CN109003823A - The manufacturing method of lithium-ion capacitor with the high power charging-discharging ability long-life - Google Patents
The manufacturing method of lithium-ion capacitor with the high power charging-discharging ability long-life Download PDFInfo
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- CN109003823A CN109003823A CN201810895549.XA CN201810895549A CN109003823A CN 109003823 A CN109003823 A CN 109003823A CN 201810895549 A CN201810895549 A CN 201810895549A CN 109003823 A CN109003823 A CN 109003823A
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 77
- 239000003990 capacitor Substances 0.000 title claims abstract description 74
- 238000007599 discharging Methods 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910021383 artificial graphite Inorganic materials 0.000 claims abstract description 18
- 239000010406 cathode material Substances 0.000 claims abstract description 9
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims description 38
- 239000011248 coating agent Substances 0.000 claims description 37
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 30
- 229910052744 lithium Inorganic materials 0.000 claims description 30
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 23
- 238000012360 testing method Methods 0.000 claims description 23
- 239000011889 copper foil Substances 0.000 claims description 22
- 239000011888 foil Substances 0.000 claims description 20
- 239000003610 charcoal Substances 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 17
- 229910052782 aluminium Inorganic materials 0.000 claims description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 14
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 13
- 239000005030 aluminium foil Substances 0.000 claims description 12
- 239000006258 conductive agent Substances 0.000 claims description 11
- 239000003792 electrolyte Substances 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 claims description 10
- BTGRAWJCKBQKAO-UHFFFAOYSA-N adiponitrile Chemical compound N#CCCCCC#N BTGRAWJCKBQKAO-UHFFFAOYSA-N 0.000 claims description 10
- 239000011230 binding agent Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 239000002985 plastic film Substances 0.000 claims description 8
- 229920006255 plastic film Polymers 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 7
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- WDXYVJKNSMILOQ-UHFFFAOYSA-N 1,3,2-dioxathiolane 2-oxide Chemical compound O=S1OCCO1 WDXYVJKNSMILOQ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 229910001290 LiPF6 Inorganic materials 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 4
- 239000010903 husk Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 239000002006 petroleum coke Substances 0.000 claims description 4
- 238000004080 punching Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229910013872 LiPF Inorganic materials 0.000 claims description 3
- 101150058243 Lipf gene Proteins 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 2
- 244000060011 Cocos nucifera Species 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 244000018633 Prunus armeniaca Species 0.000 claims description 2
- 235000009827 Prunus armeniaca Nutrition 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 238000005524 ceramic coating Methods 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 239000011280 coal tar Substances 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 claims description 2
- 239000008151 electrolyte solution Substances 0.000 claims description 2
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 238000010030 laminating Methods 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 239000011302 mesophase pitch Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 229910021382 natural graphite Inorganic materials 0.000 claims description 2
- 239000011331 needle coke Substances 0.000 claims description 2
- 239000004745 nonwoven fabric Substances 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 239000011295 pitch Substances 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 238000007788 roughening Methods 0.000 claims description 2
- 238000003466 welding Methods 0.000 claims description 2
- 230000009977 dual effect Effects 0.000 claims 1
- 238000009818 secondary granulation Methods 0.000 claims 1
- 239000010439 graphite Substances 0.000 abstract description 20
- 238000005516 engineering process Methods 0.000 abstract description 3
- 240000003936 Plumbago auriculata Species 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 14
- 239000010703 silicon Substances 0.000 description 14
- 229910052710 silicon Inorganic materials 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 6
- 239000007773 negative electrode material Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 239000011149 active material Substances 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000004087 circulation Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 238000002847 impedance measurement Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 229910021483 silicon-carbon alloy Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000006256 anode slurry Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000006257 cathode slurry Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021450 lithium metal oxide Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The present invention relates to the manufacturing method of the lithium-ion capacitor with the high power charging-discharging ability long-life, positive electrode specific capacity is not less than 0.25mAh/cm2, positive the area specific impedance be no more than 12 Ω cm2, cathode specific capacity is not less than 1.2mAh/cm2, cathode areas specific impedance be no more than 5 Ω cm2, the N/P ratio of cathode specific capacity and positive electrode specific capacity is not less than 2, and the ratio of positive the area specific impedance and cathode areas specific impedance is not less than 2.5.Cathode of the present invention uses artificial graphite or silicon carbon cathode material, has high energy density and power density；Meanwhile after recycling 10000 times at a temperature of 55 DEG C, internal resistance value added is no more than 10%, and capacity attenuation rate is no more than 5%.By using lithium-ion capacitor prepared by the technology of the present invention, widely used artificial plumbago negative pole in lithium ion battery is used, there are the performance characteristics of low cost and long-life, is conducive to the occupation rate of market for expanding lithium-ion capacitor product.
