiber cloth in the oven at 70 ℃ for drying for 12 h;
secondly, mixing powder: mixing SiO 2 Mixing the Si powder and the C powder according to the mass ratio of 1:0.4:0.5, putting the mixture into a planetary ball mill, grinding the mixture for 12 hours at 200 revolutions per minute to obtain mixed uniform powder, taking the powder out, and putting the powder into a 70 ℃ oven to dry the powder for 8 hours;
thirdly, directionally synthesizing the SiC nanowires on the surface of the carbon fiber cloth:
weighing 2g of the powder obtained in the second step, placing the powder into a graphite crucible, placing the dried carbon fiber impregnated with metal salt on the top of the graphite crucible, placing the graphite crucible 2cm away from the bottom of the crucible into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1 Pa; then filling argon into the atmosphere sintering furnace at the flow rate of 10 mL/min; and then heating the atmosphere sintering furnace to 1500 ℃ at the heating rate of 5 ℃/min, preserving heat for 4 hours at the temperature, then stopping heating, cooling to room temperature along with the furnace, opening the furnace to obtain the SiC nanowire array which directionally grows on the surface of the carbon fiber cloth, and completing the preparation.
Example 6:
firstly, carbon fiber cloth treatment: cleaning carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, placing the carbon fiber cloth in an oven at 70 ℃ for drying for 12h, placing the dried carbon fiber cloth in a 1mol/L cobalt nitrate solution for soaking for 1h, taking out the carbon fiber cloth, and placing the carbon fiber cloth in the oven at 70 ℃ for drying for 12 h;
secondly, mixing powder: mixing SiO 2 Mixing the Si powder and the C powder according to the mass ratio of 1:0.4:0.5, putting the mixture into a planetary ball mill, grinding the mixture for 12 hours at 200 revolutions per minute to obtain mixed uniform powder, taking the powder out, and putting the powder into a 70 ℃ oven to dry the powder for 8 hours;
thirdly, directionally synthesizing the SiC nanowires on the surface of the carbon fiber cloth:
weighing 2g of the powder obtained in the second step, placing the powder into a graphite crucible, placing the dried carbon fiber impregnated with metal salt on the top of the graphite crucible, placing the graphite crucible 2cm away from the bottom of the crucible into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1 Pa; then filling argon into the atmosphere sintering furnace at the flow of 10 mL/min; and then heating the atmosphere sintering furnace to 1600 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h at the temperature, then stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally grown on the surface of the carbon fiber cloth, thus completing the preparation.
The invention provides a preparation method of a carbon fiber cloth surface oriented SiC nanowire array. 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 a single carbon fiber, and obtains the 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 new technology and a method for preparing the SiC nanowire directional array.
The technical solution of the present invention is not limited to the above-mentioned embodiments, and various changes may be made. That is, all other embodiments obtained from the claims and the content of the description of the present application belong to the scope of protection of the present invention.
Claims (4)
1. A surface-oriented SiC nanowire array of carbon fiber cloth is characterized in that SiC nanowires are smooth in surface and uniform in size, are uniformly distributed on the whole carbon fiber cloth and uniformly grow on single carbon fibers in an in-situ and oriented manner.
2. A method for preparing the carbon fiber cloth surface orientation SiC nanowire array as recited in claim 1, characterized by comprising the following steps:
step 1, carbon fiber cloth treatment: placing the pretreated carbon fibers in a metal salt catalyst solution, soaking for 1-10 h, taking out, placing in a 60-100 ℃ oven, and drying for 5-24 h;
step 2, powder mixing: mixing SiO 2 Mixing Si and C powder according to the mass ratio of 1: 0.1-0.5: 0.3-0.7, grinding the mixture in a planetary ball mill at 150-200 rpm for 12-24 h to obtain mixed uniform powder, taking out the mixed uniform powder, and drying the mixed uniform powder in an oven at 60-100 ℃ for 5-12 h;
step 3, directionally synthesizing the SiC nanowires on the surface of the carbon fiber cloth: putting the powder obtained in the step (2) into a graphite crucible, arranging the dried carbon fiber impregnated with metal salt on the top of the graphite crucible, wherein the distance between the dried carbon fiber and the bottom of the crucible is 1-5 cm, putting the graphite crucible into an atmosphere sintering furnace, vacuumizing, and controlling the vacuum degree of the atmosphere sintering furnace to be 0.1-0.4 Pa; then filling argon 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 the heating rate of 5-20 ℃/min, preserving the heat at the temperature for 1-10 h, then stopping heating, cooling to room temperature along with the furnace, and opening the furnace to obtain the SiC nanowire array directionally grown on the surface of the carbon fiber cloth.
3. The method of claim 2, wherein: the carbon fiber cloth pretreatment is to wash the carbon fiber cloth with deionized water, absolute ethyl alcohol and acetone respectively, and to dry the carbon fiber cloth in an oven at 60-100 ℃ for 8-24 hours.
