CN109922548A - A kind of carbon-based Electric radiant Heating Film and preparation method thereof - Google Patents
A kind of carbon-based Electric radiant Heating Film and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of carbon-based Electric radiant Heating Films and preparation method thereof, belong to carbon nanomaterial technical field, are related to a kind of preparation of carbon film and its application in field of electric heating.Of the invention is skeleton unit using three-dimensional grapheme, is filling with polyacrylonitrile, final to obtain to be graphitized crystallite as the carbon-based electric-heating thin film of crosslinking agent by hot pressing, pre-oxidation, high temperature cabonization.Different from tradition, self-assembled structures bring anisotropy and the stack effect of graphene film, the electricity of this film, thermal property remain the isotropism of three-dimensional grapheme to a certain extent layer by layer.Meanwhile operating voltage is low, heating rate is fast, is optimal one of the thin-film material of the electric heating property reported at present.
Description
Technical field
The present invention relates to a kind of carbon-based Electric radiant Heating Films and preparation method thereof, belong to carbon nanomaterial technical field, are related to one kind
Carbon film preparation and its field of electric heating application.
Background technique
Coal heating is the long-term main heating system in China, is inevitably generated more pollutants and titanium dioxide
Carbon brings more serious problem of environmental pollution to China.Electric energy is the clean and environmental protection energy, will be played in the following heating field
Very important status.And commonly electric heating system is based on the materials such as resistance wire, metal mesh, by taking nichrome as an example, not only
It is expensive, and density is big, quality is heavy, and electric conversion efficiency is low, it is difficult to process.Therefore, be badly in need of developing a kind of low-density,
Flexibility is good, efficient thermo electric material.
Graphene has excellent mechanics, electricity, thermal property, and density is low, easy processing, corrosion-resistant.These are excellent
Physical property makes it have very high potential in thermo electric material field.Currently, a kind of there are two types of the preparation methods of graphene Electric radiant Heating Film
It is such as glass, PET on a transparent substrate, transparent graphene Electric radiant Heating Film is obtained by the method for chemical vapor deposition, it is main to use
In fields such as removing fog on automobile glass.But this method is at high cost, it is not resistant to bending, can not large area preparation.Another method be by
Macromolecule resin and graphene powder are mixed into slurry, by the methods of printing, spraying film forming.This Electric radiant Heating Film structural homogeneity
Poor, fever is unevenly, electric conversion efficiency is low, cannot embody the intrinsic thermoelectricity capability of graphene film.It is superb et al. to have invented one
Kind intercalated graphite alkene Electric radiant Heating Film, operating voltage is higher, and electric conversion efficiency is lower, and temperature rate is slower.Liu Juan et al. invention
A kind of graphene Electric radiant Heating Film of 36V operating voltage, operating voltage is higher, and does not provide the electric conversion ginseng of Electric radiant Heating Film
Number.
Summary of the invention
Technology of the invention solves the problems, such as: overcome the deficiencies in the prior art, proposes a kind of carbon-based Electric radiant Heating Film and its preparation
Method, the carbon-based Electric radiant Heating Film are filling with polyacrylonitrile, by hot pressing, pre-oxidation, high temperature using three-dimensional grapheme as skeleton unit
Carbonization, it is final to obtain to be graphitized crystallite as the carbon-based electric-heating thin film of crosslinking agent, it is different from tradition self-assembled structures band layer by layer
The stack effect of the anisotropy and graphene film come, the electricity of this film, thermal property remain three-dimensional stone to a certain extent
The isotropism of black alkene.Meanwhile operating voltage is low, heating rate is fast, and under 1.75V voltage, temperature may be up to 235 DEG C, is
Optimal one of the thin-film material of the electric heating property reported at present.In addition, excellent electric heating circulating performance makes it under bending state
It can operate in harsh environment.
