CN103198929B - A kind of super capacitor electrode sheet and preparation method thereof - Google Patents
A kind of super capacitor electrode sheet and preparation method thereof Download PDFInfo
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- CN103198929B CN103198929B CN201310071496.7A CN201310071496A CN103198929B CN 103198929 B CN103198929 B CN 103198929B CN 201310071496 A CN201310071496 A CN 201310071496A CN 103198929 B CN103198929 B CN 103198929B
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- electrode
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- conducting resinl
- active material
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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 super capacitor manufacturing technology field, relate to a kind of super capacitor electrode sheet and preparation method thereof.Electrode slice is to embed conductive carbon particle one of collector or two surfaces, and this surface is bonded together composition by conducting resinl and electrode material；Electrode material is made up of electrode active material, conductive agent and binding agent；Conducting resinl is made up of conductive agent and rubber, and rubber is possible to prevent collector electrochemical corrosion in the electrolytic solution；Collector selects 20 μm～the aluminium foil of 30 μ m-thick, by the method for spark discharge, embeds conductive carbon particle with high purity graphite rod at collection liquid surface.Electrode active material is asphalt-base globular activated carbon, its specific surface area >=2000m2/g, and particle diameter is 10 μm～23 μm, and aperture is 1nm～3nm.Present invention reduces the internal resistance of EDLC, improve the electrochemically resistant corrosive power of EDLC collector, extend the service life of EDLC, stabilize running voltage.
Description
Technical field
The invention belongs to super capacitor manufacturing technology field, particularly to a kind of super capacitor electrode sheet and preparation side thereof
Method.
Background technology
Ultracapacitor, also referred to as double layer capacitor (Electric Double Layer Capacitor, EDLC),
It it is effective energy-storage travelling wave tube.In order to increase energy density and power density, a direction being widely known by the people is to reduce internal resistance, increases
Running voltage and working time.But, as described below, during reaching above-mentioned target, met with all difficulties.
One of them difficulty is to have one layer of dielectric oxide film on EDLC electrode metal collector.This dielectric oxide film increases
Contact resistance between carbon-coating and the metal collector of nano aperture.The contact resistance increased result in the increase of internal resistance, with
And correspondingly reduce the efficiency of output power density and capacitor.
Eliminate known to one the method for oxide-film effect be utilize known mechanical treatment (such as pressurize, supersound process
Deng) on aluminum collector, embed carbon granule, but, these trials do not obtain very good result.Can also be by aluminum afflux
Body is heated to fusing point (such as, profit is heated by resistive), is then compressed on the collector of fusing by carbon electrode.But, this needs
Substantial amounts of energy could allow aluminum 660 DEG C of fusings.Additionally, this method cannot be used for the relatively thin aluminum collector of ratio, and EDLC leads to
Often use is exactly aluminum foil current collector.
The nano-carbon powder resistivity forming nano aperture carbon-coating on electrode is also the important component part of EDLC internal resistance.Nanometer
The resistivity of carbon dust self is to reduce another difficulty of EDLC internal resistance.
Another difficulty is the electrochemical corrosion of EDLC metal parts, the electrochemical corrosion of especially EDLC anode.Make us
Worry, electrochemical corrosion can cause the reduction of running voltage.
Therefore, will reach the target than EDLC the most on the market with higher power density and efficiency, having the most very much must
Internal resistance to be reduced and raising running voltage.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of novel super capacitor electrode sheet and preparation side thereof
Method, electrode plates prepared by the method can reduce the internal resistance of super capacitor and stablize the running voltage of super capacitor.
The electrode slice of super capacitor of the present invention, including single-side electrode sheet and double-face electrode sheet two kinds.