4. The method of claim 2, wherein: the metal salt solution includes but is not limited to: ferric nitrate, cobalt nitrate, nickel nitrate, ferrous sulfate, cobalt sulfate, nickel sulfate, ferric chloride, cobalt chloride or nickel chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210661138.0A CN115058885B (en) | 2022-06-13 | 2022-06-13 | Carbon fiber cloth surface orientation SiC nanowire array and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210661138.0A CN115058885B (en) | 2022-06-13 | 2022-06-13 | Carbon fiber cloth surface orientation SiC nanowire array and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115058885A true CN115058885A (en) | 2022-09-16 |
| CN115058885B CN115058885B (en) | 2024-01-30 |
Family
ID=83200017
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210661138.0A Active CN115058885B (en) | 2022-06-13 | 2022-06-13 | Carbon fiber cloth surface orientation SiC nanowire array and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115058885B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819102A (en) * | 2022-12-10 | 2023-03-21 | 西北工业大学 | C f Oriented SiCNWs @ VGNs micro-nano multi-scale strengthening and toughening carbon-based composite material and preparation method thereof |
| CN116003164A (en) * | 2022-12-16 | 2023-04-25 | 西北工业大学 | Method for improving binding force between C/C composite material matrix and SiC coating |
| CN116396091A (en) * | 2023-04-07 | 2023-07-07 | 西北工业大学 | High-strength and high-heat-conductivity ablation-resistant ceramic gradient modified C/C composite material and preparation method thereof |
| CN116715533A (en) * | 2023-08-11 | 2023-09-08 | 西南交通大学 | Preparation method of carbon fiber reinforced pantograph slide plate for growing silicon carbide nanowire |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050077678A (en) * | 2004-01-30 | 2005-08-03 | 한국과학기술연구원 | Synthesis method of sic nanorod and nanowire |
| US20080038520A1 (en) * | 2005-12-29 | 2008-02-14 | Nanosys, Inc. | Methods for oriented growth of nanowires on patterned substrates |
| CN102126859A (en) * | 2011-03-03 | 2011-07-20 | 西北工业大学 | Method for preparing bamboo-shaped SiC nanowire-toughened HfC ceramic |
| CN102491332A (en) * | 2011-11-15 | 2012-06-13 | 西北工业大学 | Method for preparing SiC nanobelts on SiC ceramic surface |
| CN102828249A (en) * | 2012-04-27 | 2012-12-19 | 中国人民解放军第二炮兵工程学院 | Method for preparing monocrystalline silicon carbide nano-wires on flexible carbon fiber substrate |
| CN106544642A (en) * | 2016-10-19 | 2017-03-29 | 张家港市东大工业技术研究院 | A kind of method that utilization microwave method prepares silicon carbide nanometer line thin film |
| CN107059129A (en) * | 2017-04-05 | 2017-08-18 | 西北工业大学 | Co-precipitation and the preparation method of thermal evaporation techniques fabricated in situ taper SiC whiskers |
| CN107128926A (en) * | 2017-06-28 | 2017-09-05 | 湖南大学 | A kind of preparation method of self-supporting Carbide-derived carbons nano wire |
| CN107602154A (en) * | 2017-08-08 | 2018-01-19 | 华南理工大学 | A kind of string-of-pearls-like SiC/SiO2Heterojunction structure and its synthetic method |
| CN112614705A (en) * | 2020-11-03 | 2021-04-06 | 宁波工程学院 | Preparation method of zigzag nitrogen-doped SiC nanowires growing on carbon fiber cloth |
| US20210114940A1 (en) * | 2019-10-16 | 2021-04-22 | Northwestern Polytechnical University | Process for the preparation of a ceramic nanowire preform |
-
2022
- 2022-06-13 CN CN202210661138.0A patent/CN115058885B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050077678A (en) * | 2004-01-30 | 2005-08-03 | 한국과학기술연구원 | Synthesis method of sic nanorod and nanowire |
| US20080038520A1 (en) * | 2005-12-29 | 2008-02-14 | Nanosys, Inc. | Methods for oriented growth of nanowires on patterned substrates |
| CN102126859A (en) * | 2011-03-03 | 2011-07-20 | 西北工业大学 | Method for preparing bamboo-shaped SiC nanowire-toughened HfC ceramic |
| CN102491332A (en) * | 2011-11-15 | 2012-06-13 | 西北工业大学 | Method for preparing SiC nanobelts on SiC ceramic surface |
| CN102828249A (en) * | 2012-04-27 | 2012-12-19 | 中国人民解放军第二炮兵工程学院 | Method for preparing monocrystalline silicon carbide nano-wires on flexible carbon fiber substrate |
| CN106544642A (en) * | 2016-10-19 | 2017-03-29 | 张家港市东大工业技术研究院 | A kind of method that utilization microwave method prepares silicon carbide nanometer line thin film |
| CN107059129A (en) * | 2017-04-05 | 2017-08-18 | 西北工业大学 | Co-precipitation and the preparation method of thermal evaporation techniques fabricated in situ taper SiC whiskers |