The technical solution of the invention is as follows:
A kind of carbon-based Electric radiant Heating Film, the raw material of the carbon-based Electric radiant Heating Film include three-dimensional grapheme and polyacrylonitrile, three-dimensional grapheme
For skeleton unit, polyacrylonitrile is filled in the skeleton of three-dimensional grapheme；
The composition of carbon-based Electric radiant Heating Film includes three-dimensional grapheme and graphite microcrystal, and three-dimensional grapheme and graphite microcrystal are crosslinking knot
Structure；
Carbon-based Electric radiant Heating Film with a thickness of 10 μm~500 μm；
Carbon-based Electric radiant Heating Film has good tensile property and bending property；
Carbon-based Electric radiant Heating Film has height than heating rate, high to be not less than 213 DEG C of s-1V-1 than heating rate；
Carbon-based Electric radiant Heating Film has low-work voltage, can work in 10V or less.
A kind of the step of preparation method of carbon-based Electric radiant Heating Film, this method includes:
Graphene oxide and the first organic solvent are mixed, and stirred by the first step, are obtained after mixing evenly uniformly molten
Then obtained solution is carried out solvent thermal reaction by liquid in a high pressure reaction kettle；
Second step, the product that the first step is obtained and water carry out exchange of solvent, are freeze-dried after the completion of exchange of solvent；
The product that second step obtains is heated under inert atmosphere or vacuum condition, obtains three-dimensional by third step
Porous graphene skeleton structure；
Polyacrylonitrile long-chain molecule and the second organic solvent are mixed, and stirred by the 4th step, obtain homogeneous solution；
5th step, the three-dimensional porous graphene skeleton structure that third step is obtained, which is added in the solution that the 4th step obtains, to be made
Polyacrylonitrile long-chain molecule is filled in three-dimensional grapheme hole, dry after the completion of filling, and it is compound to obtain graphene/polyacrylonitrile
Material；
Graphene/polyacrylonitrile composite material that 5th step obtains is carried out hot pressing in a mold, obtains graphite by the 6th step
Alkene/polyacrylonitrile composite material film；
7th step pre-oxidizes graphene/polyacrylonitrile composite material film that the 6th step obtains in tube furnace,
It further under Ar protective atmosphere, is carbonized, obtains carbon-based Electric radiant Heating Film.
In the first step, the first organic solvent is ethyl alcohol, acetone, tetrahydrofuran or n,N-Dimethylformamide, oxygen
The concentration of graphite alkene is 0.375~10mg/mL, and solvent thermal reaction temperature is 130-250 DEG C.
The advantages of graphene oxide is dispersed using the first organic solvent are as follows: prepared using organic solvent as dispersion liquid
Three-dimensional grapheme, graphene element stack is seldom in microstructure, is that the graphene film of single layer or few layer is crosslinked shape with chemical bond
At network structure, ensure that the intrinsic structure and performance of graphene.
In the third step, heat treatment temperature is 200~1000 DEG C, heating treatment time 30-300min；
In 4th step, the second organic solvent is n,N-Dimethylformamide, n,N-dimethylacetamide, dimethyl
One or more of sulfoxide, ethylene carbonate, N-methyl pyrrolidones are mixed according to arbitrary proportion；Polyacrylonitrile long-chain
The molecular weight of molecule is 5~200,000；
In 5th step, the mass ratio of three-dimensional porous graphene skeleton structure and polyacrylonitrile long-chain molecule is 10:
10~90；Advantage is: the graphite microcrystal crystallite dimension after the polyacrylonitrile carbonization of higher molecular weight is larger, and defect is less；Poly- third
On the one hand the number of alkene nitrile can be filled up completely the hole of three-dimensional grapheme, can be formed with three-dimensional grapheme after being on the one hand carbonized
Cross-linked structure forms three-dimensional conductive, passage of heat；
In 6th step, hot pressing temperature is 25~150 DEG C, and hot pressing pressure is 19~500Pa；Mold be diameter 10~
The circular die of 100mm.According to different demands, mold can be made the arbitrary shapes such as rectangle, square.Different hot pressing pressures and
The advantages of temperature, is: can guarantee the thermoplasticity of polyacrylonitrile precursor, and then guarantee its cause with three-dimensional graphene composite material
Close property；
In 7th step, Pre oxidation is 250~320 DEG C, and carburizing temperature is 800~3000 DEG C.
