CN106128788B - A kind of supercapacitor and preparation method thereof - Google Patents
A kind of supercapacitor and preparation method thereof Download PDFInfo
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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 belongs to materials science fields, disclose a kind of supercapacitor and preparation method thereof, include the following steps: that positively charged Cationic retention aid aqueous solution is added in cellulose pulp by (1), stirs, obtain the fiber mixed pulp for being enclosed with retention agent；(2) graphene oxide water solution is mixed again with the fiber mixed pulp for being enclosed with retention agent, is slowly stirred, obtain graphene oxide cellulose mixed pulp；(3) by obtained mixed pulp, copy paper, press dewatering obtain graphene oxide/cellulose extrusion coating paper on manual handsheet machine after drying；(4) obtained extrusion coating paper addition reducing agent is reduced into graphene/cellulose extrusion coating paper；(5) above-mentioned extrusion coating paper is cut out, attached addition electrolyte and diaphragm are packaged fixation on a current collector, are assembled into symmetrical supercapacitor.Preparation process of the present invention is simple, and super capacitor quality obtained is slim and graceful, flexible.
Description
Technical field
The present invention relates to a kind of based on graphene/cellulose extrusion coating paper supercapacitor and preparation method thereof, belongs to super
Grade capacitor technology field.
Background technique
Supercapacitor is a kind of a kind of novel energy storage apparatus between physical capacitor and secondary cell.This dress
Set its energy savings and release during it is unique, be not only presented as burst rate charge and discharge process, while also having
There is the advantages of high-energy and high-specific-power, i.e., the charge and discharge time, only tens of seconds, power density were higher by 10- compared with battery
100 times；Energy density is then as many as 100 times of physical capacitor.
Graphene is single layer carbon molecules made of one kind is arranged and is connected with each other according to hexagon as carbon atom.Through grinding
Study carefully discovery, there is very excellent performance using graphene as the supercapacitor of electrode material.Research shows that Young's modulus is about
For 1100Gpa, breaking strength 125Gpa, mechanical strength 1060Gpa, thermal conductivity 5000W/mK, and have superior
Electron transport ability since graphene self-discovery, has caused the great interest of scientific circles, has been to study most popular material in recent years
One of material.The specific surface area of single-layer graphene can reach 2630m2/ g is highly desirable super capacitor energy-storage material.And
And using supercapacitor made of graphene, the charging time only needs several milliseconds.However, graphene-based super capacitor exists at present
There is graphenes during preparation the problem of being easy to happen reunion under van der Waals interaction and stacking, and is difficult to realize
Large-scale production under low cost.
Summary of the invention
The purpose of the present invention is to provide a kind of based on graphene/cellulose extrusion coating paper supercapacitor and its preparation side
Method.
According to one aspect of the present invention, a kind of preparation method of compound paper electrode of graphene/cellulose is provided, is wrapped
It includes: Cationic retention aid is added in cellulose pulp, stir after being sufficiently mixed, then graphene oxide water solution is added
Into above-mentioned paper pulp, after being uniformly mixed, copy paper shapes on the manual handsheet machine of paper.Dehydration and drying is squeezed under squeezer
After obtain graphene oxide/cellulose extrusion coating paper.It restores to obtain the compound paper electrode of graphene/cellulose using reducing agent.
A kind of preparation method of supercapacitor, includes the following steps:
(1) graphite oxide is added to the water, ultrasonic disperse obtains graphene oxide water solution；By positively charged sun
Ionic retention agent is added to the water, and stirs evenly, and obtains retention agent aqueous solution；Cellulose paper is added to the water, is discongested point
It dissipates, obtains cellulose pulp；
(2) retention agent aqueous solution is added in cellulose pulp, stirs (about 1~2min), obtains being enclosed with retention agent
Fiber mixed pulp；
(3) graphene oxide water solution is mixed again with the fiber mixed pulp for being enclosed with retention agent, is slowly stirred (about 2
~4min), obtain graphene oxide cellulose mixed pulp；
(4) by obtained mixed pulp on manual handsheet machine copy paper, press dewatering obtained after drying graphene oxide/
Cellulose extrusion coating paper；
(5) obtained extrusion coating paper addition reducing agent is reduced into graphene/cellulose extrusion coating paper；
(6) above-mentioned extrusion coating paper is cut out, it is attached that electrolyte is added and diaphragm is packaged fixation on a current collector,
It is assembled into symmetrical supercapacitor.
