CN114974933A - Preparation method of sisal fiber carbon paper for supercapacitor - Google Patents
Preparation method of sisal fiber carbon paper for supercapacitor Download PDFInfo
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- CN114974933A CN114974933A CN202210650335.2A CN202210650335A CN114974933A CN 114974933 A CN114974933 A CN 114974933A CN 202210650335 A CN202210650335 A CN 202210650335A CN 114974933 A CN114974933 A CN 114974933A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method of sisal fiber carbon paper for a supercapacitor, which comprises the following steps: s1) uniformly mixing the sisal segments and a strong alkali solution in a reaction kettle, carrying out hydrothermal reaction, collecting solid matters after the hydrothermal reaction is finished, and washing to obtain sisal fiber slurry; s2) diluting the sisal fiber slurry, pouring the diluted sisal fiber slurry into a mould, pressing and forming, and fully drying to obtain sisal fiber paper; s3) heating and carbonizing the sisal fiber paper under the anaerobic condition, and cooling to obtain the sisal fiber carbon paper after carbonization is completed. According to the preparation method of some examples of the invention, the raw materials are cheap and easy to obtain, the sisal fiber carbon paper with controllable shape is obtained by pressing with a mould, the sisal fiber carbon paper with better performance and complete shape is obtained, the specific surface area is large, the fiber structure is compact, and the sisal fiber carbon paper is an excellent supercapacitor material and is expected to replace foamed nickel, commercial carbon paper and carbon cloth to be used as a substrate of a supercapacitor.
Description
Technical Field
The invention belongs to the field of new materials, and particularly relates to a preparation method of sisal fiber carbon paper for a supercapacitor.
Background
As a novel energy storage element, the super capacitor has the advantages of high charging speed, long placing time, environmental protection, higher specific capacitance, higher specific power, longer service life and the like, so that the super capacitor has huge potential and wide application prospect in the fields of electronic communication, electric vehicles, national defense science and technology and the like. The carbon-based material has the advantages of higher conductivity, relatively lower price, better stability and the like, and is widely applied to research in the aspect of supercapacitors.
In order to solve the problems of energy cost, environmental pollution and resource shortage, the preparation of an activated carbon material with high electrochemical performance by using biomass as a carbon source is shown as a new technology with great potential and market value. Sisal hemp is a tropical perennial plant, has wide adaptability, fast growth and high yield, has a bast fiber structure, and provides a raw material for preparing a high-performance carbon fiber material for super capacitor research.
CN108950738A discloses a preparation method of sisal activated carbon fiber, which comprises the following steps: carbonizing sisal fibers to obtain carbonized sisal fibers; carrying out impregnation treatment on the carbonized sisal fibers by using a KOH solution to obtain impregnated sisal fibers; and carrying out activation treatment on the impregnated sisal fibers to obtain the sisal activated carbon fibers. The sisal fibers selected by the invention are rich in source, environment-friendly and low in cost; according to the preparation method, the sisal fibers are carbonized firstly, so that the damage to the sisal fiber structure can be avoided fully, and the activated sisal fibers are impregnated and activated by KOH, so that the maximum specific surface area of the prepared sisal activated carbon fibers can reach 2289m 2 ·g -1 And has rich pore distribution; the prepared sisal hemp activated carbon fiber is used in a super capacitor at 0.5 A.g -1 The specific capacitance below (A) is up to 415F/g, and the energy density under a 6.0M KOH aqueous electrolyte two-electrode system is up to 12.6 Wh/Kg.
CN107665777A discloses a preparation method of a biomass-based activated carbon electrode material. The method comprises the following steps: an oxidation process of the biomass material; dipping the mixed solution of organic amine and an alkaline compound; carbonizing; mixing with an activator; activating; wherein the activation temperature is 500-1000 ℃, preferably 500-800 ℃, and most preferably 500-650 ℃; washing and drying to obtain the active carbon material for the electrode of the super capacitor; and electrical performance testing was performed. The product prepared by the invention shows high energy density and long cycle life in the super capacitor.
The existing method is relatively complex, and the performance needs to be further improved.
Disclosure of Invention
The invention aims to overcome at least one defect in the prior art and provides a preparation method of sisal fiber carbon paper for a supercapacitor.
