CN110233065A - The preparation method of complex carbon material flexible super capacitance electrode - Google Patents
The preparation method of complex carbon material flexible super capacitance electrode Download PDFInfo
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- CN110233065A CN110233065A CN201910385381.2A CN201910385381A CN110233065A CN 110233065 A CN110233065 A CN 110233065A CN 201910385381 A CN201910385381 A CN 201910385381A CN 110233065 A CN110233065 A CN 110233065A
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- carbon material
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- capacitance electrode
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- super capacitance
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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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- 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 kind of preparation methods of complex carbon material flexible super capacitance electrode, and described method includes following steps: Step 1: carrying out ball mill grinding processing to coal-based carbon material using ball mill；Step 2: carrying out pickling and deionized water carrying out washing treatment to the coal-based carbon material after ball mill grinding；Step 3: ultrasonic disperse in deionized water is added in treated coal-based carbon material and inorganic binder, configuration crushes coal-based carbon material dispersion liquid；Step 4: ultrasonic disperse pretreatment is carried out to carbon cloth using aqueous solutions of organic solvent, it is spare after dry；Step 5: vacuum filtration crushes coal-based carbon material dispersion liquid, up to coal-based carbon material based flexible super capacitance electrode after drying using pretreated carbon cloth as substrate.Electrode slice prepared by the present invention has good flexible, uniform active material distribution, good capacitive property, and processes, is easy to operate, and simple process, fabrication cycle is short, is expected to realize large-scale industry preparation.
Description
Technical field
The invention belongs to electrochemical energy storage technical fields, are related to a kind of preparation method of flexible super capacitance electrode, specifically
It is related to a kind of preparation method of coal-based carbon material flexibility super capacitor electrode.
Background technique
With the raising that people require the properties of product such as intelligent electronic device, intelligent clothing, all kinds of flexible wearable electricity
Sub- equipment occurs in succession.And in many energy storage devices, supercapacitor is due to meeting the features such as " safety ", " service life is long ", quilt
Extensive concern.This kind of flexibility energy storage devices include the forms such as sandwich type, interdigitation, cable-type, threadiness, threadiness at present,
Wherein sandwich type supercapacitor is stacked formed alternatively up and down by positive and negative electrode, solid electrolyte, and configuration is simple and reliable, is easy to
Preparation and maintenance, and it is preferable with describing property of clothing.In order to more adapt to the demand for development of flexible electronic, design and develop with
The flexible high-performance super capacitor to match become current research hotspot.
The core link of flexible super capacitor preparation is designing and preparing for flexible electrode.Supercapacitor is a kind of
The device of energy storage is carried out based on electrode interface double electrical layers, and porous carbon materials are since hole is abundant, structure is easy to regulate and control, machine
Tool is had excellent performance, and is widely studied the flexible electrode material for doing supercapacitor.In the past mostly using vapour deposition process, spray coating method,
Active material is supported on flexible current-collecting body component and obtains the porous carbon of self-supporting, macrostructure by the preparation methods such as print process
Material.Conventional method generally passes through the deposition that the conditions such as redox reaction or high temperature, high pressure carry out active material, need to additionally draw
Enter chemical reagent or more exacting terms is provided.
Summary of the invention
When for the production cost for saving flexible electrode, the preparation process for simplifying flexible electrode, reduction flexible electrode manufacture
High requirement, the application field for widening flexible electrode to a greater extent to device, the present invention provides a kind of compound carbon materials
Expect the preparation method of flexible super capacitance electrode.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation method of complex carbon material flexible super capacitance electrode, by the coal-based carbon material for introducing binder and crushing
Slurries are made, it is directly supported by way of vacuum filtration to electroactive substance on a current collector, and then is significantly simple
Change flexible electrode preparation process.Specifically comprise the following steps:
Step 1: carrying out ball mill grinding processing to coal-based carbon material using ball mill, core purpose is to introduce oxygen-containing function
Group, enables carbon material to be preferably scattered in dispersion liquid；
In this step, mill ball used in the ball mill is stainless-steel grinding ball, in corundum mill ball, hard alloy mill ball
One kind, preferably mill ball are stainless-steel grinding ball.
