CN114436660A - Preparation method of carbon nano tube-ceramic composite membrane - Google Patents
Preparation method of carbon nano tube-ceramic composite membrane Download PDFInfo
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- CN114436660A CN114436660A CN202210160899.8A CN202210160899A CN114436660A CN 114436660 A CN114436660 A CN 114436660A CN 202210160899 A CN202210160899 A CN 202210160899A CN 114436660 A CN114436660 A CN 114436660A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 239000000919 ceramic Substances 0.000 title claims abstract description 50
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000012528 membrane Substances 0.000 title claims abstract description 10
- 239000002238 carbon nanotube film Substances 0.000 claims abstract description 67
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 19
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 18
- 239000002041 carbon nanotube Substances 0.000 claims description 14
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 14
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 9
- 239000000853 adhesive Substances 0.000 claims description 9
- 230000001070 adhesive effect Effects 0.000 claims description 9
- 229910052709 silver Inorganic materials 0.000 claims description 9
- 239000004332 silver Substances 0.000 claims description 9
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 9
- 238000001723 curing Methods 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004132 cross linking Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000002048 multi walled nanotube Substances 0.000 claims 2
- 239000002109 single walled nanotube Substances 0.000 claims 2
- 230000000087 stabilizing effect Effects 0.000 claims 2
- 238000013007 heat curing Methods 0.000 claims 1
- 238000007711 solidification Methods 0.000 claims 1
- 230000008023 solidification Effects 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 125000000962 organic group Chemical group 0.000 abstract description 4
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- 238000006243 chemical reaction Methods 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
- C04B35/515—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
- C04B35/565—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 based on silicon carbide
- C04B35/573—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 based on silicon carbide obtained by reaction sintering or recrystallisation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
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- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
Abstract
The invention discloses a preparation method of a carbon nano tube-ceramic composite membrane. According to the invention, the polycarbosilane is rapidly cured in situ in a manner of consuming skeleton carbon by using Joule heat spontaneously generated by electrifying the carbon nanotube film, and is used as a precursor of the silicon carbide ceramic. Sintering at higher joule heating temperature to remove organic group from polycarbosilane and convert it into silicon carbide to obtain the carbon nanotube-ceramic composite film. The invention is characterized in that: the traditional muffle furnace heating is replaced by the Joule heat high temperature generated by electrifying the carbon nano tube film with the ultra-fast temperature rise and temperature drop characteristics (> 500 ℃/s). Therefore, the whole treatment process has the characteristics of low energy consumption and short time, and a new method is provided for quickly preparing the high-performance carbon-based composite material.
Description
Technical Field
The invention belongs to the field of composite material preparation, and particularly relates to a method for quickly preparing a carbon nano tube-ceramic composite film with excellent comprehensive performance based on an ultrafast response joule heat high temperature.
Background
The carbon-based composite material generally has the advantages of high strength, high modulus, light specific gravity, corrosion resistance, thermal shock resistance, friction resistance, good chemical stability and the like, and is widely applied to the fields of aerospace and the like. As an advanced engineering material, the performance of carbon-based composites depends to a large extent on the manufacturing process. The preparation process of the traditional carbon-based composite material is generally long in period, high in cost, harsh in process temperature, quite complex in process reaction, and particularly high in energy consumption and long in time in the high-temperature treatment stage. This is mainly due to the fact that conventional resistive heat source devices are generally large in size and weight, require high voltage and high energy consumption during operation, and have generally low temperature rise and fall rates (< 100 ℃/min). For example, the conventional preparation method of the carbon nanotube composite material mainly comprises liquid phase mixing and object infiltration, and is assisted with an external heat source and high pressure to promote the uniformity and densification treatment of the carbon nanotube composite material, so that the efficiency and the cost are high in industrial production, and the development and the application of the high-performance carbon-based composite material are limited. Particularly, when the heating treatment is carried out at a high temperature of more than 1000 ℃, the heating and cooling of the traditional muffle furnace heating method takes a lot of time, which brings great inconvenience to the industrial production.
On the other hand, a macroscopic assembly structure (film, fiber and the like) of a carbon-based material such as a carbon nanotube has a very high joule heating temperature response rate (> 500 ℃/second) and a very high withstand temperature (under an inert atmosphere-3000 ℃) and can be prepared into various required shapes according to actual needs. Compared with the traditional metal and ceramic joule heating materials, the material also has the advantages of lighter weight, more flexibility, better chemical corrosion resistance and the like. Therefore, the carbon nanotube-based high-temperature composite material prepared by utilizing the self-ultrafast joule heat high-temperature response characteristic has important application value.
