CN118007283A - Bimodal aperture flexible carbon fiber material prepared by electrostatic spinning and method - Google Patents
Bimodal aperture flexible carbon fiber material prepared by electrostatic spinning and method Download PDFInfo
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- CN118007283A CN118007283A CN202410255991.1A CN202410255991A CN118007283A CN 118007283 A CN118007283 A CN 118007283A CN 202410255991 A CN202410255991 A CN 202410255991A CN 118007283 A CN118007283 A CN 118007283A
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- carbon fiber
- electrostatic spinning
- fiber material
- material prepared
- flexible carbon
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- 239000000463 material Substances 0.000 title claims abstract description 52
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 39
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 39
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 30
- 230000002902 bimodal effect Effects 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000011148 porous material Substances 0.000 claims abstract description 41
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000835 fiber Substances 0.000 claims abstract description 17
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000003763 carbonization Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- 238000009656 pre-carbonization Methods 0.000 claims abstract description 4
- 239000002243 precursor Substances 0.000 claims description 18
- 238000010000 carbonizing Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000001523 electrospinning Methods 0.000 claims description 6
- 238000009987 spinning Methods 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000003990 capacitor Substances 0.000 abstract description 3
- 239000007772 electrode material Substances 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 3
- -1 electrocatalysis Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 9
- 238000005452 bending Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Fibers (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning and a method thereof, belonging to the field of carbon fiber materials. According to the invention, polyacrylonitrile and melamine are taken as raw materials, dissolved in a dimethylformamide solvent, prepared into a fiber felt through an electrostatic spinning technology, and then subjected to links such as drying, pre-carbonization, high-temperature carbonization and the like to form the carbon fiber felt. Because of the adsorption adhesion in the electrostatic spinning process, the fibers self-assemble to form a beam-shaped structure, an enlarged pore structure is formed in the material, and meanwhile, secondary holes of about 100 nanometers are formed in the fiber bundles. The material obtained by the invention has higher flexibility and higher liquid permeability, adjustable pore structure and simple preparation process, and has important application value in the fields of electrode materials, electrocatalysis, capacitors and the like.
Description
Technical Field
The invention belongs to the field of carbon fiber materials, and particularly relates to a bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning and a method thereof.
Background
In recent years, developments in the fields of batteries, capacitors, electrocatalysis and the like have important significance for energy storage and conversion. Conventional materials have some limitations in these applications, such as low energy density, short cycle life, or lack of catalytic activity. Thus, there is a need to develop new materials to meet these challenges and provide a more efficient, reliable, and durable solution.
Carbon fiber is a light, high-strength material with good conductivity and chemical stability. This makes carbon fibers have great potential in the field of energy storage and conversion. However, conventional carbon fiber materials have some limitations in terms of flexibility and pore structure, resulting in limited applications. For example, the preparation process is complex, the flexibility is insufficient, the pore structure is difficult to regulate and control, and the like. Therefore, a novel carbon fiber material is needed, which has excellent flexibility and adjustable pore structure, so as to meet the requirements of high-performance materials in the fields of electrode materials, electrocatalysis, capacitors and the like.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning with simple process and low cost and a method thereof, and the bimodal pore diameter structure formed by self-assembly can meet the application requirements in the electrochemical and electrocatalytic fields. The preparation method provided by the invention has the advantages of simple process and low cost, and can be used for mass production.
The specific technical scheme adopted by the invention is as follows:
in a first aspect, the invention provides a preparation method of a bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning, which comprises the following steps:
Dissolving polyacrylonitrile and melamine in dimethylformamide, and uniformly stirring to obtain a precursor solution; spinning and collecting the precursor solution in a high-voltage environment by utilizing an electrostatic spinning technology, and then taking down and drying the collected fiber felt; and pre-carbonizing the dried fiber mat in an air atmosphere, carbonizing at a high temperature in a nitrogen atmosphere, and cooling to obtain the bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning.