Single-side electrode sheet is to embed conductive carbon particle on a surface of collector, and this surface is by conducting resinl and electrode material
Material is bonded together composition, and wherein, the area ratio of collection liquid surface embedding carbon is 50%～85%；Electrode material is by electrode activity
Material, conductive agent conductive carbon particles such as (graphite) acetylene blacks and binding agent (politef) composition, the mass fraction of three
It is respectively 85%～95%, 2%～10% and 3%～5%；Conducting resinl is by conductive agent (graphite, the conductive carbon particle such as acetylene black) and rubber
(Kynoar PVDF) forms, and rubber is possible to prevent collector electrochemical corrosion in the electrolytic solution, and the quality of PVDF is for leading
The 20%～60% of electricity colloid amount；
Double-face electrode sheet is all to embed conductive carbon particle on two surfaces of collector, and conducting resinl is passed through on two surfaces respectively
Being bonded together composition with electrode material, wherein, it is 50%～85% that collection liquid surface embeds the area ratio of carbon；Electrode material by
Electrode active material, conductive agent conductive carbon particles such as (graphite) acetylene blacks and binding agent (polytetrafluoroethylene PTFE) composition, three
The mass fraction of person is respectively 85%～95%, 2%～10% and 3%～5%；Conducting resinl is by Kynoar (PVDF) and conductive agent
The composition such as (graphite, acetylene black conductive carbon particle), the quality of PVDF is the 20%～60% of conducting resinl quality.
Collector selects 20 μm～the aluminium foil of 30 μ m-thick, by the method for spark discharge, with high purity graphite rod at afflux
Surface embeds conductive carbon particle.
Electrode active material is that the asphalt-base globular active carbon made with Colophonium etc. for raw material is (with asphalt for raw material system
Take granular active carbon, triumph petrochemical industry, 1979-8-29), then obtain through polybasic carboxylic acid pickling, filtration, heat treated.
Asphalt-base globular active carbon material specific surface area >=2000m after process2/ g, particle diameter is 10 μm～23 μm, aperture be 1nm～
3nm。
The preparation method of electrode slice of the present invention, comprises the steps:
1) with high purity graphite rod as raw material, conductive carbon particle is embedded by the method for spark discharge at collection liquid surface, embedding
The area ratio entering carbon is 50%～85%；
2) prepare asphalt-base globular active carbon, then through polybasic carboxylic acid pickling, filter, heat and obtain electrode active material；
3) in the mixed solvent of deionized water and ethanol, add ptfe emulsion, be stirring evenly and then adding into conduction
Agent, is stirring evenly and then adding into electrode active material, with mortar grinder, obtains electrode material；Then electrode material is pressed into 80
～100 electrode slices of μm；In electrode active material, the quality of electrode active material, conductive agent and PTFE binder is divided
Number is respectively 85%～95%, 2%～10% and 3%～5%；Politef and conductive agent in the mixed solvent of deionized water and ethanol
Concentration be 3～5wt%, the volume ratio of deionized water and ethanol is 1:1～2；
4) Kynoar is put in ketopyrrolidine and stir, put into conductive agent after being completely dissolved, continue to stir,
To conducting resinl；Wherein the mass ratio of Kynoar, conductive agent and ketopyrrolidine is 1:0.67～4:7～15；
5) conducting resinl of one or two surface-coated 4～5 μ m-thick of the collector processed in step 1)；Then by electricity
Pole piece is bonded together by conducting resinl with collector, dries 20～60 minutes for 120～150 DEG C, 180～210 DEG C of vacuum drying 5
～8h, thus obtain one side and two-sided electrode slice.
Then preparing stacked ultracapacitor, barrier film is alternately placed with electrode slice, and PP/PE/PP tri-and half chosen by barrier film
Permeable membrane, uses ultrasonic bonding machine to weld with respective lug the pole piece at the two poles of the earth respectively, and shell selects three layers of aluminum plastic film composite membrane,
Inject organic electrolyte after encapsulation, finally seal.