Disclosure of Invention
The invention provides a method for preparing a carbon-based composite material based on a joule heat high temperature of ultra-fast response of a carbon nano tube film, which aims to make up for the defects of the prior art and quickly obtain the composite material needing high-temperature synthesis.
The invention solves the technical problems by the following scheme:
the composite film material is prepared by using carbon nanotube film as substrate, utilizing joule heat produced by carbon nanotube itself and its carbon-containing skeleton to crosslink and solidify polycarbosilane loaded on the surface of the film, and high temperature sintering.
A preparation method of a carbon nano tube-ceramic composite membrane comprises the following steps:
(1) pretreatment of the carbon nanotube film: cutting the carbon nano tube film into a required size, soaking the carbon nano tube film in concentrated nitric acid to remove impurities in the film, then washing the film for a plurality of times by using deionized water and alcohol, and drying the film.
(2) Curing of polycarbosilane: leaving a part of bonding electrodes at two ends of the carbon nanotube film, uniformly coating a layer of polycarbosilane on two surfaces of the rest middle part, electrifying the film by an external power supply of the electrodes, and crosslinking and curing the coated polycarbosilane by using the self-joule heat high temperature of the film.
(3) Preparing silicon carbide ceramic: and (3) after the polycarbosilane is cured in the step (2), continuing to increase the voltage to increase the temperature of the Joule heat generated by the film, and preserving the heat for a certain time to sinter and ceramize the cured polycarbosilane, thus preparing the required carbon nanotube-ceramic composite material.
The carbon nanotube film substrates with different lengths and widths can be selected according to specific requirements, and appropriate external power supply conditions are matched.
Wherein the crosslinking curing time in the step (2) is 1-10 minutes, and the curing temperature is 200-600 ℃.
Wherein the ceramic sintering temperature in the step (3) is 900-.
As a preferred technical scheme, the specific processes of the steps (2) and (3) are as follows: reserving parts with the length of 5mm at two ends of the processed carbon nano tube film respectively, and dripping polycarbosilane diluted by tetrahydrofuran on the other surfaces. And horizontally suspending the carbon nanotube film covered with the polycarbosilane, and drying in an air-blast drying oven. And adhering the dried carbon nanotube film covered with the polycarbosilane on a sample rack in a joule heating furnace through conductive silver adhesive, and then starting a vacuum pump to pump the cavity to a certain vacuum degree and connect a direct current power supply. The surface temperature of the carbon nano tube film is rapidly raised to 250 ℃ by controlling the voltage, and the polycarbosilane is crosslinked and cured by keeping the temperature for 5 minutes. And continuously increasing the voltage to the cured carbon nanotube film to enable the surface temperature of the carbon nanotube film to reach 900 ℃, and keeping the voltage constant for 5 minutes to obtain the required carbon nanotube-ceramic composite film material.
As a preferred technical scheme, the specific processes of the steps (2) and (3) are as follows: reserving parts with the length of 5mm at two ends of the processed carbon nano tube film respectively, and dripping polycarbosilane diluted by tetrahydrofuran on the other surfaces. And horizontally suspending the carbon nanotube film covered with the polycarbosilane, and drying in an air-blast drying oven. And adhering the dried carbon nanotube film covered with the polycarbosilane on a sample rack in a joule heating furnace through conductive silver adhesive, and then starting a vacuum pump to pump the cavity to a certain vacuum degree and connect a direct current power supply. The surface temperature of the carbon nano tube film is stabilized at 400 ℃ by controlling the voltage, and the polycarbosilane is crosslinked and cured by keeping the temperature for 2 minutes. And continuously increasing the voltage to the cured carbon nanotube film to ensure that the surface temperature of the carbon nanotube film reaches 1200 ℃, and keeping the constant voltage for 2 minutes to obtain the required carbon nanotube-ceramic composite film material.