Preferably, in the precursor solution, the polyacrylonitrile solid molecular weight is Mw 149000 ～ 151000, the polyacrylonitrile mass fraction is 8% -12%. Wt. (more preferably 10%. Wt.), and the melamine mass fraction is 2% -3%. Wt. (more preferably 3%. Wt.).
Preferably, the process parameters of the electrospinning are as follows:
the pushing speed is 1-3mL/min (more preferably 1-1.5 mL/min), the positive pressure is 15-18kV, the negative pressure is 2-8kV (more preferably 5-8 kV), the distance between the needle head and the receiver is 8-13cm, the rotating speed of the receiver is 200-3000rpm, the ambient temperature is 20-40 ℃, and the humidity is 20-40%.
Preferably, the drying is performed at a temperature of 40-60 ℃ for 8-12 hours under a vacuum environment.
Preferably, the pre-carbonization means carbonization at a temperature of 220-260 ℃ (more preferably 230-250 ℃) for 1-2 hours, and a heating rate of not more than 5 ℃/min (more preferably 2-3 ℃/min).
Preferably, the high-temperature carbonization means carbonization at a temperature of 800-1200 ℃ (more preferably 1000-1100 ℃) for 1-2 hours, and a heating rate of not more than 5 ℃/min (more preferably 2-3 ℃/min).
In a second aspect, the invention provides a bimodal pore size flexible carbon fiber material prepared by electrospinning obtained by any of the preparation methods of the first aspect.
Preferably, the material has a pore structure with two pore diameters of 1 μm and 100nm, and the diameter is 100-200nm.
Preferably, the material is bent at an angle of up to 170 ° without breaking.
Preferably, the resistivity of the material is 158.8mΩ·cm.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention has simple process and low cost, and can be produced in large scale.
(2) The carbon fiber material prepared by the invention has higher flexibility than the common electrospun carbon fiber, and can be widely applied to the fields of wearable electronic products such as various sensors, conductive fabrics, flexible electrode materials and the like.
(3) The carbon fiber material prepared by the invention has a unique bimodal pore diameter structure, overcomes the contradiction problem between the permeability and the specific surface area of a single pore diameter, can realize high liquid permeability and high specific surface area at the same time, and can realize important performance breakthrough in the fields of electrochemistry and electrocatalysis.
Drawings
FIG. 1 is a scanning electron microscope image of a self-assembled bimodal pore size structure flexible carbon fiber prepared by electrostatic spinning;
FIG. 2 is a graph of a curved comparison of examples and comparative examples; wherein, (a) is an example and (b) is a comparative example;
fig. 3 is a graph of pore size distribution of examples and comparative examples.
Detailed Description
The invention is further illustrated and described below with reference to the drawings and detailed description. The technical features of the embodiments of the invention can be combined correspondingly on the premise of no mutual conflict.
The invention provides a bimodal pore-size flexible carbon fiber material prepared by electrostatic spinning, which is prepared by using two components, namely polyacrylonitrile and melamine through an electrostatic spinning technology and carbonization, and the preparation method comprises the following steps:
And dissolving polyacrylonitrile and melamine in dimethylformamide, and uniformly stirring to obtain a precursor solution. And (3) putting the obtained precursor solution into a needle tube of an injector, spinning and collecting the precursor solution in a high-voltage environment by using an electrostatic spinning technology, and taking down and drying the collected fiber felt after a certain time. And pre-carbonizing the dried fiber felt in an air atmosphere, carbonizing at a high temperature in a nitrogen atmosphere, and cooling to obtain the bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning.
As a preferred embodiment of the invention, the molecular weight of polyacrylonitrile solid in the precursor solution is Mw149000 ～ 151000, the mass fraction of polyacrylonitrile in the precursor solution is 8% -12% wt, and the mass fraction of melamine in the precursor solution is 2% -3% wt.
As a preferred embodiment of the present invention, the process parameters of electrospinning are as follows:
The pushing speed of the injector is 1-3mL/min, the positive pressure is 15-18kV, the negative pressure is 2-8kV, the distance between the needle head and the receiver is 8-13cm, the rotating speed of the roller receiver is 200-3000rpm, the ambient temperature is 20-40 ℃, and the humidity is 20% -40%.