Description
[technical field]
The present invention relates to a kind of lithium-ion capacitor, more particularly, to a kind of cathode using graphite/silicon charcoal cathode lithium from
Sub-capacitor belongs to electrochemical energy storage component field.
[background technique]
Lithium-ion capacitor is a kind of combination double layer capacitor and lithium that developed on the basis of double layer capacitor
The new type of energy storage device of both ion batteries advantage has both high power long-life and the height of lithium ion battery of double layer capacitor
Energy response has received widespread attention and applies in fields such as new-energy automobile, rail traffic, modern logistics.
Lithium-ion capacitor usually anode is provided electric double layer energy storage by active carbon, and cathode is by embeddable/abjection lithium ion
Graphite, amorphous charcoal (soft/hard charcoal), silicon-carbon alloy (Si-C), containing the materials such as lithium metal oxide (lithium titanate) provide lithium ion
Energy storage, and combine the technologies synthesizer part such as porous electrode foil, pre- embedding lithium.Japanese fuji heavy industry is most early in CN200580001396
The manufacture patent of lithium-ion capacitor is disclosed, proposes a kind of operating voltage in the lithium-ion capacitor of 3.8~2.2V range
Manufacturing method.Hereafter, the manufacturing process of domestic and international lithium-ion capacitor has also followed the process program of patent proposition substantially.
In existing lithium-ion capacitor manufacture craft, the cathode overwhelming majority use with the long-life, low expansion it is non-
Graphitized charcoal is as electrode material；Therefore the active carbon anode of collocation long-life, the lithium-ion capacitor of preparation also have longevity
The characteristic of life.However, being limited to the high price of non-graphitic carbon, the overall cost of lithium-ion capacitor is still higher at present.Stone
Ink is cheap, popularization is wide as widely applied negative electrode material in lithium ion battery, is expected in the negative of lithium-ion capacitor
It is applied in the material of pole.
Patent CN200710163254 proposes a kind of product of graphite as lithium-ion capacitor negative electrode material, furthermore specially
Sharp CN201710627442 proposes a kind of product of silicon charcoal cathode as lithium-ion capacitor negative electrode material.However, commercially available
Use graphite for the lithium-ion capacitance product of cathode in use, the shortcomings that due to itself high expansion of graphite/silicon Carbon Materials,
Lithium-ion capacitor in high power charging-discharging after a period of use, product inevitably occur thickness it is exceeded and
Internal resistance increases the problems such as too fast；And graphite material (0~0.2V vs.Li lower to lithium current potential+/ Li), in high magnification charging process
Middle because polarization increases, graphite cathode is lower than 0V to lithium current potential, is also easy to produce the number of disadvantages such as Li dendrite, capacity attenuation be too fast, thus
Expectation of the market to graphite-based lithium-ion capacitor is much not achieved.The materials such as graphite/silicon charcoal not can solve in high magnification charge and discharge
Volume expansion is larger in electric process, internal resistance increases very fast disadvantage, using graphite/silicon charcoal as lithium-ion capacitor negative electrode material
Scale application certainly will significantly limit.
[summary of the invention]
It is an object of the invention to can solve the materials such as graphite/silicon charcoal during high power charging-discharging volume expansion compared with
Greatly, internal resistance increases very fast disadvantage, and design is a to have high magnification using graphite/silicon charcoal as lithium-ion capacitor negative electrode material
The lithium-ion capacitor of charging and discharging capabilities long-life.