The solute of organic electrolyte be tetraethyl ammonium phosphate, tetra-allkylammonium, tetraethyl ammonium tetrafluoroborate, hexafluorophosphate or
Their mixture of person；Solvent is nitrile (acetonitrile, propionitrile, 3 methoxypropionitriles), lactone (gamma-butyrolacton, gamma-valerolactone
Deng), carbonate (propylene carbonate, ethylene carbonate, Ethyl methyl carbonate etc.), DMF, 1-methyl-2-pyrrolidine
Ketone, butanone, glycol dimethyl ether, or the mixed solvent of above-mentioned solvent composition, the concentration of organic electrolyte is 1mol/L.
Compared with prior art, the invention has the beneficial effects as follows the internal resistance reducing EDLC, improve EDLC collector
Electrochemically resistant corrosive power, extends the service life of EDLC, stabilizes running voltage.
Accompanying drawing explanation
The collector schematic diagram that Fig. 1: one side processes；
1 is the conductive carbon particle embedding aluminium foil surface, and 2 is aluminium foil；
Fig. 2: for the collector schematic diagram of double treatment；
Fig. 3: for single-side electrode chip architecture schematic diagram, 3 is electrode material, and 4 is conducting resinl；
Fig. 4: for double-face electrode chip architecture schematic diagram；
Fig. 5: for stacked capacitor arrangement sectional view, 5 is single-side electrode sheet, and 6 is double-face electrode sheet, and 7 is barrier film, and 8 are
Lug, 9 is shell, and 10 is electrolyte；
Fig. 6: collector prepared by the different embodiments internal resistance change curve under different voltages, curve 1,2,3 is respectively
Embodiment 1, embodiment 2, embodiment 3.
Fig. 7: collector prepared by the different embodiments time constant change curve under different voltages, curve 1,2,3 points
Not Wei embodiment 1, embodiment 2, embodiment 3.
Fig. 8, the volume change curve under different voltage ranges after adding conductive adhesive layer, curve 2,3 is respectively circulation 200 times
After, embodiment 2 and the embodiment 3 volume change curve under different voltage ranges.
Detailed description of the invention
Embodiment 1
Asphalt-base globular active carbon may comprise the compound of the impurity of 0.5%wt, such as iron oxides and other ferrum.
Impurity forms oxygen-containing functional group at activated carbon surface, such as carbonyl, hydroxide, ether etc..Iron compound and oxygen-containing functional group are miscellaneous
Matter adds the self discharge of EDLC and shortens service life.
Impurity can remove by the following method: asphalt-base globular active carbon filters after carboxylic acid pickling, collects filtering residue, will
Filtering residue is heated to 1200 DEG C from 600 DEG C under inert gas shielding.Heating process can remove surface oxygen functional group and increase
Plus nano carbon dust graphitization, strengthens electric conductivity.Specific surface area >=2000m is obtained after process2/ g, aperture is in the activity of 1nm～3nm
Charcoal.The particle diameter activated carbon in 18～23 μm is screened as electrode active material with the sieve of 600 mesh and 800 mesh.
Weigh deionized water and ethanol that volume ratio is 1:1, mix homogeneously, add PTFE(politef) emulsion, stir
Adding acetylene black after mixing uniformly, continue stirring, in mixed solvent, solid concentration is 4wt%.After after mix homogeneously, addition processes
Electrode active material, with mortar grinder, along with moisture and ethanol are slowly evaporated, forms argillaceous；Then with roll squeezer by clay
Shape electrode material is pressed into the electrode slice of 80 μm.Electrode active material, acetylene black, PTFE three's mass fraction are 95%, 2% and
3%；
Select the aluminium foil of 23 μ m-thick as collector, by the method for spark discharge with high purity graphite rod as raw material,
Collection liquid surface embeds conductive carbon particle.Electrode A (electrode specification φ 2.5 × 40mm) with graphite rod as working machine, with aluminium foil
As another electrode material B, use small-power low-voltage electric spark working machine, working power 120V, operating current 1A, frequency
50Hz, operating power is at 80W.It is 50% that collector embeds carbon area ratio, thus obtains the collector after surface processes.
PVDF is put in ketopyrrolidine and stir, put into acetylene black after being completely dissolved, continue to stir, conducted electricity
Glue.PVDF, acetylene black are 1:2:7 with the mass ratio of ketopyrrolidine.