The concentration of step (1) graphene oxide water solution is 0.001~0.005g/ml；The concentration of retention agent aqueous solution is
0.0005~0.001g/ml.
Step (1) graphite oxide is prepared by Hummers or improved Hummers method.
Step (1) retention agent is cationic polyacrylamide, diallyl dimethyl ammoniumchloride, polyethyleneimine
One or more of with chitosan quaternary ammonium salt.
Step (1) the ultrasonic disperse ultrasonic cleaner or cell crushing instrument ultrasonic disperse, ultrasonic cleaner
Parameter Conditions are as follows: 50~60 DEG C, 80~100W ultrasound, 2~4h；The Parameter Conditions of cell crushing instrument be 30~60 DEG C, 400~
10~30min of 600W ultrasound.The stirring condition of the Cationic retention aid are as follows: 50~150rpm of revolving speed, 10~12h of time.
The stirring condition of the cellulose cardboard are as follows: 10000~20000 turns.
The stirring condition of step (1) described retention agent are as follows: 50~150rpm of revolving speed, 10~12h of time；The cellulose paper
Discongest condition are as follows: 10000~20000 turns.
The mass ratio of step (3) retention agent and graphite oxide is 0.4~4wt%, the mass ratio of graphite oxide and cellulose
For 0.3~16wt%.
Step (5) reducing condition is reductase 12-10h at 95 DEG C；Reducing agent is ascorbic acid, hydrazine hydrate and tea polyphenols
One or more of.
Collector described in step (6) is nickel foam, steel disc, titanium sheet or gold-plated polyethylene terephthalate (PET)
Film；The electrolyte is potassium hydroxide, sodium hydroxide, and the diaphragm is filter paper, polyvinyl alcohol gel.
Cellulose described in step (1) is cotton linter, needle wood pulp, broad-leaved wood pulp or waste paper.
Invention with existing technology, has the advantage that relatively
(1) present invention keeps graphene oxide using Cationic retention aid, avoids the loss of graphene oxide, and
And since Cationic retention aid has positive charge, can be made with the LBL self-assembly of fibrin fiber and graphene oxide
It obtains and is most uniformly dispersed in paper through restoring obtained graphene afterwards.
(2) present invention is compound by cellulose and graphene, during graphene can be adsorbed on cellulose fibre, Ke Yiyou
Prevent to effect the reunion between graphene.For prepared compound paper electrode with the property of graphene and cellulose, performance is excellent
It is different, such as the flexibility folding property of paper, the high mechanical performance of graphene, good electric conductivity etc..The super capacitor quality of preparation
Merrily and lightheartedly, flexible.
(3) the extrusion coating paper electrode material prepared by the present invention is from a wealth of sources, cheap, and preparation process is simple, Er Qieke
Directly to carry out on traditional paper technology, it is very easy to realize large scale preparation.
Detailed description of the invention
Fig. 1 is graphene/cellulose extrusion coating paper outside drawing prepared by embodiment 1.
Fig. 2 is graphene/cellulose extrusion coating paper scanning electron microscope (SEM) photograph prepared by embodiment 1.Graphite as we can see from the figure
Alkene is attached to the surface of fiber, effectively prevents the reunion between graphene.
Fig. 3 be graphene/cellulose extrusion coating paper square resistance prepared by embodiment 2 increase with different graphene contents and
The curve graph of reduction.
Fig. 4 is the picture of extrusion coating paper connection circuit lightening LED lamp prepared by embodiment 2.
Fig. 5 be embodiment 3 prepare based on graphene/cellulose extrusion coating paper super capacitor under different scanning rates
Cyclic voltammetric (CV) curve.
Fig. 6 be embodiment 3 prepare based on graphene/cellulose extrusion coating paper super capacitor under different current densities
Constant current charge-discharge curve.
Specific embodiment
The present invention is more specifically described in detail combined with specific embodiments below, but embodiments of the present invention are unlimited
Routine techniques progress can refer to for not specifically specified technological parameter in this.
Embodiment 1
(1) graphite oxide of 0.192g (improved Hummers method is prepared) is added to equipped with 80ml ultrapure water
In beaker, 20min is stirred evenly, then beaker is transferred in cell crushing instrument, it is then super with (30 DEG C, 400W) of cell crushing instrument
Sound 10min.Obtain the graphene oxide aqueous dispersions that graphene oxide concentration is 0.0024g/ml.
(2) it is added in Pulp dredger after shredding 2.208g old newsprint (after vacuum drying), 1000ml water is added and discongests
10000 turns.It obtains starching dense about 0.22% paper pulp.
(3) 0.01g cationic polyacrylamide is added in the beaker equipped with 10ml ultrapure water, is stirred on 100rpm
12h.Obtain the cationic polyacrylamide aqueous solution that concentration is about 0.001g/ml.
(4) it takes the cationic polyacrylamide aqueous solution in 3.84ml (3) to be added in the cellulose pulp of (2), uses glass
Glass stick is slowly stirred 2min.Then the graphene oxide aqueous dispersions in (1) are added, then glass bar is slowly stirred 4min.Finally
The manual handsheet machine copy paper forming of mixed pulp conversion paper, it is about 120g/m that grammes per square metre is obtained after squeezing and drying2Aoxidize stone
The extrusion coating paper of black alkene content about 8%.
(5) extrusion coating paper is cut into 1cm × 1cm size with scissors, impregnates in water, 1ml hydrazine hydrate solution is added, 95
Reductase 12 h at DEG C, obtained paper dry spare after washing away excessive hydrazine hydrate with ultrapure water.
(6) the compound paper electrode of the graphene obtained after reduction is attached in nickel foam, uses filter paper as diaphragm, instills 6M hydrogen
Potassium oxide is assembled into super capacitor as electrolyte, by two pieces of electrode materials.
Embodiment 2
(1) graphite oxide of 0.192g (improved Hummers method is prepared) is added to equipped with 80ml ultrapure water
In beaker, 20min is stirred evenly, beaker is then transferred to ultrasonic cleaner, 80W, 60 DEG C of ultrasound 2h.Obtain graphene oxide
Concentration is the graphene oxide aqueous dispersions of 0.0024g/ml.
(2) 2.208g needlebush pulp material (after vacuum drying) is added in Pulp dredger, 1000ml water is added and discongests
15000 turns.It obtains starching dense about 0.22% needle wood pulp.
(3) 0.01g chitosan quaternary ammonium salt is added in the beaker equipped with 10ml ultrapure water, 12h is stirred on 100rpm.
Obtain the chitosan quaternary ammonium saline solution that concentration is about 0.001g/ml.
(4) it takes the chitosan quaternary ammonium saline solution in 3.84ml (3) to be added in the cellulose pulp of (2), uses glass bar
It is slowly stirred 2min.Then the graphene oxide aqueous dispersions in (1) are added, then glass bar is slowly stirred 4min.Final is mixed
The manual handsheet machine copy paper forming of combined paper slurry conversion paper, obtains extrusion coating paper after squeezing and drying.
(5) extrusion coating paper is cut into 1cm × 2cm size with scissors, impregnates in water, adds 0.008g ascorbic acid,
95 DEG C of reduction 10h under the conditions of being protected from light.
(6) the compound paper electrode of the graphene obtained after reduction is attached in gold-plated polyethylene terephthalate thin film,
It uses filter paper as diaphragm, instills 6M potassium hydroxide as electrolyte, two pieces of electrode materials are assembled into super capacitor.
Embodiment 3
(1) graphite oxide of 0.192g (improved Hummers method is prepared) is added to equipped with 80ml ultrapure water
In beaker, 20min is stirred evenly, then beaker is transferred in cell crushing instrument, it is then super with (30 DEG C, 400W) of cell crushing instrument
Sound 10min.Obtain the graphene oxide aqueous dispersions that graphene oxide concentration is 0.0024g/ml.
(2) 2.208g needlebush pulp material (after vacuum drying) is added in Pulp dredger, 1000ml water is added and discongests
15000 turns.It obtains starching dense about 0.22% needle wood pulp.
(3) 0.01g cationic polyacrylamide is added in the beaker equipped with 10ml ultrapure water, is stirred on 100rpm
12h.Obtain the cationic polyacrylamide aqueous solution that concentration is about 0.001g/ml.
(4) it takes the cationic polyacrylamide aqueous solution in 3.84ml (3) to be added in the cellulose pulp of (2), uses glass
Glass stick is slowly stirred 2min.Then the graphene oxide aqueous dispersions in (1) are added, then glass bar is slowly stirred 4min.Finally
The manual handsheet machine copy paper forming of mixed pulp conversion paper, it is about 120g/m that grammes per square metre is obtained after squeezing and drying2Aoxidize stone
The extrusion coating paper of black alkene content about 8%.
(5) extrusion coating paper is cut into 1cm × 1cm size with scissors, impregnates in water, adds 0.004g ascorbic acid,
95 DEG C of reduction 10h under the conditions of being protected from light.
(6) the compound paper electrode of the graphene obtained after reduction is attached in nickel foam, 1M potassium hydroxide/polyvinyl alcohol in drop
Gel is as electrolyte and diaphragm, and after drying moisture, two pieces of identical electrodes material fittings are assembled into super capacitor.
Embodiment 4
(1) graphite oxide of 0.192g (improved Hummers method is prepared) is added to equipped with 80ml ultrapure water
In beaker, 20min is stirred evenly, then beaker is transferred in cell crushing instrument, it is then super with (30 DEG C, 400W) of cell crushing instrument
Sound 10min.Obtain the graphene oxide aqueous dispersions that graphene oxide concentration is 0.0024g/ml.
(2) 2.208g needlebush pulp material (after vacuum drying) is added in Pulp dredger, 1000ml water is added and discongests
15000 turns.It obtains starching dense about 0.22% needle wood pulp.
(3) 0.01g cationic polyacrylamide is added in the beaker equipped with 10ml ultrapure water, is stirred on 100rpm
12h.Obtain the cationic polyacrylamide aqueous solution that concentration is about 0.001g/ml.
(4) it takes the cationic polyacrylamide aqueous solution in 3.84ml (3) to be added in the cellulose pulp of (2), uses glass
Glass stick is slowly stirred 2min.Then the graphene oxide aqueous dispersions in (1) are added, then glass bar is slowly stirred 4min.Finally
The manual handsheet machine copy paper forming of mixed pulp conversion paper, it is about 120g/m that grammes per square metre is obtained after squeezing and drying2Aoxidize stone
The extrusion coating paper of black alkene content about 8%.
(5) extrusion coating paper is cut into 1cm × 1cm size with scissors, impregnates in water, adds 0.004g ascorbic acid,
95 DEG C of reduction 10h under the conditions of being protected from light.
(6) the compound paper electrode of the graphene obtained after reduction is attached in the PET film for having plated gold, 1M hydroxide in drop
Potassium/polyvinyl alcohol gel is as electrolyte and diaphragm, and after drying moisture, two pieces of identical electrodes material fittings are assembled into super electricity
Hold.
Embodiment 5
(1) graphite oxide of 0.384g (improved Hummers method is prepared) is added to equipped with 160ml ultrapure water
In beaker, 0.5h is stirred evenly, then beaker is transferred in cell crushing instrument, it is then super with (30 DEG C, 400W) of cell crushing instrument
Sound 10min.Obtain the graphene oxide aqueous dispersions that graphene oxide concentration is 0.0024g/ml.
(2) 2.016g needle wood pulp (after vacuum drying) is added in Pulp dredger, 1000ml water is added and discongests
20000 turns.It obtains starching dense about 0.2% cellulose pulp.
(3) 0.01g cationic polyacrylamide is added in the beaker equipped with 10ml ultrapure water, is stirred on 100rpm
12h.Obtain the cationic polyacrylamide aqueous solution that concentration is about 0.001g/ml.
(4) it takes the cationic polyacrylamide aqueous solution in 1.54ml (3) to be added in the cellulose pulp of (2), uses glass
Glass stick is slowly stirred 2min.Then the graphene oxide aqueous dispersions in (1) are added, then glass bar is slowly stirred 4min.Finally
The manual handsheet machine copy paper forming of mixed pulp conversion paper, it is about 120g/m that grammes per square metre is obtained after squeezing and drying2Aoxidize stone
The extrusion coating paper of black alkene content about 16%.
(5) extrusion coating paper is cut into 1cm × 4cm size with scissors, impregnates in water, adds 0.032g ascorbic acid,
Under the conditions of being protected from light after 95 DEG C of reduction 10h, dry spare.
(6) using the compound paper electrode one end of the graphene obtained after reduction use conductive silver glue be stained with the aluminium foil of 1cm × 1cm as
Collector, 1M potassium hydroxide/polyvinyl alcohol gel is as electrolyte and diaphragm in drop, after drying moisture, by two pieces of identical electrodes
Material fitting is assembled into super capacitor.
Table 1 for supercapacitor prepared by embodiment 1-4 specific capacitance (under 5mV/s CV curve integral area calculate institute
)
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Electrolyte | KOH | KOH | KOH/PVA | KOH/PVA | KOH/PVA |
| Collector | Nickel foam | Gold-plated PET | Nickel foam | Gold-plated PET | Aluminium foil |
| Specific capacitance (F/g) | 134 | 159 | 98 | 112 | 86 |
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of supercapacitor, which comprises the steps of:
(1) graphite oxide is added to the water, ultrasonic disperse obtains graphene oxide water solution；By positively charged cation
Type retention agent is added to the water, and stirs evenly, and obtains retention agent aqueous solution；Cellulose paper is added to the water, dispersion is discongested, obtains
To cellulose pulp；
(2) retention agent aqueous solution is added in cellulose pulp, stirs, obtains the fiber mixed pulp for being enclosed with retention agent；
(3) graphene oxide water solution is mixed again with the fiber mixed pulp for being enclosed with retention agent, is slowly stirred, is aoxidized
Graphene fiber element mixed pulp；
(4) by obtained mixed pulp, copy paper, press dewatering obtain graphene oxide/fiber on manual handsheet machine after drying
Plain extrusion coating paper；
(5) obtained extrusion coating paper addition reducing agent is reduced into graphene/cellulose extrusion coating paper；
(6) above-mentioned extrusion coating paper is cut out, attached that electrolyte is added and diaphragm is packaged fixation on a current collector, assembling
At symmetrical supercapacitor.
2. the method according to claim 1, wherein the concentration of step (1) graphene oxide water solution is 0.001
~0.005g/ml；The concentration of retention agent aqueous solution is 0.0005~0.001g/ml.
3. the method according to claim 1, wherein step (1) retention agent be cationic polyacrylamide,
One or more of diallyl dimethyl ammoniumchloride, polyethyleneimine and chitosan quaternary ammonium salt.
