CN105845451A - Supercapacitor electrode materials based on plant fiber base and preparation method thereof - Google Patents
Supercapacitor electrode materials based on plant fiber base and preparation method thereof Download PDFInfo
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- CN105845451A CN105845451A CN201610269460.3A CN201610269460A CN105845451A CN 105845451 A CN105845451 A CN 105845451A CN 201610269460 A CN201610269460 A CN 201610269460A CN 105845451 A CN105845451 A CN 105845451A
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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
-
- 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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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
- H01G11/46—Metal oxides
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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
-
- 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 present invention relates to a supercapacitor electrode materials based on a plant fiber base and a preparation method thereof. Carbonized plant fibers, namely carbon fibers are taken as a substrate, CNTs with high conductivity, high specific surface area and different capacities are generated at the surface in-site of monofilament carbon fibers through adoption of a CVD method, and nanocrystalline metal oxides with different morphologies are directly prepared at the surface of the CNTs through adoption of a hydrothermal method, so that the electrode materials with the nanometer multistage composite structure are realized and are able to reduce the resistance of electrodes and provide a rapid diffusion path for ions in the electrolyte to allow the electrode material to display the excellent electrochemical performance.
Description
Technical field
The invention belongs to the technical field of electrode material for super capacitor, be specifically related to relate to a kind of nanometer hierarchical structure nano electrode material based on string and preparation method thereof.
Background technology
Along with increasingly sharpening of the fast development of global economy, the exhaustion of fossil fuel, and environmental pollution, therefore in the urgent need to high power, environmental friendliness, the continuable energy solves current problem encountered.Ultracapacitor has caused substantial amounts of concern owing to having high power density, quick discharge and recharge, long cycle period and low cost.So research electrode material for super capacitor is to solve the energy and one of them main method of environmental problem now.Electrode material is mixed by traditional ultracapacitor the most by a certain percentage with binding agent and conducting objects, the capacitive property of this ultracapacitor reduced greatly.Therefore from the energy density of electrode material for super capacitor, power density and cost consideration, a kind of self-supporting is probed into, binder free, environmental friendliness, the electrode material for super capacitor of low cost have potential using value.String is owing to having its low cost, environmental friendliness, light weight and the pore-size distribution characteristic such as rationally so that string has great advantage as electrode material for super capacitor three-dimensional conductive network substrates.
In current research, the foam of polymers of business and sponge, cellulose paper, bafta have had shown that certain using value in electrode material for super capacitor.But use these to yet suffer from substantial amounts of deficiency as electrode material for super capacitor, cellulose paper and bafta are only capable of the self-supporter as electrode material, and to need to introduce CNTs and the Graphene etc. of high connductivity as the three-dimensional conductive body of electrode material.And the most most of methods at plant fibre surface introducing CNTs are all the dippings of carbon nano-tube solution, due to CNT bad dispersibility, although adding the dispersion of auxiliary agent beneficially CNTs, but affect the performance of intrinsic, such as crystallinity, draw ratio etc..This will can not give full play to the CNTs characteristic as electrode material for super capacitor.And the string studied at present/CNTs electrode material only has high power density, and compared with battery, energy density is the lowest.
Original position on CNTs surface introduces nano-metal-oxide, it is possible to achieve its nanometer hierarchical hierarchy, can be effectively improved the utilization rate of active material, increases specific surface area, improves the diffusion mass transfer performance of material.Improve the power density of its electrode material, and eliminate the use of additive material, eliminate the suppression process to electrode.This simple process is easy, environmental protection, is expected to be with a wide range of applications in energy storage field.
Summary of the invention
Solve the technical problem that
In place of the deficiencies in the prior art, the present invention proposes a kind of nanometer hierarchical structure nano electrode material based on string and preparation method thereof, prepare the CNTs/ string/metal oxide ultracapacitor multilevel hierarchy electrode material of the three-dimensional conductive network structure of binder free, low cost, environmental friendliness, self-supporting, to solve the binding agent in existing electrode material for super capacitor and the conductive agent impact on performance, and on string, realize its nanometer hierarchy.
Technical scheme
A kind of based on plant fiber-based electrode material for super capacitor, it is characterised in that to include string substrate, CNTs and metal oxide after carbonization；String substrate overlying in the carbonized is stamped CNTs, is provided with metal oxide on CNTs.
A kind of preparation method based on plant fiber-based electrode material for super capacitor, it is characterised in that step is as follows:
Growth in situ high connductivity, high-specific surface area CNTs on step 1, string in the carbonized:
String after carbonization be impregnated in the Ni (NO of 0.005～0.1M3)3. deionized water solution, vacuum outgas makes solution impregnation in micropore, then takes out and be dried to mass fraction water content in the environment of 60～120 DEG C less than 5%；
Use and on CVD carbon fiber surface after impregnating, prepare CNTs/ carbon fiber; CVD growth condition is: with ethene as carbon source; reaction temperature is at 700-800 DEG C, and temperature retention time is 0-30min, using hydrogen and argon gas gaseous mixture as carrier gas; the volume ratio of its hydrogen is 10-20%; reaction time is 10-20min, after question response completes, is cooled to less than 100 DEG C under Ar protects; CNTs/ carbon fibre composite, the mass fraction of CNTs be carbon fiber 50 to；500%, specific surface area is higher than 300m2/g；
Step 2, preparation CNTs/ string/MnO2Nanometer combined electrode: be placed in autoclave by CNTs/ carbon fibre composite, reaction solution is the KMnO of 0.001～0.01M4, at 60-200 DEG C, react 2-12h, obtain the fiber after oxide is combined；
Use deionized water rinsing multipass, prepare nanometer MnO of different-shape2/ CNTs/ carbon fiber/combination electrode material, the mass fraction of oxide is the 30～70% of overall electrode material.
The employing deionized water rinsing multipass of described step 2 is 3 times.
String after described carbonization is that string carries out carbonization, and carbonization technique step is:
Step 1: string braid be impregnated in distilled water, is heated to 120-200 DEG C with 5-10 DEG C/min in an oven, is incubated 30-60min, after temperature is cooled to room temperature, with deionized water rinsing, then in 80 DEG C of baking ovens, is dried；
Step 2: dried string braid is carried out in inert atmosphere stove carbonization, heating rate is 5-20 DEG C/min, and carburizing temperature is 800-1000 DEG C, carbonization time 60-200min；After carbonization completes, under Ar gas shielded, it is cooled to room temperature, obtains the string after carbonization.
Beneficial effect
A kind of based on string nanometer hierarchical structure nano electrode material that the present invention proposes and preparation method thereof, it is substrate by the string of carbonization i.e. carbon fiber, CVD realizes at monofilament carbon fiber surface growth in situ high connductivity, high-specific surface area, the CNTs of different loads amount, hydro-thermal method directly prepares the nano-metal-oxide of different-shape on CNTs surface, thus realize its electrode material with nanometer hierarchical composite construction, this plant fiber-based nanometer hierarchical structure electrode material can reduce the internal resistance of electrode, and provide quick diffusion admittance for electrolyte intermediate ion, electrode material is made to demonstrate the chemical property of excellence.
Accompanying drawing explanation
Fig. 1 is to prepare CNTs/ string/MnO2The manufacture craft schematic diagram of combination electrode
Fig. 2 is CNTs/ string/MnO2Combined electrode structure schematic diagram
Fig. 3 is the high power SEM schematic diagram of flax fiber after carbonization
Fig. 4 is the EDS analysis chart of flax fiber after carbonization
Fig. 5 is the high power SEM schematic diagram of flax fiber growth CNTs after carbonization
Fig. 6 is CNTs/ flax fiber/MnO2High power SEM schematic diagram
Fig. 7 is CNTs/ flax fiber/MnO2EDS analysis chart
Fig. 8 is CNTs/ flax fiber/MnO2Constant current charge-discharge figure
Detailed description of the invention
In conjunction with embodiment, accompanying drawing, the invention will be further described:
Specific embodiment 1:
Carbonate plant fiber concrete steps:
(1) string braid dipping distilled water, puts in baking oven, is heated to 120-200 DEG C with 5-10 DEG C/min, is incubated 30-60min, after temperature is cooled to room temperature, and, with deionized water rinsing, it is then placed in the baking oven of 80 DEG C, is dried.
(2) braid dried in step 1 is carried out carbonization in inert atmosphere stove; heating rate is 5-20 DEG C/min; carburizing temperature is 800-1000 DEG C; carbonization time 60-200min; make its abundant carbonization, after carbonization completes, under Ar gas shielded, be cooled to room temperature; obtain the string after carbonization, i.e. carbon fiber.Fig. 2 is SEM figure after carbonization completes, and Fig. 3 is that carbon fiber is carried out EDS analysis, and carbon content is 100%, for the 15% of original flax fiber.
Prepared by CNTs/ carbon fiber combination electrode
(1) by carbonate plant fiber impregnation in the Ni (NO of 0.005～0.1M3)3. deionized water solution, vacuum outgas, it is ensured that solution impregnation, in micropore, then takes out and is dried to mass fraction water content in the environment of 60～120 DEG C less than 5%.
(2) CNTs/ carbon fiber will be prepared by CVD on the carbon fiber surface of impregnated catalyst, CVD growth condition is: with ethene as carbon source, reaction temperature is at 700-800 DEG C, temperature retention time is 0-30min, using hydrogen and argon gas gaseous mixture as carrier gas, the volume ratio of its hydrogen is 10-20%, and the reaction time is 10-20min.After question response completes, it is cooled to less than 100 DEG C under Ar protects.Obtain CNTs/ carbon fibre composite, mass fraction is carbon fiber the 50 to 500% of CNTs.Specific surface area is higher than 300m2/ g, at the SEM of grown on carbon fibers CNTs as shown in 4 figures.
CNTs/ flax fiber/MnO2The preparation of nanometer combined electrode
(1) CNTs/ carbon fibre composite is placed in reaction solution in autoclave is the KMnO of 0.001～0.01M4, at 60-100 DEG C, react 2-12h, the deionized water rinsing three times of the fiber after oxide is compound, prepare acicular nanometer MnO2/ CNTs/ carbon fiber/combination electrode material.The mass fraction of oxide is the 30～70% of overall electrode material.At CNTs superficial growth MnO2SEM and EDS as shown in 5 and 6 figures, constant current charge-discharge is as shown in 7 figures
Specific embodiment 2:
The carbonization technique of string is identical with the carbonization technique in embodiment 1, and CNTs growth time on carbon fiber is 20min, obtains the CNTs/ string nanometer combined electrode with different loads amount.With needle-like MnO2Combination process identical with embodiment 1.
Specific embodiment 3:
The carbonization technique of string is identical with the carbonization technique in embodiment 1, and the CNTs technique being grown on specific embodiment 1 on carbon fiber is identical, except for the difference that MnO2Pattern, it is the KMnO of 0.001～0.01M that CNTs/ carbon fibre composite is placed in reaction solution in autoclave4, at 100-200 DEG C, react 2-12h, being prepared for is the MnO of tubulose2
Specific embodiment 4:
The carbonization technique of string is identical with the carbonization technique in embodiment 1, and CNTs growth time on carbon fiber is 20min, obtains the CNTs/ string nanometer combined electrode with different loads amount.With tubulose MnO2Combination process identical with embodiment 3.
Described nano-metal-oxide can prepare tubulose, sheet, acicular texture according to hydrothermal condition change.
Claims (4)
1. one kind based on plant fiber-based electrode material for super capacitor, it is characterised in that include the plant fiber-based after carbonization
The end, CNTs and metal oxide；String substrate overlying in the carbonized is stamped CNTs, on CNTs
It is provided with metal oxide.
2. a preparation method based on plant fiber-based electrode material for super capacitor, it is characterised in that step is as follows:
Growth in situ high connductivity, high-specific surface area CNTs on step 1, string in the carbonized:
String after carbonization be impregnated in the Ni (NO of 0.005～0.1M3)3. deionized water solution, vacuum outgas makes
Solution impregnation in micropore, then take out and in the environment of 60～120 DEG C, be dried to mass fraction water content less than 5%；
Using and prepare CNTs/ carbon fiber on CVD carbon fiber surface after impregnating, CVD growth condition is: with
Ethene is carbon source, and reaction temperature is at 700-800 DEG C, and temperature retention time is 0-30min, using hydrogen and argon gas gaseous mixture as
Carrier gas, the volume ratio of its hydrogen is 10-20%, and the reaction time is 10-20min, after question response completes, protects at Ar
Under be cooled to, less than 100 DEG C, obtain CNTs/ carbon fibre composite；
Step 2, preparation CNTs/ string/MnO2Nanometer combined electrode: CNTs/ carbon fibre composite is placed in
In autoclave, reaction solution is the KMnO of 0.001～0.01M4, at 60-200 DEG C, react 2-12h, obtain
Fiber after oxide is compound；
Use deionized water rinsing multipass, prepare nanometer MnO2/ CNTs/ carbon fiber/combination electrode material.