In this step, the ball mill grinding time is 0 ~ 48h.
Step 2: carrying out pickling and deionized water carrying out washing treatment to the coal-based carbon material after step 1 ball mill grinding；
In this step, when pickling a length of 8 ~ 48h.
In this step, the spent pickling acid is the one or more of the hydrochloric acid of 0.1 ~ 1mol/L, sulfuric acid, hydrofluoric acid, preferably
Spent pickling acid is hydrochloric acid.
Step 3: ultrasonic disperse in deionized water is added in step 2 treated coal-based carbon material and inorganic binder,
Configuration crushes coal-based carbon material dispersion liquid；
In this step, the inorganic binder is one of CMC, PVDF, and preferably inorganic binder is CMC.
In this step, the additional amount of the inorganic binder is the 5 ~ 10% of dispersion liquid gross mass, and the amount of being preferably added to is dispersion
The 5% of liquid gross mass.
In this step, the mass ratio of the coal-based carbon material and deionized water is 1:1 ~ 1:3, and preferred mass ratio is 1:3.
In this step, the ultrasonic disperse time is 0.1 ~ 3h, and the preferably ultrasonic disperse time is 3h.
Step 4: ultrasonic disperse pretreatment is carried out to carbon cloth using aqueous solutions of organic solvent, it is spare after dry；
In this step, the organic solvent is the one or two of ethyl alcohol, acetone, other lower alcohols or ketone, preferably organic
Solvent is ethyl alcohol.
In this step, the volume ratio of organic solvent and deionized water is 1:3 ~ 3:1 in the aqueous solutions of organic solvent, preferably
Volume ratio is 1:1.
In this step, the ultrasonic disperse time is 1 ~ 3h, and the preferably ultrasonic disperse time is 3h.
In this step, the drying temperature is 20 ~ 80 DEG C, and drying time is 4 ~ 12h, and preferably drying temperature is 20 DEG C, is done
The dry time is 8h.
Step 5: using the pretreated carbon cloth of step 4 as substrate, the crushing coal-based carbon material of vacuum filtration step 3 preparation
Dispersion liquid is expected, up to coal-based carbon material based flexible super capacitance electrode after drying.
In this step, when crushing coal-based carbon material dispersion liquid is filtered by vacuum using instillation mode, dispersion liquid is placed in
It is filtered by vacuum in overall process and is constantly in ultrasonic disperse state；Coal-based carbon material dispersion liquid is crushed to use
When the mode of pouring into is filtered by vacuum, graduated cylinder should be placed in the dispersion liquid progress in ultrasonic disperse machine to measurement after entering graduated cylinder by liquid relief
Ultrasonic disperse.
Compared with the prior art, the present invention has the advantage that
The present invention is directly supported processed coal-based carbon material on carbon cloth by way of vacuum filtration, passes through vacuum filtration
The electrode slice of method preparation has good flexible, uniform active material distribution, good capacitive property, and chemistry is greatly saved
The loss of raw material simplifies the production process of pole plate, requirement when reducing pole plate manufacture to device condition, and processes, behaviour
Make simplicity, simple process, fabrication cycle is short, is expected to realize large-scale industry preparation.
Detailed description of the invention
Fig. 1 is the preparation flow figure of complex carbon material flexible super capacitance electrode；
Fig. 2 is the quality that preceding dry carbon cloth is supported in embodiment 1 and the quality for supporting rear carbon cloth；
Fig. 3 is the quality that preceding dry carbon cloth is supported in embodiment 2 and the quality for supporting rear carbon cloth.
Specific embodiment
Below with reference to embodiment, further description of the technical solution of the present invention, and however, it is not limited to this, all right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be contained
Lid is within the protection scope of the present invention.
Embodiment 1:
As shown in Figure 1, the present embodiment prepares complex carbon material flexible super capacitance electrode in accordance with the following steps:
(1) 200mg coal-based carbon material is weighed, 1.5g dry ice is placed in planetary ball mill and crushes 48h；
(2) pickling 12h is carried out to smashed coal-based carbon material using the HCl solution of 0.5mol/L, pickling is placed on centrifuge
Middle centrifugation layering outwells and carries out washing 12h to sample using deionized water after the spent acid of upper layer, and washing, which is placed in centrifuge, to be centrifuged
Layering, outwells the deionized water on upper layer；
(3) repeat the pickling of step (2), after deionized water washing operation 2 times in drying at room temperature for 24 hours；
(4) ultrasonic disperse 1h in 45ml deionized water is added in coal-based carbon material, 5mg CMC solid after weighing 45mg drying；
(5) it cuts the carbon cloth that size is 2cm × 2cm size and is placed in ultrasonic disperse 1h in the solution of 200ml ethyl alcohol, 200ml water, surpass
Drying at room temperature 8h is taken out after sound dispersion, is weighed after dry；
(6) filter paper is placed in below carbon cloth and ultrasonic suction filtration is carried out to the dispersion liquid of step (4), dispersant liquid drop is fashionable, uses rubber head
Dropper drop by drop instills dispersion liquid, removes carbon cloth drying at room temperature 12h after instilling 10ml dispersion liquid, weighs after dry to get coal
Base carbon material based flexible super capacitance electrode.
As shown in Figure 2, dry carbon cloth instills dispersion liquid 10ml in total before supporting, in dispersion liquid there are 11.11mg(10ml ×
50mg/45ml) dispersate, has supported 5.97mg dispersate, and the rate of supporting is about 53.74%.
Embodiment 2:
The present embodiment prepares complex carbon material flexible super capacitance electrode in accordance with the following steps:
(1) 200mg coal-based carbon material is weighed, 1.5g dry ice is placed in planetary ball mill and crushes for 24 hours；
(2) pickling 8h is carried out to smashed sample using the HCl solution of 0.5mol/L, pickling is placed on centrifugation point in centrifuge
Layer is outwelled and carries out washing 8h to sample using deionized water after the spent acid of upper layer, and washing, which is placed in centrifuge, is centrifuged layering, outwells
After the deionized water on upper layer for 24 hours in drying at room temperature；
(3) ultrasonic disperse 1h in 45ml deionized water is added in coal-based carbon material, 5mg CMC solid after weighing 45mg drying；
(4) it cuts the carbon cloth that size is 2cm × 2cm size and is placed in ultrasonic disperse 1h in the solution of 250ml ethyl alcohol, 150ml water, surpass
Drying at room temperature 8h is taken out after sound dispersion, is weighed after dry；
(5) filter paper is placed in below carbon cloth and graduated cylinder is used when dispersion liquid is added to the ultrasonic suction filtration of dispersion liquid progress of step (4)
It is quickly poured into after precise 10ml dispersion liquid, carbon cloth drying at room temperature 12h is removed after suction filtration, is weighed after dry to get coal
Base carbon material based flexible super capacitance electrode.
From the figure 3, it may be seen that dry carbon cloth instills dispersion liquid 10ml in total before supporting, in dispersion liquid there are 11.11mg(10ml ×
50mg/45ml) dispersate, has supported 3.83mg dispersate, and the rate of supporting is about 34.47%.
Claims (10)
1. a kind of preparation method of complex carbon material flexible super capacitance electrode, it is characterised in that the method includes walking as follows
It is rapid:
Step 1: carrying out ball mill grinding processing to coal-based carbon material using ball mill；
Step 2: carrying out pickling and deionized water carrying out washing treatment to the coal-based carbon material after step 1 ball mill grinding；
Step 3: ultrasonic disperse in deionized water, configuration is added in step 2 treated coal-based carbon material and inorganic binder
Crush coal-based carbon material dispersion liquid；
Step 4: ultrasonic disperse pretreatment is carried out to carbon cloth using aqueous solutions of organic solvent, it is spare after dry；
Step 5: using the pretreated carbon cloth of step 4 as substrate, the crushing coal-based carbon material point of vacuum filtration step 3 configuration
Dispersion liquid, up to coal-based carbon material based flexible super capacitance electrode after drying.
2. the preparation method of complex carbon material flexible super capacitance electrode according to claim 1, it is characterised in that described
In step 1, mill ball used in ball mill is one of stainless-steel grinding ball, corundum mill ball, hard alloy mill ball；Ball
Mill grinding time is 0 ~ 48h.