| CN107128926A (en) * | 2017-06-28 | 2017-09-05 | 湖南大学 | A kind of preparation method of self-supporting Carbide-derived carbons nano wire |
| CN107602154A (en) * | 2017-08-08 | 2018-01-19 | 华南理工大学 | A kind of string-of-pearls-like SiC/SiO2Heterojunction structure and its synthetic method |
| US20210114940A1 (en) * | 2019-10-16 | 2021-04-22 | Northwestern Polytechnical University | Process for the preparation of a ceramic nanowire preform |
| CN112614705A (en) * | 2020-11-03 | 2021-04-06 | 宁波工程学院 | Preparation method of zigzag nitrogen-doped SiC nanowires growing on carbon fiber cloth |
Non-Patent Citations (2)
| Title |
|---|
| HONGFEI GAO等: "Oxidation simulation study of silicon carbide nanowires: A carbon-rich interface state", 《APPLIED SURFACE SCIENCE》, no. 439, pages 882 - 888, XP085944738, DOI: 10.1016/j.apsusc.2019.07.016 * |
| 朱奇妙;陈建军;吴仁兵;李宝生;潘颐;: "针尖状SiC纳米线的合成与机理分析", 材料科学与工程学报, vol. 27, no. 03, pages 361 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819102A (en) * | 2022-12-10 | 2023-03-21 | 西北工业大学 | C f Oriented SiCNWs @ VGNs micro-nano multi-scale strengthening and toughening carbon-based composite material and preparation method thereof |
| CN116003164A (en) * | 2022-12-16 | 2023-04-25 | 西北工业大学 | Method for improving binding force between C/C composite material matrix and SiC coating |
| CN116003164B (en) * | 2022-12-16 | 2024-01-30 | 西北工业大学 | Method for improving binding force between C/C composite material matrix and SiC coating |
| CN116396091A (en) * | 2023-04-07 | 2023-07-07 | 西北工业大学 | High-strength and high-heat-conductivity ablation-resistant ceramic gradient modified C/C composite material and preparation method thereof |
| CN116715533A (en) * | 2023-08-11 | 2023-09-08 | 西南交通大学 | Preparation method of carbon fiber reinforced pantograph slide plate for growing silicon carbide nanowire |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115058885B (en) | 2024-01-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN115058885B (en) | Carbon fiber cloth surface orientation SiC nanowire array and preparation method thereof | |
| US20210114940A1 (en) | Process for the preparation of a ceramic nanowire preform | |
| CN110256082B (en) | Method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material by reaction sintering | |
| CN108285355B (en) | Method for preparing SiC nanowire reinforced reaction sintered silicon carbide ceramic matrix composite | |
| CN105543598B (en) | Preparation method of reinforced magnesium matrix composite | |
| CN107721429B (en) | Zirconium carbide-silicon carbide composite powder material and preparation method thereof | |
| CN108033801A (en) | Silicon nitride nanowire reinforced porous silicon nitride composite material and preparation method thereof | |
| CN101104515A (en) | SiC nano-wire and preparing method thereof | |
| CN104451957B (en) | Low density SiC nanofiber and its preparation method | |
| CN108129151B (en) | Graphene/silicon carbide nano composite structure monolithic ceramic and preparation method thereof | |
| CN109437203A (en) | A kind of preparation method of high-purity one dimension SiC nano material | |
| CN113718370B (en) | Preparation method of hollow silicon carbide fiber | |
| CN106784667A (en) | A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof | |
| CN110668447B (en) | Synthesis method of silicon carbide nanowire | |
| CN115745643A (en) | Carbon nanotube modified composite material and preparation method thereof | |
| CN1861521A (en) | Synthesis process of needle shape nano silicon carbide | |
| CN104446501A (en) | Preparation method of silicon nitride ceramic fiber | |
| CN110042468A (en) | A kind of preparation method of micrometer silicon carbide zirconium whisker | |
| CN115259159B (en) | Inverted cone-shaped nitrogen doped silicon carbide nanowire with high length-diameter ratio and preparation method thereof | |
| CN111484017A (en) | Method for preparing SiC nanoparticles based on silica microspheres @ C | |
| CN111533131B (en) | Based on CaCl2Preparation method of nano silicon carbide particles of shape regulator | |
| CN109957859B (en) | Silicon carbide fiber and preparation method thereof | |
| CN112195503B (en) | Method for synthesizing hafnium carbide crystal whisker with large length-diameter ratio by carbothermic reduction method | |
| CN109898179B (en) | Preparation method of titanium carbide fiber material | |
| CN108546142B (en) | CfPreparation method of-HfCnw micro-nano multi-scale strengthening and toughening carbon-based composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |