CN108950736A - Nanoporous carbon fiber and preparation method thereof - Google Patents
Nanoporous carbon fiber and preparation method thereof Download PDFInfo
- Publication number
- CN108950736A CN108950736A CN201810960771.3A CN201810960771A CN108950736A CN 108950736 A CN108950736 A CN 108950736A CN 201810960771 A CN201810960771 A CN 201810960771A CN 108950736 A CN108950736 A CN 108950736A
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- China
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- preparation
- carbon fiber
- sodium alginate
- aqueous solution
- nanoporous carbon
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- 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
-
- 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
- H01G11/40—Fibres
-
- 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 nanoporous carbon fibers and preparation method thereof, prepare certain density sodium alginate soln and FeCl respectively2Solution is freeze-dried after mixing evenly, under nitrogen protection, controls temperature program, and obtained sample is placed on tube furnace charing at a certain temperature, the oxide particle of Fe is washed away after being cooled to room temperature with hydrochloric acid, obtains flexible, porous carbon nano-fiber.This method mild condition, simple process, it is selected materials nature rich reserves, cheap, it can industrialized production；Obtained carbon fiber is bent, large specific surface area, degree of graphitization are high, presents good chemical property as electrode material for super capacitor.
Description
Technical field
The invention belongs to electrode material for super capacitor technical fields, and in particular to nanoporous carbon fiber and its preparation side
Method and its application in supercapacitor.
Background technique
With the rapid development of social economy, the non-regeneration energies such as petroleum, coal are increasingly depleted, and in energy consumption
Serious destruction produced to environment in the process, energy crisis and environmental problem have become human society to be faced it is main
Problem, thus it is extremely urgent for the exploitation of clean energy resource and novel energy-storing material.From new energy technology development and application
From the point of view of, requirement of the people to power supply energy density and cycle performance is higher and higher, promotes high capacity and high circulation stability
The development of electrochemical power source, in this context, supercapacitor is come into being.Supercapacitor is also known as electrochemical capacitor,
It is a kind of novel energy storage apparatus between traditional capacitor and battery, because its power is big, the charging time is short, has extended cycle life
The features such as have received widespread attention, have very in fields such as hybrid vehicle, big aircraft, high-speed rail, electronics
Good application prospect.
Electrode material be influence supercapacitor chemical property core, as application time at most, industrialization
The highest carbon material of degree, the advantages that by its huge specific surface area, stable physicochemical properties and good electric conductivity
Extensive concern is obtained.The one kind of carbon nano-fiber as carbon material has better compared with the carbon nano-particle of zero dimension
Continuity has bigger specific surface area, preferably flexible and flexibility compared with two-dimensional carbon nanosheet, and flexibility can be worn
The appearance of wearing electronic device has more pushed the development of carbon nano-fiber.
The preparation method of traditional carbon nano-fiber is with fossil energy such as polyacrylonitrile, pitch etc. for raw material, however its
Production and application process in can cause environmental pollution, and due to its fossil energy it is non-renewable the problems such as presence,
It is largely limited further to develop.Therefore, using renewable, free of contamination natural resources as raw material, develop it is environmental-friendly,
Cheap synthesis technology will have and its important role.
Summary of the invention:
The technical issues of solution: the present invention provides a kind of nanoporous carbon fiber and preparation method thereof method, and this method has step
Simply, green non-pollution, feature low in cost, and the flexible, porous carbon nano-fiber synthesized has bent, specific surface
The advantages that product is big, degree of graphitization is high, shows good chemical property as electrode material for super capacitor.
Technical solution: nanoporous carbon fiber production method, including following synthesis step: (1) certain density sea is prepared
Alginic acid sodium water solution, stirs to clarify, and a certain amount of molysite aqueous solution is then slowly added dropwise under conditions of being stirred continuously, and continues
2h is stirred to being uniformly mixed, is freeze-dried；(2) under nitrogen protection, control tube furnace heating rate is 5 DEG C/min, 600
1h is carbonized at DEG C -900 DEG C, cooled to room temperature is taken out, and clean 1h with 4M HCl, then filtering is washed with deionized
To neutrality, 80 DEG C of drying 12h obtain flexible, porous carbon nano-fiber.
Preferably, it is 1% that above-mentioned sodium alginate aqueous solution, which is mass concentration,.
Preferably, above-mentioned molysite aqueous solution is the FeCl that mass concentration is 1%2Aqueous solution, dosage are sodium alginate aqueous solution
The 50% of volume.
Preferably, the time of above-mentioned freeze-drying is 48h.