As a preferred embodiment of the present invention, drying means drying at a temperature of 40-60℃for 8-12 hours under a vacuum atmosphere (e.g., a vacuum oven). Pre-carbonization refers to carbonization in a muffle furnace or a tube furnace at 220-260 ℃ for 1-2h, wherein the heating rate is not more than 5 ℃/min. High temperature carbonization means carbonization in a tube furnace at 800-1200 ℃ for 1-2 hours at a heating rate of not more than 5 ℃/min.
The carbon fiber material obtained by the preparation method provided by the invention has a pore structure with two pore diameters of 1 mu m and 100 nm. The diameter of the carbon fiber material is 100-200nm, the surface of the fiber is smooth, and no obvious protrusion exists. Compared with the traditional electrostatic spinning carbon fiber, the carbon fiber material prepared by the invention has higher flexibility, and the bending angle reaches 170 degrees without fracture. The carbon fiber material prepared by the invention has higher conductivity and the resistivity is 158.8mΩ cm.
The specific steps of the process of the invention and the properties of the resulting materials will be further illustrated by the examples and comparative examples.
Examples
The embodiment prepares a bimodal pore-size flexible carbon fiber material prepared by electrostatic spinning, and the preparation method specifically comprises the following steps:
(1) 1g of polyacrylonitrile (molecular weight Mw 149000 ～ 151000) and 0.3g of melamine were dissolved in 8.7g of dimethylformamide, and stirred for 12 hours, to obtain a precursor solution.
(2) Putting the precursor solution in the step (1) into a needle tube of an injector, spinning and collecting the precursor solution in a high-voltage environment by utilizing an electrostatic spinning technology, wherein electrostatic spinning parameters are as follows: the pushing speed of the injector is 1mL/min, the positive pressure is 15kV, the negative pressure is 5kV, the distance between the needle head and the receiver is 11cm, the rotating speed of the roller receiver is 3000rpm, the ambient temperature is 30 ℃, and the humidity is 30%.
(3) And (3) placing the sample obtained in the step (2) in a vacuum drying oven, and drying at the temperature of 40 ℃ for 8 hours.
(4) And (3) placing the sample obtained in the step (3) in a muffle furnace, carbonizing for 1.5h at 230 ℃ and heating at a speed of 3 ℃/min.
(5) Carbonizing the sample obtained in the step (4) in a tube furnace at the temperature of 1000 ℃ for 1.5h, wherein the heating rate is 5 ℃/min.
Comparative example
The comparative example prepared a carbon fiber material, the preparation method specifically comprises the following steps:
(1) 1g of polyacrylonitrile (molecular weight Mw 149000 ～ 151000) was dissolved in 9g of dimethylformamide and stirred for 12 hours to obtain a precursor solution.
(2) Putting the precursor solution in the step (1) into a needle tube of an injector, spinning and collecting the precursor solution in a high-voltage environment by utilizing an electrostatic spinning technology, wherein electrostatic spinning parameters are as follows: the pushing speed of the injector is 1mL/min, the positive pressure is 15kV, the negative pressure is 5kV, the distance between the needle head and the receiver is 11cm, the rotating speed of the roller receiver is 500rpm, the ambient temperature is 30 ℃, and the humidity is 30%.
(3) And (3) placing the sample obtained in the step (2) in a vacuum drying oven, and drying at the temperature of 40 ℃ for 8 hours.
(4) Carbonizing the sample obtained in the step (3) in a muffle furnace at 230 ℃ for 1.5h, wherein the heating rate is 3 ℃/min.
(5) Carbonizing the sample obtained in the step (4) in a tube furnace at the temperature of 1000 ℃ for 1.5h, wherein the heating rate is 5 ℃/min.
The results obtained are as follows:
Fig. 1 is a scanning electron microscope image of the material obtained in the example, and it can be seen that the fibers of the material self-assemble to form fiber bundles, pores with slightly larger size are formed between the fiber bundles, and pores with slightly smaller size are formed between the fibers.