As a preferred technical scheme, the specific processes of the steps (2) and (3) are as follows: reserving parts with the length of 5mm at two ends of the processed carbon nano tube film respectively, and dripping polycarbosilane diluted by tetrahydrofuran on the other surfaces. And horizontally suspending the carbon nano tube film covered with the polycarbosilane in the air and placing the carbon nano tube film in the air blast drying box for drying. And adhering the dried carbon nanotube film covered with the polycarbosilane on a sample rack in a joule heating furnace through conductive silver adhesive, and then starting a vacuum pump to pump the cavity to a certain vacuum degree and connect a direct current power supply. The surface temperature of the carbon nano tube film is stabilized at 600 ℃ by controlling the voltage, and the polycarbosilane is crosslinked and cured after heat preservation for 1 minute. And continuously increasing the voltage on the cured carbon nanotube film to ensure that the surface temperature of the carbon nanotube film reaches 1500 ℃, and keeping the constant voltage for 1 minute to obtain the required carbon nanotube-ceramic composite film material.
The beneficial technical effects which can be realized by the invention at least comprise: the traditional muffle furnace heating, crosslinking, curing and ceramic sintering process is replaced by the Joule heat high temperature generated by electrifying the carbon nano tube film with the characteristics of rapid heating and cooling. Therefore, the whole preparation process has the characteristics of short time and low energy consumption, and can realize the rapid low-cost preparation of large-batch carbon nanotube composite materials. In addition, the method takes the carbon nano tube as a matrix to prepare the composite carbon nano tube material with the surface uniformly covered with the silicon carbide, and can greatly enhance the comprehensive mechanical property and the thermal property of the material.
Drawings
FIG. 1 is a flow chart of the preparation of the carbon nanotube-ceramic composite membrane based on ultrafast Joule thermal temperature response according to the present invention.
FIG. 2 is a voltage-temperature response curve of the carbon nanotube-ceramic composite film according to the present invention.
Fig. 3 is a scanning electron microscope image of the carbon nanotube-ceramic composite film prepared in example 1 of the present invention.
Fig. 4 is an XPS chart of the carbon nanotube-ceramic composite film prepared in example 1 of the present invention.
Fig. 5 is a photograph showing a real object of the carbon nanotube-ceramic composite film according to example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be fully described below with reference to the accompanying drawings. Obviously, the described embodiment is only a part of the operation example of the present invention, and other embodiments obtained by those skilled in the art without any inventive work are within the protection scope of the present invention based on the embodiment of the present invention.
Example 1
The invention relates to a preparation method of a carbon nano tube-ceramic composite film, which utilizes joule heat generated by electrifying a carbon nano tube film to quickly solidify polycarbosilane in situ in a mode of consuming framework carbon, further takes the polycarbosilane as a precursor of silicon carbide ceramic, and removes organic groups of the polycarbosilane to convert the polycarbosilane into silicon carbide at higher spontaneous joule heat temperature so as to obtain the carbon nano tube composite film material of the surface modified silicon carbide ceramic.
A preparation method of a carbon nano tube-ceramic composite membrane specifically comprises the following steps:
firstly, cutting a carbon nanotube film with the length of 3 cm and the width of 2 cm, soaking the carbon nanotube film in a beaker by concentrated nitric acid for 24 hours to clean catalyst particles and the like in the film, so that the film has a more compact structure and higher conductivity; then washed repeatedly with deionized water to neutrality. Two ends of the treated film are reserved with parts with the length of 5mm respectively, and polycarbosilane (40 wt%) diluted by tetrahydrofuran is dripped on the other surfaces, and 20 mu l of the polycarbosilane is dripped per square centimeter. And horizontally suspending the carbon nanotube film coated with the polycarbosilane, and drying in an air-blast drying oven. Adhering the dried film on a sample holder in a joule heating furnace via conductive silver adhesive, starting a vacuum pump, and pumping the furnace chamber to 10 deg.C-2Pa vacuum degree and connecting a direct current power supply. And controlling the voltage to stabilize the surface temperature of the film at 250 ℃, and keeping the temperature for 5 minutes to crosslink the polycarbosilane. And continuously increasing the voltage to the crosslinked composite film to ensure that the surface temperature of the crosslinked composite film reaches 900 ℃, and keeping the constant voltage for 5 minutes to obtain the carbon nano tube-ceramic composite film material.
Example 2
The invention relates to a preparation method of a carbon nano tube-ceramic composite film, which utilizes joule heat generated by electrifying a carbon nano tube film to quickly solidify polycarbosilane in situ in a mode of consuming framework carbon, further takes the polycarbosilane as a precursor of silicon carbide ceramic, and removes organic groups of the polycarbosilane to convert the polycarbosilane into silicon carbide at higher spontaneous joule heat temperature so as to obtain the carbon nano tube composite film material of the surface modified silicon carbide ceramic.