Preparation method the most according to claim 2, it is characterised in that: the employing deionized water rinsing of described step 2
Multipass is 3 times.
The most according to claim 1 based on described in plant fiber-based electrode material for super capacitor or claim 2
Preparation method, it is characterised in that: the string after described carbonization is that string is carried out carbonization, carbonizer
Skill step is:
Step 1: string braid be impregnated in distilled water, is heated to 5-10 DEG C/min in an oven
120-200 DEG C, it is incubated 30-60min, after temperature is cooled to room temperature, with deionized water rinsing, then 80 DEG C of bakings
In case, it is dried；
Step 2: dried string braid is carried out in inert atmosphere stove carbonization, heating rate is 5-20 DEG C
/ min, carburizing temperature is 800-1000 DEG C, carbonization time 60-200min；After carbonization completes, under Ar gas shielded
It is cooled to room temperature, obtains the string after carbonization.
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| CN107578926A (en) * | 2017-07-20 | 2018-01-12 | 西北工业大学 | The preparation method of carbon fiber transition metal carbon nano tube flexible nanometer combined electrode material |
| CN107938323A (en) * | 2018-01-03 | 2018-04-20 | 北京北方国能科技有限公司 | A kind of graphene carbon fiber, its preparation method and its application |
| CN108147504A (en) * | 2017-11-22 | 2018-06-12 | 广东信丰达环保科技有限公司 | Electroactive reaction cloth and preparation method thereof |
| CN108264034A (en) * | 2018-02-06 | 2018-07-10 | 陕西师范大学 | The method of growth spiral shape carbon nanotube on the porous carbon of timber |
| CN109930140A (en) * | 2019-03-21 | 2019-06-25 | 南昌航空大学 | A kind of preparation method of flexible electrode |
| CN110233054A (en) * | 2019-05-22 | 2019-09-13 | 中南林业科技大学 | A kind of Asymmetric Supercapacitor and preparation method thereof |
| CN110229627A (en) * | 2019-06-20 | 2019-09-13 | 深圳昌茂粘胶新材料有限公司 | Double Antistatic protective films of a kind of silica gel and preparation method thereof |
| CN111408282A (en) * | 2020-04-29 | 2020-07-14 | 郑州大学 | Carbon nanotube/carbon nanofiber composite film and preparation method and application thereof |
| CN112086299A (en) * | 2020-09-30 | 2020-12-15 | 华南理工大学 | Flexible thin film electrode material of super capacitor and preparation method thereof |
| CN113223873A (en) * | 2021-05-13 | 2021-08-06 | 百色学院 | Preparation method of plant fiber doped and polymerization modified activated carbon electrode |
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Cited By (13)
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| CN107578926A (en) * | 2017-07-20 | 2018-01-12 | 西北工业大学 | The preparation method of carbon fiber transition metal carbon nano tube flexible nanometer combined electrode material |
| CN108147504A (en) * | 2017-11-22 | 2018-06-12 | 广东信丰达环保科技有限公司 | Electroactive reaction cloth and preparation method thereof |
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| CN109930140A (en) * | 2019-03-21 | 2019-06-25 | 南昌航空大学 | A kind of preparation method of flexible electrode |
| CN110233054A (en) * | 2019-05-22 | 2019-09-13 | 中南林业科技大学 | A kind of Asymmetric Supercapacitor and preparation method thereof |
| CN110233054B (en) * | 2019-05-22 | 2021-05-28 | 中南林业科技大学 | Asymmetric super capacitor and preparation method thereof |
| CN110229627A (en) * | 2019-06-20 | 2019-09-13 | 深圳昌茂粘胶新材料有限公司 | Double Antistatic protective films of a kind of silica gel and preparation method thereof |
| CN111408282A (en) * | 2020-04-29 | 2020-07-14 | 郑州大学 | Carbon nanotube/carbon nanofiber composite film and preparation method and application thereof |
| CN112086299A (en) * | 2020-09-30 | 2020-12-15 | 华南理工大学 | Flexible thin film electrode material of super capacitor and preparation method thereof |
| CN112086299B (en) * | 2020-09-30 | 2022-04-22 | 华南理工大学 | Flexible thin film electrode material of super capacitor and preparation method thereof |
| CN113223873A (en) * | 2021-05-13 | 2021-08-06 | 百色学院 | Preparation method of plant fiber doped and polymerization modified activated carbon electrode |
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