For the above-mentioned problems in the prior art, the invention discloses one kind to have high power charging-discharging ability long-lived
The production method of the lithium-ion capacitor of life, cathode use artificial graphite or silicon carbon cathode material.It is made of the present invention
Graphite (/ silicon charcoal) base lithium ion capacitor has high energy density and power density；And in repeated multiple times high magnification charge and discharge
In electric process, the volume expansion variation of lithium-ion capacitor is small, internal resistance increasing degree is few, after 55 DEG C of 10000 circulations of high temperature
Internal resistance, which increases, is no more than 10%, and capacity attenuation is no more than 5%, cathode analysis lithium does not occur.
It is described as follows for the production method of lithium-ion capacitor of the invention:
A kind of lithium-ion capacitor with the high power charging-discharging ability long-life, include: active carbon with high specific surface area is just
Pole, artificial graphite (or silicon charcoal) material cathode, electrolyte, diaphragm, aluminum plastic film, tab terminal, the positive aluminium as collector
Foil and negative copper foil, and act on the conductive coating on positive pole aluminium foil/negative copper foil.
A kind of manufacturing method of the lithium-ion capacitor with the high power charging-discharging ability long-life, which is characterized in that packet
Include the anode of active carbon with high specific surface area, the cathode of artificial graphite or silicon carbon cathode material, electrolyte, diaphragm, aluminum plastic film, tab end
Son, positive pole aluminium foil and negative copper foil as collector, and act on the system of the conductive coating on positive pole aluminium foil/negative copper foil
Standby, preparation step is as follows:
Step 1, anode preparation:
The anode includes active carbon, conductive agent and the binder of high-specific surface area, and active carbon, conductive agent and binder are pressed
It is mixed and made into slurry according to 70~95:3 of mass ratio~20:3~15, surface is coated uniformly on and is coated on the aluminium foil of conductive coating；Institute
The specific surface area of active carbon is stated in 600~3500m2/g；It controls positive electrode specific capacity and is not less than 0.25mAh/cm2, more preferably positive ultimate ratio
Capacity is not less than 0.5mAh/cm2, further positive electrode specific capacity is not less than 0.7mAh/cm2More preferably, but it is no more than 1.5mAh/
cm2；It controls positive the area specific impedance and is no more than 12 Ω cm2, more preferably positive the area specific impedance is no more than 8 Ω cm2, into one
The positive the area specific impedance of step is no more than Ω cm2More preferably.
Active carbon is with the raw mineral materials such as department of botanys' raw material or coal, petroleum coke, pitch such as coconut husk, apricot shell, rice husk, by water
Steam or highly basic high temperature pore-creating handle to obtain；The aluminium foil can be LITHIUM BATTERY light foil, the processed capacitor yin of surface corrosion
Pole foil or perforated aluminum foil；Not perforated aluminium foil can obtain having logical after positive coating molding by the mode of mechanical punching
It is stand-by to be punched into cathode pole piece after drying, roll-in, cutting for the lithium-ion capacitor anode of well format, electrode.
Step 2, cathode preparation:
The cathode includes artificial graphite or silicon carbon cathode material, conductive agent and binder, artificial graphite or silicon charcoal cathode
Material, conductive agent, binder are mixed and made into slurry according to 70~98:0 of mass ratio~15:2~15, are coated uniformly on surface and are coated with
On the copper foil of conductive coating；The artificial graphite with mesophase pitch, coal tar, petroleum coke, needle coke etc. for raw material, through excessively high
Temperature charing obtains, and D50 partial size is no more than 10um；Or with D90 natural graphite, artificial graphite for being no more than 3um etc. by secondary
Prilling obtains the artificial graphite that D50 partial size is no more than 15um；It controls cathode specific capacity and is not less than 1.2mAh/cm2；It is more excellent
Cathode specific capacity be not less than 1.8mAh/cm2, further cathode specific capacity is not less than 2.5mAh/cm2More preferably, but it is no more than
8.4mAh/cm2；The ratio N/P ratio of control cathode specific capacity and positive electrode specific capacity is not less than 2, cathode specific capacity and positive specific volume
The ratio N/P ratio of amount is more preferably not less than 4, and further N/P ratio more preferably not less than 5.5, but is no more than 10；Control cathode areas
Specific impedance is no more than 5 Ω cm2, more preferably cathode ASI is no more than 3 Ω cm2, further ASI is no more than 1.5 Ω cm2More
It is good；The ratio for controlling positive the area specific impedance and cathode areas specific impedance is not less than 3.5, more preferably positive and negative anodes the area specific impedance
Ratio is not less than 4, and the ratio of further positive and negative anodes the area specific impedance is preferred not less than 5, but is no more than 10.