The technical scheme adopted by the invention is as follows:
a preparation method of sisal fiber carbon paper for a supercapacitor comprises the following steps:
s1) uniformly mixing the sisal segments and a strong alkali solution in a reaction kettle, carrying out hydrothermal reaction, collecting solid matters after the hydrothermal reaction is finished, and washing to obtain sisal fiber slurry;
s2) diluting the sisal fiber pulp, pouring the diluted sisal fiber pulp into a mould, pressing and forming, and fully drying to obtain sisal fiber paper;
s3) heating and carbonizing the sisal fiber paper under the anaerobic condition, and cooling to obtain the sisal fiber carbon paper after carbonization.
In some examples of the preparation method, the temperature of the hydrothermal reaction is 140 to 180 ℃.
In some examples of the preparation method, the hydrothermal reaction time is 12-30 h.
In some examples of the preparation method, the temperature of the hydrothermal reaction is 140-180 ℃, and the time of the hydrothermal reaction is 12-30 h.
In some examples of the preparation method, the carbonization is carried out by raising the temperature to 800-1000 ℃.
In some examples of the preparation method, the temperature rise rate is 3-7 ℃/min.
In some examples of the preparation method, the carbonization time is 30 to 120 min.
In some examples of the preparation method, the temperature is increased to 800-1000 ℃ for carbonization, and the carbonization time is 30-120 min.
In some examples of the preparation method, the temperature is increased to 800-1000 ℃ for carbonization, the carbonization time is 30-120 min, and the temperature increasing rate is 3-7 ℃/min.
In some examples of the preparation method, the mixing ratio of the strong alkaline solution to sisal segments is 50 mL: (3-6) g.
In some examples of the preparation method, the concentration of the strong alkali solution is 2-3M.
In some examples of the preparation method, the mixing ratio of the strong alkaline solution to sisal segments is 50 mL: (3-6) g, wherein the concentration of the strong alkali solution is 2-3M.
In some examples of the preparation method, the pressure of the pressing is not higher than 4 Mpa.
In some examples of the preparation method, the pressing time is not less than 30 s.
In some examples of the production method, the pressure of the pressing is not higher than 4 Mpa, and the time of the pressing is not lower than 30 s.
In some examples of the preparation method, the length of the sisal segments is 1-2 cm.
In some examples of the method of making, the sisal fiber paper has a moisture content of no more than 1%.
The invention has the beneficial effects that:
according to the preparation method of some embodiments of the invention, the raw materials are cheap and easy to obtain, and the sisal fiber carbon paper with controllable shape is obtained by pressing with the mold, so that the sisal fiber carbon paper with better performance and complete shape can be obtained.
The sisal fiber carbon paper prepared by the preparation method provided by the invention has a relatively complete fiber structure, a large specific surface area and a compact fiber structure, is an excellent supercapacitor material, and is expected to replace foamed nickel, commercial carbon paper and carbon cloth to be used as a substrate of a supercapacitor.
Drawings
FIG. 1 is a scanning electron micrograph of sisal fiber carbon paper obtained at different calcination temperatures, wherein (a) is 800 ℃, (b) is 900 ℃, and (c) is 1000 ℃.
Fig. 2 shows the adsorption isotherms (a) and pore size distributions (b) for different materials.
FIG. 3 shows the values of the different materials at 10 mV s -1 Circulation ofVoltammograms (a) and specific capacitances (b) at different currents.
Detailed Description
A preparation method of sisal fiber carbon paper for a supercapacitor comprises the following steps:
s1) uniformly mixing the sisal segments and a strong alkali solution in a reaction kettle, carrying out hydrothermal reaction, collecting solid matters after the hydrothermal reaction is finished, and washing to obtain sisal fiber slurry;
s2) diluting the sisal fiber slurry, pouring the diluted sisal fiber slurry into a mould, pressing and forming, and fully drying to obtain sisal fiber paper;
s3) heating and carbonizing the sisal fiber paper under the anaerobic condition, and cooling to obtain the sisal fiber carbon paper after carbonization is completed.
In some examples of the preparation method, the temperature of the hydrothermal reaction is 140 to 180 ℃. The structural integrity of the sisal fibers can be better maintained at this reaction temperature.
In some examples of the preparation method, the hydrothermal reaction time is 12-30 h. This makes it possible to achieve sufficient reaction.
In some examples of the preparation method, the temperature of the hydrothermal reaction is 140-180 ℃, and the time of the hydrothermal reaction is 12-30 h.
In some examples of the preparation method, the carbonization is carried out by raising the temperature to 800-1000 ℃. Thus, the carbonization becomes more sufficient.
In some examples of the preparation method, the temperature rise rate is 3-7 ℃/min. This is advantageous in order to better maintain the structural integrity of the sisal fibers.