Collector and the electrode material sheet suppressed after being processed on surface with conducting resinl are bonded together, conductive adhesive layer
Thickness 4 μm.Dry 20 minutes for 150 DEG C, after cutting out, 180 DEG C of vacuum drying 8h, obtain electrode slice to be assembled.By barrier film and electricity
Pole piece is alternately placed, and uses ultrasonic bonding machine to weld with respective lug respectively the pole piece at the two poles of the earth.
By tetraethyl ammonium tetrafluoroborate (Et4NBF4) put in acetonitrile, it is sufficiently stirred for, obtains the electrolysis that concentration is 1mol/L
Liquid.Injecting electrolyte after encapsulation, sealing i.e. obtains ultracapacitor monomer.
Embodiment 2
Asphalt-base globular active carbon is filtered after carboxylic acid pickling, collect filtering residue, by filtering residue under inert gas shielding from
600 DEG C are heated to 1200 DEG C.Specific surface area >=2000m is obtained after process2/ g, aperture is at the activated carbon of 1nm～3nm.With 1000
The sieve of mesh and 1340 mesh screens the particle diameter activated carbon in 10～13 μm as electrode active material.
Weigh deionized water and ethanol that volume ratio is 1:2, mix homogeneously, add PTFE solution, be stirring evenly and then adding into
Acetylene black, continues stirring.In mixed solvent, solid concentration is 4wt%.Activated carbon after addition processes after mix homogeneously, with grinding
Alms bowl grinds.Electrode material after grinding with roll squeezer is pressed into the thin slice of 100 μm.Electrode active material, acetylene black, PTFE tri-
The mass fraction of person is 85%, 10% and 5%.
Select the aluminium foil of 23 μ m-thick as collector, by the method for spark discharge, with high purity graphite rod as raw material,
Collection liquid surface embeds conductive carbon particle.Electrode A (electrode specification with graphite rod as working machine), with aluminium foil
As another electrode material B, use small-power low-voltage electric spark working machine, working power 120V, operating current 1A, frequency
50Hz, operating power is at 80W.Collector embeds carbon area ratio 80%.Obtain the collector after surface processes.
PVDF is put in ketopyrrolidine and stir, put into graphite after being completely dissolved, continue to stir, obtain conducting resinl.
PVDF, acetylene black are 1:2:15 with the mass ratio of ketopyrrolidine.
With conducting resinl, collector and the electrode material sheet suppressed are bonded together, thickness 5 μm of conductive adhesive layer.120
DEG C dry 60 minutes, after cutting out, 180 DEG C vacuum drying 8h, obtain electrode slice to be assembled.Barrier film is alternately placed with pole piece,
Ultrasonic bonding machine is used to weld with respective lug respectively the pole piece at the two poles of the earth.
By tetraethyl tetrafluoro ammonium phosphate (Et4NPF6) put in Allyl carbonate, it is sufficiently stirred for, obtaining concentration is 1mol/L
Electrolyte.Injecting electrolyte after encapsulation, sealing i.e. obtains ultracapacitor monomer.
Embodiment 3
The present embodiment uses the collector processed without surface, and electrode material is applied directly on collector, does not has
Having use conducting resinl, other processes are completely the same with embodiment 2.
Asphalt-base globular active carbon is filtered after carboxylic acid pickling, collect filtering residue, by filtering residue under inert gas shielding from
600 DEG C are heated to 1200 DEG C.Specific surface area >=2000m is obtained after process2/ g, mean diameter 10 μm, aperture is 1nm's～3nm
Electrode active material.
Weigh deionized water and ethanol that volume ratio is 1:2, mix homogeneously, add PTFE solution, be stirring evenly and then adding into
Acetylene black, continues stirring.In mixed solvent, solid concentration is 4wt%.Activated carbon after addition processes after mix homogeneously, electrode
Active substance, acetylene black, the mass fraction of PTFE three are 85%, 10% and 5%.