In the third step, obtained three-dimensional grapheme is as the starting material advantage for preparing electric-heating thin film are as follows: with biography
System LBL self-assembly preparation method is compared, and three-dimensional grapheme effectively prevents the stacking in graphene film forming procedure to act on, centainly
The electricity of film, thermal property is set to maintain the isotropism of three-dimensional grapheme in degree.
Beneficial effect
(1) of the invention using three-dimensional grapheme is skeleton unit, is filling with polyacrylonitrile, by hot pressing, pre-oxidation,
High temperature cabonization, it is final to obtain to be graphitized crystallite as the carbon-based electric-heating thin film of crosslinking agent.Different from traditional LBL self-assembly knot
The stack effect of structure bring anisotropy and graphene film, the electricity of this film, thermal property remain three to a certain extent
Tie up the isotropism of graphene.Meanwhile operating voltage is low, heating rate is fast, is optimal thin of the electric heating property reported at present
One of membrane material.
(2) Electric radiant Heating Film operating voltage of the invention is low, and heating rate is fast, and flexibility is good, can use under harsh environment.
It can be used for the fields such as domestic heating, building heating, aircraft deicing, have the effect of clean and environmental protection, energy saving.
Detailed description of the invention
Fig. 1 a is the tensile stress strain curve of Electric radiant Heating Film；
Fig. 1 b is Electric radiant Heating Film resistance change rate under different curvature radius；
Fig. 2 be under certain curvature radius, under 1V voltage, the bend cycles stability of electric-heating thin film；
Fig. 3 is the temperature to cool down after carbon-based Electric radiant Heating Film heats up and powers off at 0.88V, 1.13V, 1.30V, 1.61V voltage
Curve graph.
Specific embodiment
Below in conjunction with specific case study on implementation, the present invention is further described, but protection scope of the present invention is not limited to
Content described in case study on implementation.
Embodiment 1
It weighs 60mg graphene oxide to be dispersed in 60mL ethyl alcohol, stirring is uniformly dispersed for 1 hour, and obtained dispersion liquid is fallen
Enter in 100mL polytetrafluoro reaction kettle, is reacted 12 hours at 150 DEG C.
Obtained graphite ene product is subjected to solvent displacement, ethyl alcohol is all replaced as water, is freeze-dried later.
Dry graphene skeleton is placed in tube furnace and is annealed 1 hour at 800 DEG C of temperature.
The polyacrylonitrile that 20mg molecular weight is 150,000 is weighed in 10ml n,N-Dimethylformamide, 50 DEG C is heated to, stirs
Dissolution is mixed, 20mg three-dimensional grapheme is put into solution, is allowed to uniformly mixed.It is compound that polyacrylonitrile/graphene is obtained after drying
Object.
It is warm by above-mentioned compound as hot pressing 3 hours, pressure 100Pa in the round stainless steel mould that diameter is 40mm
Degree is 100 DEG C.
By above-mentioned heat pressure film as in tube furnace, 6 hours, Pre oxidation 270 are pre-oxidized in air atmosphere
℃.Further, it is carbonized under an ar atmosphere 6 hours, carburizing temperature is 800 DEG C, finally obtains carbon-based Electric radiant Heating Film.Film thickness
It is 16 μm, density 0.92mg/cm3。
Bendability and electric heating property test are carried out to obtained carbon-based Electric radiant Heating Film, as a result such as Fig. 1 a, Fig. 1 b Fig. 2 and Fig. 3 institute
Show, as shown in Figure 1, the tensile strength 50MPa of this Electric radiant Heating Film shows the electricity of very little when radius of curvature is 10~26mm
Resistive illustrates the tensile property and bending property of film.As shown in Figure 2 under 1V voltage, electric heating property is shown very well
Bend cycles stability.As shown in Figure 3 as voltage increases, saturation temperature is gradually risen, under different voltages, Electric radiant Heating Film
It can be quickly raised to saturation temperature.
Embodiment 2
It weighs 60mg graphene oxide to be dispersed in 60mL ethyl alcohol, stirring is uniformly dispersed for 1 hour, and obtained dispersion liquid is fallen
Enter in 100mL polytetrafluoro reaction kettle, is reacted 12 hours at 180 DEG C.
Obtained graphite ene product is subjected to solvent displacement, ethyl alcohol is all replaced as water, is freeze-dried later.
Dry graphene skeleton is placed in tube furnace and is annealed 1 hour at 1000 DEG C of temperature.
The polyacrylonitrile that 30mg molecular weight is 150,000 is weighed in 10ml n,N-Dimethylformamide, 50 DEG C is heated to, stirs
Dissolution is mixed, 20mg three-dimensional grapheme is put into solution, is allowed to uniformly mixed.It is compound that polyacrylonitrile/graphene is obtained after drying
Object.
It is warm by above-mentioned compound as hot pressing 3 hours, pressure 120Pa in the round stainless steel mould that diameter is 40mm
Degree is 150 DEG C.
By above-mentioned heat pressure film as in tube furnace, 6 hours, Pre oxidation 270 are pre-oxidized in air atmosphere
℃.Further, it is carbonized under an ar atmosphere 6 hours, carburizing temperature is 800 DEG C, finally obtains carbon-based Electric radiant Heating Film.Film thickness
For 20um, density 0.95mg/cm3。
Embodiment 3
It weighs 90mg graphene oxide to be dispersed in 60mL ethyl alcohol, stirring is uniformly dispersed for 1 hour, and obtained dispersion liquid is fallen
Enter in 100mL polytetrafluoro reaction kettle, is reacted 12 hours at 150 DEG C.
Obtained graphite ene product is subjected to solvent displacement, ethyl alcohol is all replaced as water, is freeze-dried later.
Dry graphene skeleton is placed in tube furnace and is annealed 1 hour at 800 DEG C of temperature.
The polyacrylonitrile that 50mg molecular weight is 150,000 is weighed in 10ml n,N-Dimethylformamide, 50 DEG C is heated to, stirs
Dissolution is mixed, 20mg three-dimensional grapheme is put into solution, is allowed to uniformly mixed.It is compound that polyacrylonitrile/graphene is obtained after drying
Object.
It is warm by above-mentioned compound as hot pressing 3 hours, pressure 120Pa in the round stainless steel mould that diameter is 40mm
Degree is 150 DEG C.
By above-mentioned heat pressure film as in tube furnace, 6 hours, Pre oxidation 270 are pre-oxidized in air atmosphere
℃.Further, it is carbonized under an ar atmosphere 6 hours, carburizing temperature is 800 DEG C, finally obtains carbon-based Electric radiant Heating Film.Film thickness
For 20um, density 1.02mg/cm3。
Embodiment 4
It weighs 90mg graphene oxide to be dispersed in 60mL ethyl alcohol, stirring is uniformly dispersed for 1 hour, and obtained dispersion liquid is fallen
Enter in 100mL polytetrafluoro reaction kettle, is reacted 12 hours at 180 DEG C.
Obtained graphite ene product is subjected to solvent displacement, ethyl alcohol is all replaced as water, is freeze-dried later.
Dry graphene skeleton is placed in tube furnace and is annealed 1 hour at 1000 DEG C of temperature.
The polyacrylonitrile that 20mg molecular weight is 150,000 is weighed in 10ml n,N-Dimethylformamide, 50 DEG C is heated to, stirs
Dissolution is mixed, 20mg three-dimensional grapheme is put into solution, is allowed to uniformly mixed.It is compound that polyacrylonitrile/graphene is obtained after drying
Object.
It is warm by above-mentioned compound as hot pressing 3 hours, pressure 100Pa in the round stainless steel mould that diameter is 40mm
Degree is 100 DEG C.