Preferably, above-mentioned carbonization temperature is respectively 600 DEG C, 700 DEG C, 800 DEG C, 900 DEG C.
Nanoporous carbon fiber made from above-mentioned preparation method.
Application of the above-mentioned flexible, porous carbon nano-fiber materials in supercapacitor.
Flexible, porous carbon nano-fiber obtained by the present invention, the application in supercapacitor pass through electro-chemical test
To evaluate, the specific steps are as follows:
Sample powder is mixed with conductive agent (acetylene black) and binder (PTFE) with the mass ratio of 8:1:1, and is led to
It crosses and suitable ethanol wet is added, be sufficiently stirred and mud is made, and it is uniformly smeared on the working electrode (s, 50 DEG C of drying 5h,
It is tested in three electrode test systems, electrolyte is 6M KOH, and electro-chemical test project includes constant current charge-discharge, circulation
Volt-ampere curve, ac impedance measurement and cycle life test.
Key of the invention is that with metal ion chela can occur for a large amount of oxygen-containing functional group in sodium alginate molecular structure
Cooperation is used.Excessive Fe2+It is introduced as source metal, the macromolecular of its every two chain is made by the chelation with sodium alginate
A referred to as chain is connected in a manner of zipping, therefore increases its physical strength, avoids single flexible chain
Molecule is reunited in carbonization process, it is hereby achieved that the carbon nano-fiber that pattern remains intact.Hydrochloric acid cleaning can fill
The removal metal oxide particle divided, generates a large amount of hole.
The utility model has the advantages that Fe2+Introducing the every two single chain molecules of sodium alginate can organically form to one, increase
Its strong mechanical strength, can effectively avoid the bending in carbonization process from reuniting, effectively keep its linear structure；With metal
Particle comes into full contact with the effect that can fully play its catalyzed graphitization, obtains the higher carbon Nanowire of degree of graphitization
Dimension, to improve its ability for transmitting electronics；A large amount of hole can be generated in the wash-off of metal, effective to improve carbon Nanowire
The specific surface area of dimension, to increase its specific capacitance.
Detailed description of the invention
Fig. 1 is the nanoporous carbon fiber transmission electron microscope picture that embodiment 2 obtains；
Fig. 2 is that the nanoporous carbon fiber high magnification that embodiment 2 obtains projects electron microscope；
Fig. 3 is constant current charge-discharge curve of the embodiment 2 under different current densities.
Specific embodiment
Preferably to illustrate the present invention to reach the technical means and efficacy that predetermined goal of the invention is taken, below by tool
Body embodiment and attached drawing are illustrated.
Embodiment 1
At room temperature, 100mg sodium alginate powder is added in the distilled water of 10mL, and stirring 3h dissolution obtains clear solution, then
Prepare the FeCl that 50mL mass concentration is 1%2Solution is slowly dropped in the sodium alginate soln being stirred continuously with needle tubing, is continued
Stirring two hours, is poured into surface plate, is freeze-dried 48h.Sample after drying is placed in tube furnace, under nitrogen protection, control
Heating rate processed be 5 DEG C/min be cooled to room temperature in 600 DEG C of charing 1h, clean 1h with 4M HCl, filtering, then spend from
Sub- water washing obtains flexible, porous carbon nano-fiber to neutrality, 80 DEG C of drying 12h.
Embodiment 2
At room temperature, 100mg sodium alginate powder is added in the distilled water of 10mL, and stirring 3h dissolution obtains clear solution, then
Prepare the FeCl that 50mL mass concentration is 1%2Solution is slowly dropped in the sodium alginate soln being stirred continuously with needle tubing, is continued
Stirring two hours, is poured into surface plate, is freeze-dried 48h.Sample after drying is placed in tube furnace, under nitrogen protection, control
Heating rate processed be 5 DEG C/min be cooled to room temperature in 700 DEG C of charing 1h, clean 1h with 4M HCl, filtering, then spend from
Sub- water washing obtains flexible, porous carbon nano-fiber to neutrality, 80 DEG C of drying 12h.
Embodiment 3
At room temperature, 100mg sodium alginate powder is added in the distilled water of 10mL, and stirring 3h dissolution obtains clear solution, then
Prepare the FeCl that 50mL mass concentration is 1%2Solution is slowly dropped in the sodium alginate soln being stirred continuously with needle tubing, is continued
Stirring two hours, is poured into surface plate, is freeze-dried 48h.Sample after drying is placed in tube furnace, under nitrogen protection, control
Heating rate processed be 5 DEG C/min be cooled to room temperature in 800 DEG C of charing 1h, clean 1h with 4M HCl, filtering, then spend from
Sub- water washing obtains flexible, porous carbon nano-fiber to neutrality, 80 DEG C of drying 12h.