Select the aluminium foil of 23 μ m-thick as collector, electrode material is applied directly on collector.Dry 60 points for 120 DEG C
Clock, after cutting out, 180 DEG C of vacuum drying 8h, obtain electrode slice to be assembled.Barrier film is alternately placed with pole piece, by the pole at the two poles of the earth
Sheet uses ultrasonic bonding machine to weld with respective lug respectively.
By tetraethyl tetrafluoro ammonium phosphate (Et4NPF6) put in Allyl carbonate, it is sufficiently stirred for, obtaining concentration is 1mol/L
Electrolyte.Injecting electrolyte after encapsulation, sealing i.e. obtains ultracapacitor monomer.
0～0.7V, 0～1.0V, 0～1.5V, the capacitor monomer in above three embodiment is carried out constant current respectively fill
Discharge test (test electric current is 0.2A), analytical data obtains the internal resistance under different test conditions of each capacitor.Can by Fig. 6
To find out, in the case of capacity is very nearly the same, the treated embodiment of collector 1 is much smaller than collection with the internal resistance of embodiment 2
The embodiment 3 that fluid does not process, and the reduction that the contrast of Fig. 7 time constant more illustrates internal resistance is unrelated with amount of capacity.
Embodiment 2 and the monomer in embodiment 3 are circulated volt-ampere test, are measuring at different electricity after circulating 200 times
The capacitance of (0～1V, 0～1.25V, 0～1.5V, 0～2.0V, 0～2.5V) under pressure scope.It can be seen that at ceiling voltage
During more than 1.5V, embodiment 3 capacity of conducting resinl is not had to reduce clearly.And add embodiment 2 volume change of conducting resinl
More much smaller than embodiment 3.It is obvious that the addition of conducting resinl serves the effect of stable operating voltage.
Claims (4)
1. the electrode slice of a super capacitor, it is characterised in that: the collector-conducting resinl-electricity of conductive carbon particle is embedded for one side
The single-side electrode sheet of pole material sheet three-decker, it is a surface at collector that one side embeds the collector of conductive carbon particle
Embedding conductive carbon particle, mosaic surface is bonded together with electrode material thin slice by conducting resinl；The thickness of electrode material thin slice is
80～100 μm, are formed by electrode material compacting；Wherein, collection liquid surface embed conductive carbon particle area ratio be 50%～
85%；Electrode material is made up of electrode active material, conductive agent graphite or acetylene black and binding agent politef, three's
Mass fraction is 85%～95%, 2%～10% and 3%～5%；Conducting resinl is made up of conductive agent and Kynoar, poly-inclined
The quality of fluorothene is the 20%～60% of conducting resinl quality；Electrode active material is asphalt-base globular active carbon, its specific surface
Long-pending >=2000m2/ g, particle diameter is 10 μm～23 μm, and aperture is 1nm～3nm.
2. the electrode slice of a super capacitor, it is characterised in that: for electrode material thin slice-conducting resinl-embedding conductive carbon particle
The double-face electrode sheet of collector-conducting resinl-electrode material thin slice five-layer structure, the collector of two-sided embedding conductive carbon particle be
Two surfaces of collector all embed conductive carbon particle, and mosaic surface is bonded together with electrode material thin slice by conducting resinl；Electricity
The thickness of pole material sheet is 80～100 μm, electrode material compacting form；Wherein, collection liquid surface embeds conductive carbon particle
Area ratio be 50%～85%；Electrode material is by electrode active material, conductive agent graphite or acetylene black and polytetrafluoroethyl-ne
Alkene binding agent forms, and the mass fraction of three is 85%～95%, 2%～10% and 3%～5%；Conducting resinl by conductive agent and
Kynoar forms, and the quality of Kynoar is the 20%～60% of conducting resinl quality；Electrode active material is asphaltic base
Spheric active carbon, its specific surface area >=2000m2/ g, particle diameter is 10 μm～23 μm, and aperture is 1nm～3nm.