By above-mentioned heat pressure film as in tube furnace, 6 hours, Pre oxidation 300 are pre-oxidized in air atmosphere
℃.Further, it is carbonized under an ar atmosphere 6 hours, carburizing temperature is 1000 DEG C, finally obtains carbon-based Electric radiant Heating Film.Film is thick
Degree is 16um, density 0.87mg/cm3。
Embodiment 5
It weighs 30mg graphene oxide to be dispersed in 60mL ethyl alcohol, stirring is uniformly dispersed for 1 hour, and obtained dispersion liquid is fallen
Enter in 100mL polytetrafluoro reaction kettle, is reacted 12 hours at 180 DEG C.
Obtained graphite ene product is subjected to solvent displacement, ethyl alcohol is all replaced as water, is freeze-dried later.
Dry graphene skeleton is placed in tube furnace and is annealed 1 hour at 800 DEG C of temperature.
The polyacrylonitrile that 30mg molecular weight is 150,000 is weighed in 10ml n,N-Dimethylformamide, 50 DEG C is heated to, stirs
Dissolution is mixed, 20mg three-dimensional grapheme is put into solution, is allowed to uniformly mixed.It is compound that polyacrylonitrile/graphene is obtained after drying
Object.
It is warm by above-mentioned compound as hot pressing 3 hours, pressure 120Pa in the round stainless steel mould that diameter is 40mm
Degree is 150 DEG C.
By above-mentioned heat pressure film as in tube furnace, 6 hours, Pre oxidation 300 are pre-oxidized in air atmosphere
℃.Further, it is carbonized under an ar atmosphere 6 hours, carburizing temperature is 1000 DEG C, finally obtains carbon-based Electric radiant Heating Film.Film is thick
Degree is 15um, density 0.84mg/cm3。
Embodiment 6
It weighs 30mg graphene oxide to be dispersed in 60mL ethyl alcohol, stirring is uniformly dispersed for 1 hour, and obtained dispersion liquid is fallen
Enter in 100mL polytetrafluoro reaction kettle, is reacted 12 hours at 200 DEG C.
Obtained graphite ene product is subjected to solvent displacement, ethyl alcohol is all replaced as water, is freeze-dried later.
Dry graphene skeleton is placed in tube furnace and is annealed 1 hour at 1000 DEG C of temperature.
The polyacrylonitrile that 50mg molecular weight is 150,000 is weighed in 10ml n,N-Dimethylformamide, 50 DEG C is heated to, stirs
Dissolution is mixed, 20mg three-dimensional grapheme is put into solution, is allowed to uniformly mixed.It is compound that polyacrylonitrile/graphene is obtained after drying
Object.
It is warm by above-mentioned compound as hot pressing 3 hours, pressure 120Pa in the round stainless steel mould that diameter is 40mm
Degree is 150 DEG C.
By above-mentioned heat pressure film as in tube furnace, 6 hours, Pre oxidation 300 are pre-oxidized in air atmosphere
℃.Further, it is carbonized under an ar atmosphere 6 hours, carburizing temperature is 1000 DEG C, finally obtains carbon-based Electric radiant Heating Film.Film is thick
Degree is 17um, density 0.89mg/cm3。
Embodiment 7
It weighs 300mg graphene oxide to be dispersed in 60mL ethyl alcohol, stirring is uniformly dispersed for 1 hour, the dispersion liquid that will be obtained
It pours into 100mL polytetrafluoro reaction kettle, is reacted 12 hours at 180 DEG C.
Obtained graphite ene product is subjected to solvent displacement, ethyl alcohol is all replaced as water, is freeze-dried later.
Dry graphene skeleton is placed in tube furnace and is annealed 1 hour at 800 DEG C of temperature.
The polyacrylonitrile that 20mg molecular weight is 150,000 is weighed in 10ml n,N-Dimethylformamide, 50 DEG C is heated to, stirs
Dissolution is mixed, 20mg three-dimensional grapheme is put into solution, is allowed to uniformly mixed.It is compound that polyacrylonitrile/graphene is obtained after drying
Object.
It is warm by above-mentioned compound as hot pressing 3 hours, pressure 100Pa in the round stainless steel mould that diameter is 40mm
Degree is 100 DEG C.
By above-mentioned heat pressure film as in tube furnace, 6 hours, Pre oxidation 300 are pre-oxidized in air atmosphere
℃.Further, it is carbonized under an ar atmosphere 6 hours, carburizing temperature is 1500 DEG C, finally obtains carbon-based Electric radiant Heating Film.Film is thick
Degree is 14um, density 0.81mg/cm3。
Embodiment 8
It weighs 300mg graphene oxide to be dispersed in 60mL ethyl alcohol, stirring is uniformly dispersed for 1 hour, the dispersion liquid that will be obtained
It pours into 100mL polytetrafluoro reaction kettle, is reacted 12 hours at 180 DEG C.
Obtained graphite ene product is subjected to solvent displacement, ethyl alcohol is all replaced as water, is freeze-dried later.
Dry graphene skeleton is placed in tube furnace and is annealed 1 hour at 1000 DEG C of temperature.
The polyacrylonitrile that 30mg molecular weight is 150,000 is weighed in 10ml n,N-Dimethylformamide, 50 DEG C is heated to, stirs
Dissolution is mixed, 20mg three-dimensional grapheme is put into solution, is allowed to uniformly mixed.It is compound that polyacrylonitrile/graphene is obtained after drying
Object.
It is warm by above-mentioned compound as hot pressing 3 hours, pressure 120Pa in the round stainless steel mould that diameter is 40mm
Degree is 150 DEG C.
By above-mentioned heat pressure film as in tube furnace, 6 hours, Pre oxidation 300 are pre-oxidized in air atmosphere
℃.Further, it is carbonized under an ar atmosphere 6 hours, carburizing temperature is 1500 DEG C, finally obtains carbon-based Electric radiant Heating Film.Film is thick
Degree is 15um, density 0.84mg/cm3。
Embodiment 9
It weighs 300mg graphene oxide to be dispersed in 60mL ethyl alcohol, stirring is uniformly dispersed for 1 hour, the dispersion liquid that will be obtained
It pours into 100mL polytetrafluoro reaction kettle, is reacted 12 hours at 200 DEG C.
Obtained graphite ene product is subjected to solvent displacement, ethyl alcohol is all replaced as water, is freeze-dried later.
Dry graphene skeleton is placed in tube furnace and is annealed 1 hour at 1000 DEG C of temperature.
The polyacrylonitrile that 50mg molecular weight is 150,000 is weighed in 10ml n,N-Dimethylformamide, 50 DEG C is heated to, stirs
Dissolution is mixed, 20mg three-dimensional grapheme is put into solution, is allowed to uniformly mixed.It is compound that polyacrylonitrile/graphene is obtained after drying
Object.
It is warm by above-mentioned compound as hot pressing 3 hours, pressure 120Pa in the round stainless steel mould that diameter is 40mm
Degree is 150 DEG C.
By above-mentioned heat pressure film as in tube furnace, 6 hours, Pre oxidation 300 are pre-oxidized in air atmosphere
℃.Further, it is carbonized under an ar atmosphere 6 hours, carburizing temperature is 1500 DEG C, finally obtains carbon-based Electric radiant Heating Film.Film is thick
Degree is 15um, density 0.92mg/cm3。
Well known to a person skilled in the art common sense for the unspecified part category of the present invention.
Claims (10)
1. a kind of carbon-based Electric radiant Heating Film, it is characterised in that: the raw material of the carbon-based Electric radiant Heating Film includes three-dimensional grapheme and polyacrylonitrile, and three
Dimension graphene is skeleton unit, and polyacrylonitrile is filled in the skeleton of three-dimensional grapheme.
2. a kind of carbon-based Electric radiant Heating Film according to claim 1, it is characterised in that: the composition of carbon-based Electric radiant Heating Film includes three-dimensional stone
Black alkene and graphite microcrystal, three-dimensional grapheme and graphite microcrystal are cross-linked structure.