In some examples of the preparation method, the carbonization time is 30 to 120 min. Thus, the carbonization becomes more sufficient.
In some examples of the preparation method, the temperature is increased to 800-1000 ℃ for carbonization, and the carbonization time is 30-120 min.
In some examples of the preparation method, the temperature is increased to 800-1000 ℃ for carbonization, the carbonization time is 30-120 min, and the temperature increasing rate is 3-7 ℃/min.
In some examples of the preparation method, the mixing ratio of the strong alkaline solution to sisal segments is 50 mL: (3-6) g.
In some examples of the preparation method, the concentration of the strong alkali solution is 2-3M.
In some examples of the preparation method, the mixing ratio of the strong alkaline solution to sisal segments is 50 mL: (3-6) g, wherein the concentration of the strong alkali solution is 2-3M.
In some examples of the preparation method, the pressure of the pressing is not higher than 4 Mpa. Too high a pressure may result in too dense a sisal fiber paper, affecting the subsequent carbonization.
In some examples of the preparation method, the pressing time is not less than 30 s.
In some examples of the production method, the pressure of the pressing is not higher than 4 Mpa, and the time of the pressing is not lower than 30 s.
In some examples of the preparation method, the length of the sisal segments is 1-2 cm.
In some examples of the method of making, the sisal fiber paper has a moisture content of no more than 1%.
The technical scheme of the invention is further explained by combining the examples.
Example 1
A preparation method of sisal fiber carbon paper for a supercapacitor comprises the following steps:
s1) screening and cleaning sisal hemp, cutting the sisal hemp into small sections with the length of 1-2 cm, weighing 5 g of the sisal hemp, placing the small sections into a polytetrafluoroethylene lining of a 100 mL high-pressure reaction kettle, adding 60 mL of 2.5M KOH, carrying out hydrothermal treatment for 20 h at 160 ℃, naturally cooling, repeatedly filtering and washing the obtained sample until the sample is neutral, and carrying out suction filtration to obtain sisal hemp fiber slurry;
s2) weighing a certain amount of sisal pulp, placing the sisal pulp in a 50 mL beaker, adding 20 mL of distilled water, stirring, pouring the mixture into a 3D printing grinding tool after uniformly stirring, pressing the mixture by a press machine, and placing the obtained sisal fiber paper in an oven at 80 ℃ overnight to obtain sisal fiber paper;
s3) placing the obtained sisal fiber paper into a corundum ark, calcining for 1 h in a tubular furnace with inert gas as protective gas, wherein the calcining temperature is 800-1000 ℃, the heating rate is 5 ℃/min, and obtaining the sisal fiber carbon paper after the furnace temperature is naturally cooled to room temperature.
S4) 6M KOH is used as electrolyte, carbon paper obtained at different calcination temperatures (800 ℃, 900 ℃ and 1000 ℃) is used as electrode material, and the button cell is assembled and tested by an electrochemical workstation.
Scanning electron micrographs of sisal fiber carbon paper obtained at different calcination temperatures are shown in fig. 1, and it can be seen from the drawings that all carbon paper carbonized at different temperatures have diameters of 2-10 μm and are interwoven together. The structure of the carbon paper carbonized at 800 ℃ and 900 ℃ is not obviously changed, and the fiber is subjected to thermal shrinkage at 1000 ℃. The graph under a high power lens shows that carbonization at 900 ℃ and 1000 ℃ has rich porous structures, and the higher carbonization temperature is beneficial to the formation of pore diameters and defects in the sisal fiber material.
The adsorption/desorption curves (a) and pore size distributions (b) of sisal fiber carbon papers obtained at different calcination temperatures are shown in fig. 2. Wherein the adsorption/desorption isotherms exhibit type I/IV characteristics, indicating the presence of micropores and mesopores/macropores in the carbon paper. The specific surface areas of the carbon paper obtained after firing at 800 ℃, 900 ℃ and 1000 ℃ are 282.7, 801.0 and 533.8 m respectively 2 g −1 . As can be seen from the pore size distribution curve (b), the average pore sizes of the carbon papers obtained by firing at 800 deg.C, 900 deg.C and 1000 deg.C were about 4.63 nm, 2.86 nm and 3.66 nm, respectively, and the pores were mainly composed of mesopores. It is clear that the carbon paper obtained after firing at 900 ℃ has the largest specific surface area and the lowest pore volume.