3. the preparation method of complex carbon material flexible super capacitance electrode according to claim 1, it is characterised in that described
In step 2, when pickling a length of 8 ~ 48h；Spent pickling acid is the one or more of hydrochloric acid, sulfuric acid, hydrofluoric acid.
4. the preparation method of complex carbon material flexible super capacitance electrode according to claim 1, it is characterised in that described
In step 3, one of inorganic binder CMC, PVDF, additional amount are the 5 ~ 10% of dispersion liquid gross mass.
5. the preparation method of complex carbon material flexible super capacitance electrode according to claim 1, it is characterised in that described
In step 3, the mass ratio of coal-based carbon material and deionized water is 1:1 ~ 1:3.
6. the preparation method of complex carbon material flexible super capacitance electrode according to claim 1, it is characterised in that described
In step 3, the ultrasonic disperse time is 0.1 ~ 3h.
7. the preparation method of complex carbon material flexible super capacitance electrode according to claim 1, it is characterised in that described
In step 4, in aqueous solutions of organic solvent the volume ratio of organic solvent and deionized water be 1:3 ~ 3:1, organic solvent be ethyl alcohol,
The one or two of acetone, other lower alcohols or ketone.
8. the preparation method of complex carbon material flexible super capacitance electrode according to claim 1, it is characterised in that described
In step 4, the ultrasonic disperse time is 1 ~ 3h.
9. the preparation method of complex carbon material flexible super capacitance electrode according to claim 1, it is characterised in that described
In step 4, drying temperature is 20 ~ 80 DEG C, and drying time is 4 ~ 12h.
10. the preparation method of complex carbon material flexible super capacitance electrode according to claim 1, it is characterised in that described
In step 5, when crushing coal-based carbon material dispersion liquid is filtered by vacuum using instillation mode, dispersion liquid is placed in ultrasonic disperse
It is filtered by vacuum in overall process and is constantly in ultrasonic disperse state；Crushing coal-based carbon material dispersion liquid, which uses, pours into mode
When being filtered by vacuum, graduated cylinder should be placed in the dispersion liquid progress ultrasound point in ultrasonic disperse machine to measurement after entering graduated cylinder by liquid relief
It dissipates.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040246658A1 (en) * | 2001-02-26 | 2004-12-09 | Adrianov Michail N. | Electrode for electric double layer capacitor and method of fabrication thereof |
| CN102214514A (en) * | 2011-03-21 | 2011-10-12 | 中南大学 | Production method of high-specific-capacitance activated carbon electrode material for super capacitor |
| CN105521765A (en) * | 2015-12-30 | 2016-04-27 | 徐州深蓝新材料科技有限公司 | A preparing method of a graphene composite membrane adopting carbon fibers as a skeleton and applications of the composite membrane |
| CN109065368A (en) * | 2018-09-04 | 2018-12-21 | 北京邮电大学 | The flexible super capacitor and preparation method thereof of the heterogeneous nano-chip arrays structure of nickel sulfide-molybdenum sulfide based on carbon cloth load |
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2019
- 2019-05-09 CN CN201910385381.2A patent/CN110233065A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040246658A1 (en) * | 2001-02-26 | 2004-12-09 | Adrianov Michail N. | Electrode for electric double layer capacitor and method of fabrication thereof |
| CN102214514A (en) * | 2011-03-21 | 2011-10-12 | 中南大学 | Production method of high-specific-capacitance activated carbon electrode material for super capacitor |
| CN105521765A (en) * | 2015-12-30 | 2016-04-27 | 徐州深蓝新材料科技有限公司 | A preparing method of a graphene composite membrane adopting carbon fibers as a skeleton and applications of the composite membrane |
| CN109065368A (en) * | 2018-09-04 | 2018-12-21 | 北京邮电大学 | The flexible super capacitor and preparation method thereof of the heterogeneous nano-chip arrays structure of nickel sulfide-molybdenum sulfide based on carbon cloth load |
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| A. JANICEK,ET AL.: ""High Performance Activated Carbon/Carbon Cloth Cathodes for Microbial Fuel Cells"", 《FUEL CELLS》 * |
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Application publication date: 20190913 |