3. a kind of carbon-based Electric radiant Heating Film according to claim 1 or 2, it is characterised in that: carbon-based Electric radiant Heating Film with a thickness of 10 μm
~500 μm.
4. a kind of preparation method of carbon-based Electric radiant Heating Film, it is characterised in that the step of this method includes:
Graphene oxide and the first organic solvent are mixed, and stirred by the first step, obtain homogeneous solution after mixing evenly,
Then obtained solution is subjected to solvent thermal reaction in a high pressure reaction kettle；
Second step, the product that the first step is obtained and water carry out exchange of solvent, are freeze-dried after the completion of exchange of solvent；
The product that second step obtains is heated under inert atmosphere or vacuum condition, is obtained three-dimensional porous by third step
Graphene skeleton structure；
Polyacrylonitrile and the second organic solvent are mixed, and stirred by the 4th step, obtain solution；
5th step, the three-dimensional porous graphene skeleton structure that third step is obtained is added in the solution that the 4th step obtains, and is done
It is dry, obtain graphene/polyacrylonitrile composite material；
6th step, the graphene that the 5th step is obtained/polyacrylonitrile composite material carry out hot pressing, obtain graphene/polyacrylonitrile
Composite material film；
7th step, graphene/polyacrylonitrile composite material film that the 6th step obtains successively is pre-oxidized in tube furnace,
Carbonization, obtains carbon-based Electric radiant Heating Film.
5. a kind of preparation method of carbon-based Electric radiant Heating Film according to claim 4, it is characterised in that: in the first step,
First organic solvent is ethyl alcohol, acetone, tetrahydrofuran or n,N-Dimethylformamide, the concentration of graphene oxide is 0.375~
10mg/mL, solvent thermal reaction temperature are 130-250 DEG C.
6. a kind of preparation method of carbon-based Electric radiant Heating Film according to claim 4, it is characterised in that: in the third step,
Heat treatment temperature is 200~1000 DEG C, heating treatment time 30-300min.
7. a kind of preparation method of carbon-based Electric radiant Heating Film according to claim 4, it is characterised in that: in the 4th step,
Second organic solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide, ethylene carbonate, N-methyl
One or more of pyrrolidones is mixed according to arbitrary proportion；The molecular weight of polyacrylonitrile is 5~200,000.
8. a kind of preparation method of carbon-based Electric radiant Heating Film according to claim 4, it is characterised in that: in the 5th step,
The mass ratio of three-dimensional porous graphene skeleton structure and polyacrylonitrile is 10:10~90.
9. a kind of preparation method of carbon-based Electric radiant Heating Film according to claim 4, it is characterised in that: in the 6th step,
Hot pressing temperature is 25~150 DEG C, and hot pressing pressure is 19~500Pa.
10. a kind of preparation method of carbon-based Electric radiant Heating Film according to claim 4, it is characterised in that: in the 7th step,
Pre oxidation is 250~320 DEG C, and carburizing temperature is 800~3000 DEG C.
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| CN105217619A (en) * | 2015-10-23 | 2016-01-06 | 南京工业大学 | A kind of preparation method of graphene film |
| CN106116580A (en) * | 2016-06-30 | 2016-11-16 | 东华大学 | A kind of flexible carbon film and preparation method thereof |
| CN106185885A (en) * | 2016-06-30 | 2016-12-07 | 天津大学 | There is isotropism height heat conduction, elastic three-dimensional grapheme and the preparation method of carbon nano tube compound material |
| CN108219366A (en) * | 2016-12-15 | 2018-06-29 | 沙特基础工业全球技术公司 | Heat conduction is three-dimensional（3-D）Graphene-polymer composite material, Its Preparation Method And Use |
| CN109244540A (en) * | 2018-11-19 | 2019-01-18 | 中国科学院宁波材料技术与工程研究所 | A kind of solid polymer electrolyte, preparation method and lithium ion battery |
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