Fig. 2 is a graph comparing the bending of the materials obtained in the examples with that obtained in the comparative examples, wherein the materials obtained in the examples are significantly more flexible and can be bent at an angle approaching 180 ° without significant breakage, but the materials obtained in the comparative examples have significantly broken when the bending amplitude is less than 90 °.
FIG. 3 is a graph showing pore size distribution of a material obtained in examples having pores of both sizes of 1 μm and 100 nm and a material obtained in comparative examples having only one pore size of about 500 nm. It can be seen that the pores between the fibers are reduced to about 100 nm due to self-assembly and mutual adhesion of the fibers, and the pores between the fiber bundles are enlarged to about 1 μm based on the original pores.
The above embodiment is only a preferred embodiment of the present invention, but it is not intended to limit the present invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, all the technical schemes obtained by adopting the equivalent substitution or equivalent transformation are within the protection scope of the invention.
Claims (10)
1. The preparation method of the bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning is characterized by comprising the following steps:
Dissolving polyacrylonitrile and melamine in dimethylformamide, and uniformly stirring to obtain a precursor solution; spinning and collecting the precursor solution in a high-voltage environment by utilizing an electrostatic spinning technology, and then taking down and drying the collected fiber felt; and pre-carbonizing the dried fiber mat in an air atmosphere, carbonizing at a high temperature in a nitrogen atmosphere, and cooling to obtain the bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning.
2. The method for preparing the bimodal pore-size flexible carbon fiber material prepared by electrostatic spinning according to claim 1, wherein in the precursor solution, the molecular weight of polyacrylonitrile solid is Mw149000 ～ 151000, the mass fraction of polyacrylonitrile is 8% -12%. Wt, and the mass fraction of melamine is 2% -3%. Wt.
3. The method for preparing the bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning according to claim 1, wherein the electrostatic spinning process parameters are as follows:
the pushing speed is 1-3mL/min, the positive pressure is 15-18kV, the negative pressure is 2-8kV, the distance between the needle head and the receiver is 8-13cm, the rotating speed of the receiver is 200-3000rpm, the ambient temperature is 20-40 ℃, and the humidity is 20% -40%.
4. The method for preparing the bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning according to claim 1, wherein the drying is performed at a temperature of 40-60 ℃ for 8-12h in a vacuum environment.
5. The method for preparing the bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning according to claim 1, wherein the pre-carbonization is carbonization for 1-2 hours at 220-260 ℃ and the heating rate is not more than 5 ℃/min.
6. The method for preparing the bimodal pore diameter flexible carbon fiber material prepared by electrostatic spinning according to claim 1, wherein the high temperature carbonization is carried out at 800-1200 ℃ for 1-2h, and the heating rate is not more than 5 ℃/min.
7. A bimodal pore size flexible carbon fiber material prepared by electrospinning obtained by the preparation method of any one of claims 1 to 6.
8. The bimodal pore diameter flexible carbon fiber material prepared by electrospinning according to claim 7, wherein the material has a pore structure with two pore diameters of 1 μm and 100nm, and a diameter of 100-200nm.
9. The bimodal pore size flexible carbon fiber material prepared by electrospinning according to claim 7, wherein the material has a bend angle of up to 170 ° without breaking.
10. The electrospun bimodal pore size flexible carbon fiber material as claimed in claim 7, wherein said material has a resistivity of 158.8mΩ -cm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410255991.1A CN118007283A (en) | 2024-03-06 | 2024-03-06 | Bimodal aperture flexible carbon fiber material prepared by electrostatic spinning and method |
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| CN202410255991.1A CN118007283A (en) | 2024-03-06 | 2024-03-06 | Bimodal aperture flexible carbon fiber material prepared by electrostatic spinning and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118281247A (en) * | 2024-05-27 | 2024-07-02 | 中石油深圳新能源研究院有限公司 | Porous carbon fiber electrode and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118281247A (en) * | 2024-05-27 | 2024-07-02 | 中石油深圳新能源研究院有限公司 | Porous carbon fiber electrode and preparation method and application thereof |
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