Embodiment 4
At room temperature, 100mg sodium alginate powder is added in the distilled water of 10mL, and stirring 3h dissolution obtains clear solution, then
Prepare the FeCl that 50mL mass concentration is 1%2Solution is slowly dropped in the sodium alginate soln being stirred continuously with needle tubing, is continued
Stirring two hours, is poured into surface plate, is freeze-dried 48h.Sample after drying is placed in tube furnace, under nitrogen protection, control
Heating rate processed be 5 DEG C/min be cooled to room temperature in 900 DEG C of charing 1h, clean 1h with 4M HCl, filtering, then spend from
Sub- water washing obtains flexible, porous carbon nano-fiber to neutrality, 80 DEG C of drying 12h.
Technical solution of the present invention is described in detail in above-described embodiment, it should be understood that more than
Described is only presently preferred embodiments of the present invention, is not intended to restrict the invention, any person skilled in the art, is not taking off
From within the scope of technical solution of the present invention, when the technology contents using the disclosure above make few modifications or are modified to equivalent variations
Equivalent embodiment, still, it is all done in spirit of the invention it is any modify or improve, should be included in this hair
Within the scope of bright.
Claims (4)
1. nanoporous carbon fiber and preparation method thereof, it is characterised in that including following synthesis step:
Certain density sodium alginate aqueous solution is prepared, stirs 3-4h at room temperature to clarification, then under conditions of being stirred continuously
Molysite aqueous solution is added, continues to stir 2h, imports surface plate, be freeze-dried 48h；
Under nitrogen protection, the heating rate for controlling tube furnace is 5 DEG C/min, under conditions of carbonization temperature is 600 DEG C -900 DEG C
1h is carbonized to sample obtained in step (1), after cooling to room temperature, cleans 1h with 4M HCl, filters, then uses deionized water
It washs to neutrality.
2. according to nanoporous carbon fiber and preparation method thereof described in claim 1, it is characterised in that the sodium alginate is water-soluble
Liquid concentration is 1%.
3. according to nanoporous carbon fiber and preparation method thereof described in claim 1, it is characterised in that the molysite aqueous solution is
The FeCl that mass concentration is 1%2Aqueous solution, the amount for the solution being added are the half of the volume of sodium alginate aqueous solution.
4. according to nanoporous carbon fiber and preparation method thereof described in claim 1, it is characterised in that the carbonization temperature difference
It is 600 DEG C, 700 DEG C, 800 DEG C and 900 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021007183A1 (en) * | 2019-07-05 | 2021-01-14 | Nicolo Brambilla | Electrodes for energy storage devices |
| CN112794323A (en) * | 2021-01-08 | 2021-05-14 | 上海应用技术大学 | Nitrogen-sulfur-doped nano porous carbon material with sodium alginate as raw material and preparation method thereof |
| CN113308763A (en) * | 2021-05-21 | 2021-08-27 | 青海师范大学 | Method and device for preparing mesoporous nanotube by combining centrifugal spinning with chelating coordination reaction |
| CN114420468A (en) * | 2022-01-25 | 2022-04-29 | 四川金汇能新材料股份有限公司 | Porous carbon nanofiber and preparation method and application thereof |
| US11450488B2 (en) | 2016-12-02 | 2022-09-20 | Fastcap Systems Corporation | Composite electrode |
| US11848449B2 (en) | 2019-07-05 | 2023-12-19 | Fastcap Systems Corporation | Electrodes for energy storage devices |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11450488B2 (en) | 2016-12-02 | 2022-09-20 | Fastcap Systems Corporation | Composite electrode |
| WO2021007183A1 (en) * | 2019-07-05 | 2021-01-14 | Nicolo Brambilla | Electrodes for energy storage devices |
| US11848449B2 (en) | 2019-07-05 | 2023-12-19 | Fastcap Systems Corporation | Electrodes for energy storage devices |
| CN112794323A (en) * | 2021-01-08 | 2021-05-14 | 上海应用技术大学 | Nitrogen-sulfur-doped nano porous carbon material with sodium alginate as raw material and preparation method thereof |
| CN113308763A (en) * | 2021-05-21 | 2021-08-27 | 青海师范大学 | Method and device for preparing mesoporous nanotube by combining centrifugal spinning with chelating coordination reaction |
| CN114420468A (en) * | 2022-01-25 | 2022-04-29 | 四川金汇能新材料股份有限公司 | Porous carbon nanofiber and preparation method and application thereof |
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