A preparation method of a carbon nano tube-ceramic composite membrane specifically comprises the following steps:
firstly, cutting a carbon nanotube film with the length of 3 cm and the width of 2 cm, soaking the carbon nanotube film in a beaker by concentrated nitric acid for 24 hours to clean catalyst particles and the like in the film, so that the film has a more compact structure and higher conductivity; then washed repeatedly with deionized water to neutrality. At each end of the treated filmA5 mm long portion was reserved, and polycarbosilane (40 wt%) diluted with tetrahydrofuran was dropped onto the remaining surface in an amount of 20. mu.l per square centimeter. And horizontally suspending the carbon nanotube film coated with the polycarbosilane, and drying in an air-blast drying oven. Adhering the dried film on a sample holder in a joule heating furnace via conductive silver adhesive, starting a vacuum pump, and pumping the furnace chamber to 10 deg.C-2Pa vacuum degree and connecting a direct current power supply. And controlling the voltage to stabilize the surface temperature of the film at 400 ℃, and keeping the temperature for 2 minutes to crosslink the polycarbosilane. And continuously increasing the voltage to the crosslinked composite film to ensure that the surface temperature of the crosslinked composite film reaches 900 ℃, and keeping the constant voltage for 2 minutes to obtain the carbon nano tube-ceramic composite film material.
Example 3
The invention relates to a preparation method of a carbon nano tube-ceramic composite film, which utilizes joule heat generated by electrifying a carbon nano tube film to quickly solidify polycarbosilane in situ in a mode of consuming framework carbon, further takes the polycarbosilane as a precursor of silicon carbide ceramic, and removes organic groups of the polycarbosilane to convert the polycarbosilane into silicon carbide at higher spontaneous joule heat temperature so as to obtain the carbon nano tube composite film material of the surface modified silicon carbide ceramic.
A preparation method of a carbon nano tube-ceramic composite membrane specifically comprises the following steps:
firstly, cutting a carbon nanotube film with the length of 3 cm and the width of 2 cm, soaking the carbon nanotube film in a beaker by concentrated nitric acid for 24 hours to clean catalyst particles and the like in the film, so that the film has a more compact structure and higher conductivity; then washed repeatedly with deionized water to neutrality. Two ends of the treated film are reserved with parts with the length of 5mm respectively, and polycarbosilane (40 wt%) diluted by tetrahydrofuran is dripped on the other surfaces, and 20 mu l of the polycarbosilane is dripped per square centimeter. And horizontally suspending the carbon nanotube film coated with the polycarbosilane, and drying in an air-blast drying oven. Adhering the dried film on a sample holder in a joule heating furnace via conductive silver adhesive, starting a vacuum pump, and pumping the furnace chamber to 10 deg.C-2Pa vacuum degree and connecting a direct current power supply. And controlling the voltage to stabilize the surface temperature of the film at 600 ℃, and keeping the temperature for 1 minute to crosslink the polycarbosilane. Continuously increasing voltage to the crosslinked composite filmThe surface temperature of the carbon nano tube is kept at 1500 ℃, and the constant voltage is kept for 1 minute, thus obtaining the carbon nano tube-ceramic composite membrane material.
Compared with the preparation process of other carbon-based ceramic composite materials, the preparation method disclosed by the invention has the advantages that the traditional muffle furnace heating is replaced by the joule heat high-temperature process generated by electrifying the carbon nanotube film, the characteristics of rapid temperature rise and temperature drop are realized, the time of the whole preparation process is short, the energy consumption is low, no pollution is caused, and the rapid low-cost preparation of large-batch carbon-based ceramic composite materials can be realized on the premise of environmental friendliness.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A preparation method of a carbon nano tube-ceramic composite membrane is characterized by comprising the following steps: in the preparation process of the material, polycarbosilane is used as a precursor, and a layer of silicon carbide is prepared on the surface of the carbon nanotube film by sintering, so that the carbon nanotube composite film with good mechanical property and flexibility is obtained.
2. The method of claim 1, wherein the method comprises the steps of: in the preparation process, the ultra-fast Joule heat high temperature of the carbon nano tube film is used as a heat source and is applied to the fast solidification of polycarbosilane and the fast sintering of a silicon carbide ceramic layer.
3. The method of claim 1, wherein the method comprises: the carbon nanotube is characterized by comprising a single-wall carbon nanotube and a multi-wall carbon nanotube or a composite of the single-wall carbon nanotube and the multi-wall carbon nanotube.