Cyclic voltammograms (a) and specific capacitances (b) of sisal fiber carbon papers obtained at different calcination temperatures and different current densities are shown in fig. 3. As can be seen from the cyclic voltammetry curves, the curves are all in a quasi-rectangular shape, which indicates that the obtained carbon paper has ideal double-layer capacitance behavior. In addition, the maximum CV area after firing at 900 ℃ indicates the best specific capacity, and is calculated to be 0.1A g −1 Specific capacitance at current density of 80.2F g −1 . At 2A g −1 Specific capacitance at current density of 62.9F g −1 The capacity retention was 78.4%.
The foregoing is a more detailed description of the invention and is not to be taken in a limiting sense. It will be apparent to those skilled in the art that simple deductions or substitutions without departing from the spirit of the invention are within the scope of the invention.
Claims (10)
1. A preparation method of sisal fiber carbon paper for a supercapacitor is characterized by comprising the following steps:
uniformly mixing the sisal segments and a strong alkali solution in a reaction kettle, carrying out hydrothermal reaction, collecting solid matters after the hydrothermal reaction is finished, and washing to obtain sisal fiber slurry;
diluting the sisal fiber slurry, pouring the diluted sisal fiber slurry into a mold, performing compression molding, and fully drying to obtain sisal fiber paper;
and (3) heating and carbonizing the sisal fiber paper under the anaerobic condition, and cooling to obtain the sisal fiber carbon paper after carbonization is finished.
2. The preparation method according to claim 1, wherein the temperature of the hydrothermal reaction is 140 to 180 ℃; and/or the time of the hydrothermal reaction is 12-30 h.
3. The method according to claim 1, wherein the carbonization is performed at a temperature of 800 to 1000 ℃.
4. The method according to claim 2, wherein the temperature is raised at a rate of 3 to 7 ℃/min.
5. The method according to claim 3 or 4, wherein the carbonization time is 30 to 120 min.
6. The preparation method according to any one of claims 1 to 4, wherein the mixing ratio of the strong alkaline solution to the sisal segments is 50 mL: (3-6) g.
7. The method according to claim 6, wherein the concentration of the alkali solution is 2 to 3M.
8. The method according to any one of claims 1 to 4, wherein the pressure of the pressing is not higher than 4 MPa; and/or the time of said pressing is not less than 30 s.
9. The method according to any one of claims 1 to 4, wherein the sisal segments have a length of 1-2 cm.
10. The method according to any one of claims 1 to 4, wherein the sisal fiber paper has a water content of not more than 1%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130027844A1 (en) * | 2010-02-11 | 2013-01-31 | Industry Foundation Of Chonnam National University | Method for preparing porous carbon nanofibers containing a metal oxide, porous carbon nanofibers prepared using the method, and carbon nanofiber products including same |
| CN106757535A (en) * | 2016-11-30 | 2017-05-31 | 桂林理工大学 | A kind of sisal fiber base tube shape hollow structure biological carbon materials and preparation method thereof |
| CN107460777A (en) * | 2017-07-31 | 2017-12-12 | 华南理工大学 | A kind of preparation method of full carbon fibre composite paper |
| CN112593436A (en) * | 2020-12-19 | 2021-04-02 | 桂林理工大学 | Preparation method of sisal fiber paper-based friction nano-generator |
| CN114496592A (en) * | 2021-12-20 | 2022-05-13 | 西安理工大学 | Preparation method of supercapacitor electrode material taking kitchen paper as raw material |
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- 2022-06-10 CN CN202210650335.2A patent/CN114974933A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130027844A1 (en) * | 2010-02-11 | 2013-01-31 | Industry Foundation Of Chonnam National University | Method for preparing porous carbon nanofibers containing a metal oxide, porous carbon nanofibers prepared using the method, and carbon nanofiber products including same |
| CN106757535A (en) * | 2016-11-30 | 2017-05-31 | 桂林理工大学 | A kind of sisal fiber base tube shape hollow structure biological carbon materials and preparation method thereof |
| CN107460777A (en) * | 2017-07-31 | 2017-12-12 | 华南理工大学 | A kind of preparation method of full carbon fibre composite paper |
| CN112593436A (en) * | 2020-12-19 | 2021-04-02 | 桂林理工大学 | Preparation method of sisal fiber paper-based friction nano-generator |
| CN114496592A (en) * | 2021-12-20 | 2022-05-13 | 西安理工大学 | Preparation method of supercapacitor electrode material taking kitchen paper as raw material |
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