The lithium-ion capacitor has high isotropism with cathode artificial graphite；It is double that the copper foil can be LITHIUM BATTERY
Face light foil, machine glazing foil or two-sided hair foil, two-sided thick foil or perforation copper foil Jing Guo surface roughening treatment；Not perforated copper foil
The lithium-ion capacitor cathode with through-hole form can be obtained by the mode of mechanical punching after cathode coating molding, electricity
It is stand-by to be punched into cathode pole piece after drying, roll-in, cutting for pole.
Step 3, electrolyte preparation:
The electrolyte includes the LiPF of about 0.8~1.5M6And organic solvent, the organic solvent wrap by weight percentage
Include 10~40% ethylene carbonate (EC), 0~20% propene carbonate (PC), 0~50% dimethyl carbonate (DMC),
10~60% methyl ethyl carbonate (EMC), 0~10% adiponitrile (ADN), 0~5% vinylene carbonate (VC) and 0~
5% ethylene sulfite (ES)；The sum of the weight percent of ethylene carbonate (EC) and propene carbonate (PC) is total organic
The 20~50% of solvent, and propene carbonate accounts for the sum of described 40% or smaller；
Step 4, lithium-ion capacitor sample preparation: the positive and negative electrode cuts into pole piece by certain size, from fold
Battery core is built up with " Z-type " on piece machine, passes through battery core high temperature drying, the pre- lithium of metal lithium sheet, the ultrasonic welding of tab terminal, aluminum plastic film
Top side seal, injecting electrolytic solution, deairing and sealing, obtain final flexible packing lithium ion electric container products.
The diaphragm includes in cellulose paper diaphragm, PET non-woven fabrics+ceramic filler diaphragm, PE+ ceramic coating membrane etc.
The porosity of one kind, diaphragm is not less than 40%；
The positive pole aluminium foil/negative copper foil surface includes conductive coating, and the thickness single side of conductive coating is no more than 2um.
Effect of the conductive coating in active carbon double layer capacitor is conducive to keep active carbon in high temperature durability by wide coverage
Low internal resistance in the process increases.Equally, reduction graphite/silicon charcoal cathode is also beneficial to applied to the conductive coating of copper foil surface filling
Because of impedance value added caused by expansion in discharge process, be conducive to the good bonding for maintaining graphite/between silicon charcoal cathode and copper foil
Power.The preparation of the techniques such as intaglio printing, silk-screen printing, spraying can be used in conductive coating, and electrocondution slurry can be from commercially available quotient
The name of an article is one or more of EB-012, EB-815, T-602 etc. mixture.
In the drying shed of control humidity, a certain amount of lithium piece is taken, the metallic copper for being attached to thickness 30um is online, copper mesh and negative
Pole, which is left white, to be ultrasonically welded together；Positive and negative electrode is left white to be ultrasonically welded together with positive and negative electrode tab terminal respectively.Battery core and aluminium
Plastic film is made lithium-ion capacitor sample and is tested after the processes such as top side seal, fluid injection, sealing, aging, secondary sealing.
Electrolyte selects 1M LiPF6/ (PC+EC+EMC+DMC), additive are adiponitrile (ADN), vinylene carbonate (VC) and sulfurous
Vinyl acetate (ES).
One kind of the invention has a high power charging-discharging ability long-life lithium-ion capacitor, cathode using artificial graphite or
Silicon carbon cathode material has high energy density and power density；Meanwhile after recycling 10000 times at a temperature of 55 DEG C, internal resistance increases
Value is no more than 10%, and capacity attenuation rate is no more than 5%.By using lithium-ion capacitor prepared by the technology of the present invention, use
Widely used artificial plumbago negative pole in lithium ion battery has the performance characteristics of low cost and long-life, is conducive to expand lithium
The occupation rate of market of ionistor product.