The electrode slice of a kind of super capacitor the most as claimed in claim 1 or 2, it is characterised in that: collector selects 20 μm～30 μ
The aluminium foil that m is thick.
4. the preparation method of the electrode slice of the super capacitor described in claim 1 or 2, its step is as follows:
1) with high purity graphite rod as raw material, embed by the method for spark discharge lead on a surface of collector or two surfaces
Carbon particles, the area ratio embedding conductive carbon particle is 50%～85%；
2) prepare asphalt-base globular active carbon, then through polybasic carboxylic acid pickling, filter, heat and obtain electrode active material；
3) in the mixed solvent of deionized water and ethanol, add ptfe emulsion, be stirring evenly and then adding into conductive agent, stir
Add electrode active material after mixing uniformly, with mortar grinder, obtain electrode material, then electrode material is pressed into 80～100 μ
The thin slice of m；In electrode active material, the mass fraction of electrode active material, conductive agent and PTFE binder is 85%
～95%, 2%～10% and 3%～5%；Politef and the concentration of conductive agent in the mixed solvent of deionized water and ethanol
Being 3～5wt%, the volume ratio of deionized water and ethanol is 1:1～2；
4) Kynoar is put in ketopyrrolidine and stir, put into conductive agent after being completely dissolved, continue to stir, led
Electricity glue；Wherein the mass ratio of Kynoar, conductive agent and ketopyrrolidine is 1:0.67～4:7～15；
5) in step 1) conducting resinl of one or two surface-coated 4～5 μ m-thick of collector that processed；Then by electrode slice
Be bonded together by conducting resinl with collector, 120～150 DEG C dry 20～60 minutes, 180～210 DEG C vacuum drying 5～
8h, thus obtain the electrode slice of single or double.
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| CN103811197A (en) * | 2014-02-26 | 2014-05-21 | 上海宝聚新化能源科技有限公司 | Manufacturing method of super capacitor |
| CN105070519A (en) * | 2015-09-08 | 2015-11-18 | 上海空间电源研究所 | High-specific-energy super capacitor negative pole sheet and preparation method thereof |
| CN105070530A (en) * | 2015-09-08 | 2015-11-18 | 上海空间电源研究所 | Electrolyte of super capacitor |
| CN105070516A (en) * | 2015-09-08 | 2015-11-18 | 上海空间电源研究所 | High-specific-energy super capacitor positive pole sheet and preparation method thereof |
| CN105304350A (en) * | 2015-11-17 | 2016-02-03 | 南通绿业中试技术研究院有限公司 | Abuse capacitor with wide temperature range and manufacturing method of abuse capacitor |
| CN106830223B (en) * | 2017-01-18 | 2020-05-05 | 北京理工大学 | Activated carbon electrode and preparation method and application thereof |
| CN110828198B (en) * | 2019-11-05 | 2022-03-08 | 中国科学院合肥物质科学研究院 | Laminated interdigital electrochemical capacitor and preparation method thereof |
| CN111916731A (en) * | 2020-07-27 | 2020-11-10 | 珠海冠宇电池股份有限公司 | Positive plate, preparation method thereof and lithium ion secondary battery comprising positive plate |
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| WO2007116244A2 (en) * | 2005-06-25 | 2007-10-18 | Elena Shembel | Method of fabricating electrodes with low contact resistance for batteries and double-layer capacitors |
| CN101404210A (en) * | 2008-11-19 | 2009-04-08 | 中国船舶重工集团公司第七一二研究所 | High-power super capacitor |
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| US6831826B2 (en) * | 2002-11-29 | 2004-12-14 | Honda Motor Co., Ltd. | Polarized electrode for electric double-layer condenser, and electric double-layer condenser manufactured using the same, and process for manufacturing electrode sheet for electric double-layer condenser, and laminating apparatus |
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| WO2007116244A2 (en) * | 2005-06-25 | 2007-10-18 | Elena Shembel | Method of fabricating electrodes with low contact resistance for batteries and double-layer capacitors |
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