4. The method of claim 1, wherein the method comprises: the method comprises the following steps:
(1) pretreatment of the carbon nanotube film: cutting the carbon nanotube film into a required size, soaking the carbon nanotube film in concentrated nitric acid to remove impurities in the film, washing the film for several times by using deionized water and alcohol, and drying the film;
(2) joule heat curing of polycarbosilane: reserving a part of bonding electrodes at two ends of the carbon nanotube film, uniformly coating a layer of polycarbosilane on two surfaces of the rest middle part, electrifying the film by an external power supply of the electrodes, and crosslinking and curing the coated polycarbosilane by using the self-joule heat high temperature of the film;
(3) preparing silicon carbide ceramic: and (3) after the polycarbosilane is cured in the step (2), continuing to increase the voltage to increase the temperature of the Joule heat generated by the film, and preserving the heat for a certain time to sinter and ceramize the cured polycarbosilane, thus preparing the required carbon nanotube-ceramic composite material.
5. The method of claim 4, wherein the carbon nanotube-ceramic composite film comprises: the curing time in the step (2) is 1-10 minutes, and the curing temperature is 200-600 ℃.
6. The method of claim 4, wherein the carbon nanotube-ceramic composite film comprises: the ceramic sintering temperature in the step (3) is 900-2000 ℃.
7. The method of claim 4, wherein the carbon nanotube-ceramic composite film is prepared by: the preparation method comprises the following specific steps of (2) and (3): reserving parts with the length of 5mm at two ends of the processed carbon nanotube film, dripping polycarbosilane diluted by tetrahydrofuran on the other surfaces of the processed carbon nanotube film, horizontally suspending the carbon nanotube film covered with the polycarbosilane in a blast drying box for drying, adhering the dried carbon nanotube film covered with the polycarbosilane on a sample rack in a joule heating furnace through conductive silver adhesive, then starting a vacuum pump, pumping the cavity to a certain vacuum degree, connecting a direct current power supply, rapidly increasing the surface temperature of the carbon nanotube film to 250 ℃ by controlling voltage, preserving heat for 5 minutes to crosslink and solidify the polycarbosilane, continuously increasing the voltage of the solidified carbon nanotube film to make the surface temperature of the solidified carbon nanotube film reach 900 ℃, and keeping the voltage constant for 5 minutes to obtain the required carbon nanotube-ceramic composite film material.
8. The method of claim 4, wherein the carbon nanotube-ceramic composite film comprises: the preparation method comprises the following steps (2) and (3): reserving parts with the length of 5mm at two ends of the processed carbon nano tube film, dripping polycarbosilane diluted by tetrahydrofuran on the rest surface of the processed carbon nano tube film, horizontally suspending the carbon nano tube film covered with the polycarbosilane in a blast drying box for drying, adhering the dried carbon nano tube film covered with the polycarbosilane on a sample rack in a joule heating furnace through conductive silver adhesive, then starting a vacuum pump, pumping the cavity to a certain vacuum degree, connecting a direct current power supply, stabilizing the surface temperature of the carbon nano tube film at 400 ℃ by controlling voltage, preserving the temperature for 2 minutes to crosslink and solidify the polycarbosilane, continuously increasing the voltage of the solidified carbon nano tube film to ensure that the surface temperature reaches 1200 ℃, and keeping the constant voltage for 2 minutes to obtain the required carbon nano tube-ceramic composite film material.
9. The method of claim 4, wherein the carbon nanotube-ceramic composite film comprises: the preparation method comprises the following specific steps of (2) and (3): reserving parts with the length of 5mm at two ends of the processed carbon nanotube film, dripping polycarbosilane diluted by tetrahydrofuran on the other surfaces of the processed carbon nanotube film, horizontally suspending the carbon nanotube film covered with the polycarbosilane in a blast drying box for drying, adhering the dried carbon nanotube film covered with the polycarbosilane on a sample rack in a joule heating furnace through conductive silver adhesive, then starting a vacuum pump, pumping the cavity to a certain vacuum degree, connecting a direct current power supply, stabilizing the surface temperature of the carbon nanotube film at 600 ℃ by controlling voltage, preserving the temperature for 1 minute to crosslink and solidify the polycarbosilane, continuously increasing the voltage of the solidified carbon nanotube film to enable the surface temperature to reach 1500 ℃, and keeping the constant voltage for 1 minute to obtain the required carbon nanotube-ceramic composite film material.
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