[Detailed description of the invention]
Fig. 1 is embodiment/comparative example different multiplying charging cathode to lithium potential change curve
Fig. 2 is embodiment/comparative example circulation front and back multiplying power charging cathode to lithium potential change curve
Fig. 3 is 55 DEG C of cycle charge discharge electric capacitance change figures of embodiment/comparative example
Fig. 4 is 55 DEG C of cycle charge-discharge internal resistance changing values of embodiment/comparative example
[specific embodiment]
The following is specific embodiments of the present invention, is further described to technical solution of the present invention, but the present invention is simultaneously
It is not limited to these embodiments.
The positive electrode specific capacity is not less than 0.25mAh/cm2, more preferably positive electrode specific capacity is not less than 0.5mAh/cm2, into one
The positive electrode specific capacity of step is not less than 0.7mAh/cm2More preferably, but it is no more than 1.5mAh/cm2.The specific capacity of the anode is tested are as follows:
The disc-shaped anode having a size of Ф 14mm is chosen, is to electrode, 1M LiPF with lithium piece6/ EC+DMC (volume ratio 1:1) is electrolysis
Liquid, in EL-cell simulating test device over-assemble at simulated battery, activated carbon electrodes are within the scope of to 4.0~2.0V of lithium current potential
With 5mA/cm2Current density carries out constant current charge-discharge test, takes subject to the test capacity of third time.
The cathode specific capacity is not less than 1.2mAh/cm2, more preferably cathode specific capacity is not less than 1.8mAh/cm2, further
Cathode specific capacity be not less than 2.5mAh/cm2More preferably, but it is no more than 8.4mAh/cm2.The assembling of same anode simulated battery, graphite/
Or silicon charcoal cathode to lithium current potential within the scope of 0.005~1.5V with 5mA/cm2Current density carries out constant current charge-discharge test, takes the
Subject to measurement capacity three times.
The ratio (N/P ratio) of the cathode specific capacity and positive electrode specific capacity is not less than 2, and more preferably N/P ratio is not less than 4, into
The N/P ratio of one step more preferably not less than 5.5, but is no more than 10.Root it is documented that, about in graphite cathode process of intercalation
Nearby there are three platforms in 190mV, 95mV, 65mV, and corresponding embedding lithium capacity is 124mAh/g, 186mAh/g, 372mAh/ respectively
G, graphite Li insertion extraction between 190mV platform and 95mV platform have high structural stability and lesser volume expansion.Consider
To the cycle life of absorbent charcoal material and graphite material, N/P ratio is maintained at suitable ratio range and is conducive to lithium-ion capacitor
Keep optimal cycle life and energy density.
The anode carries out ac impedance measurement on electrochemical workstation, measures to the simulated battery of lithium piece composition
The area specific impedance (ASI) of anode is no more than 12 Ω cm when 50%SOC charged state2, more preferably anode ASI is no more than 8
Ω·cm2, further ASI is no more than 5 Ω cm2More preferably.Charged state (SOC) refers to the ratio of still not used active material,
The corresponding SOC of full charge of active material is 100%, and the corresponding SOC of the active material to discharge completely is 0%.Area resistivity
Anti- (ASI) refers to the impedance for the device being normalized relative to surface area, and is defined as using LCZ instrument or frequency response analyzer
The impedance measured at 1KHz multiplied by electrode surface area (cm2)。
The simulated battery that the cathode forms lithium piece carries out ac impedance measurement on electrochemical workstation, measures
The area specific impedance (ASI) of cathode is no more than 5 Ω cm when 50%SOC charged state2, more preferably cathode ASI is no more than 3 Ω
cm2, further ASI is no more than 1.5 Ω cm2More preferably.
The ratio of the anode the area specific impedance (ASI) and cathode areas specific impedance is not less than 2.5, and more preferably ratio is not low
In 4, further more preferably not less than 5, but it is no more than 10.Lithium-ion capacitor anode has higher the area specific impedance, in high power
Anode bears more polarization potentials in rate charging process；Under same charge cutoff voltage, anode/cathode areas specific impedance
Ratio is bigger, and the anode the easy during constant-current charge first reaches maximum potential, charges so as to avoid cathode in high magnification
Because hypopotenia has the risk of " analysis lithium " in journey；And anode/cathode areas specific impedance ratio is more than 10, it is likely that can shadow
The capacity rung to lithium-ion capacitor constant-current charge is filled with ratio.