4. the method according to claim 1, wherein step (1) the ultrasonic disperse ultrasonic cleaner or
Person's cell crushing instrument ultrasonic disperse, the Parameter Conditions of ultrasonic cleaner are as follows: 50~60 DEG C, 80~100W ultrasound, 2~4h；Cell
The Parameter Conditions of broken instrument are 30~60 DEG C, 400~600W ultrasound, 10~30min.
5. the method according to claim 1, wherein the stirring condition of step (1) described retention agent are as follows: revolving speed 50
~150rpm, 10~12h of time；The cellulose paper discongests condition are as follows: 10000~20000 turns.
6. the method according to claim 1, wherein the mass ratio of step (3) retention agent and graphite oxide is 0.4
The mass ratio of~4wt%, graphite oxide and cellulose is 0.3~16wt%.
7. method according to claim 1 or 2 or 3 or 4 or 5 or 6, which is characterized in that step (5) described reducing condition is
Reductase 12-10h at 95 DEG C；Reducing agent is ascorbic acid, one or more of hydrazine hydrate and tea polyphenols.
8. the method according to the description of claim 7 is characterized in that collector described in step (6) is nickel foam, steel disc, titanium
Piece or gold-plated polyethylene terephthalate thin film；The electrolyte is potassium hydroxide, sodium hydroxide, and the diaphragm is filter
Paper, polyvinyl alcohol gel.
9. method according to claim 1 or 2 or 3 or 4 or 5 or 6, which is characterized in that step (1) the graphite oxide warp
It crosses Hummers or improved Hummers method is prepared；The cellulose paper is cotton linter paper pulp, needle wood pulp, broad-leaved
Wood pulp or waste paper.
10. a kind of supercapacitor, which is characterized in that it is the method as described in claim 1~9 any one claim
It is prepared.
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| CN106469809A (en) * | 2016-04-01 | 2017-03-01 | 济南圣泉集团股份有限公司 | Graphene conductive paper and paper battery and its application |
| CN106469808B (en) * | 2016-04-01 | 2020-05-22 | 山东圣泉新能源科技有限公司 | Composite material for paper electrode, paper electrode made of composite material and paper battery |
| CN106890605B (en) * | 2017-02-21 | 2019-06-04 | 中国林业科学研究院木材工业研究所 | A kind of three-dimensional grapheme composite aerogel and preparation method thereof |
| CN107161984B (en) * | 2017-06-28 | 2019-07-16 | 华南理工大学 | A kind of method that ascorbic acid/tea polyphenols synergistic effect prepares graphene |
| CN108922795B (en) * | 2018-07-15 | 2019-09-03 | 重庆文理学院 | A kind of preparation method of the excellent graphene-based composite conductive thin film of electric conductivity |
| CN108962629B (en) * | 2018-07-15 | 2019-08-09 | 重庆文理学院 | A kind of preparation method of flexible super capacitor |
| CN109098030A (en) * | 2018-08-24 | 2018-12-28 | 宿迁南航新材料与装备制造研究院有限公司 | A kind of preparation method of graphene modified glass-fiber paper |
| CN110184855B (en) * | 2019-05-15 | 2020-11-10 | 西安交通大学 | Breathable and water-washable composite flexible conductive paper and preparation method and application thereof |
| CN113643906A (en) * | 2021-08-18 | 2021-11-12 | 吉林大学重庆研究院 | High-flexibility graphene-based supercapacitor based on laser processing and preparation method thereof |
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| CN102403050A (en) * | 2010-09-08 | 2012-04-04 | 中国科学院金属研究所 | Composite material based on nanometer, preparation method of composite material and application in flexible energy storage device |
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| CN102403050A (en) * | 2010-09-08 | 2012-04-04 | 中国科学院金属研究所 | Composite material based on nanometer, preparation method of composite material and application in flexible energy storage device |
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