Embodiment 1
Electrode preparation:
The perforated aluminum foil for taking thickness 20um, percent opening 18%, the double spread trade mark is EB-012 on dimple printing machine
Electrocondution slurry, conductive coating overall thickness 4um.
According to active carbon: conductive agent: binder=85:8:7 ratio configures slurry, two-sided painting in double planetary mixer
Cloth is in the perforated aluminum foil for being pre-coated with conductive coating, coating thickness 230um.Electrode is punched into 52* after drying, roll-in, cutting
The anode pole piece of 57mm is stand-by.Positive plate is the production simulation button cell on EL-cell simulator to electrode with lithium piece,
Electrolyte is 1M LiPF6/ EC+DMC (volume ratio 1:1)；With 5mA/cm within the scope of to 4.0~2.0V of lithium current potential2Electric current carries out
Positive electrode specific capacity about 0.70mAh/cm is tested in test2。
Equally, the perforation copper foil of thickness 12um, percent opening 13% is taken, the double spread trade mark is on dimple printing machine
The electrocondution slurry of EB-815, conductive coating overall thickness 4um.
According to graphite: conductive agent: binder=90:3:7 ratio configures slurry, double spread in double planetary mixer
On the perforation copper foil for being pre-coated with conductive coating, coating thickness 126um.Electrode is punched into 55* after drying, roll-in, cutting
The cathode pole piece of 60mm is stand-by.Cathode simulates button cell and is testing specific capacity about within the scope of 0~1.5V of lithium current potential
4.03mAh/cm2。
Lithium-ion capacitor sample preparation:
It takes the diaphragm of trade name TF4535 and has been punched the positive/negative plate of size, according to " Z " type on automatic laminating machine
Build up battery core；11, anode, 12, cathode, outermost layer are cathode, design lithium-ion capacitor capacity 200mAh.The battery core folded
12h is dried in vacuo under 120 DEG C of environment.
In the drying shed of control humidity, a certain amount of lithium piece is taken, the metallic copper for being attached to thickness 30um is online, copper mesh and negative
Pole, which is left white, to be ultrasonically welded together；Positive and negative electrode is left white to be ultrasonically welded together with positive and negative electrode tab terminal respectively.Battery core and aluminium
Plastic film is made lithium-ion capacitor sample and is tested after the processes such as top side seal, fluid injection, sealing, aging, secondary sealing.
Electrolyte selects 1M LiPF6/ (PC+EC+EMC+DMC), additive are adiponitrile (ADN), vinylene carbonate (VC) and sulfurous
Vinyl acetate (ES).
Manufactured lithium-ion capacitor constant current charge-discharge in 3.8~2.2V voltage range with 2A electric current, at the beginning of measuring sample
Beginning capacity is 198mAh.55 DEG C are carried out with 10A electric current within the scope of 3.8~2.2V to the lithium-ion capacitor sample for being made low
10000 cyclic charging and discharging tests.
Pole piece testing impedance:
The simulated battery of positive and negative electrode composition, tests the AC impedance of 1KHz on electrochemical workstation respectively.It measures just
Cathode areas specific resistance is respectively 2.62 Ω cm2With 0.35 Ω cm2。
Embodiment 2
With 1 method for making its electrode of embodiment, positive coating thickness 260um.Test positive electrode specific capacity about 0.77mAh/cm2。
With 1 method for making its electrode of embodiment, cathode specific capacity is still 4.03mAh/cm2。
Pole piece testing impedance shows that positive and negative anodes area specific resistance is respectively 2.95 Ω cm2With 0.35 Ω cm2。
Manufactured lithium-ion capacitor sample initial capacity is 217mAh.
Embodiment 3
With embodiment 1, positive coating thickness 200um.Test positive electrode specific capacity about 0.6mAh/cm2。
With embodiment 1, cathode specific capacity 4.03mAh/cm2。
Pole piece testing impedance shows that positive and negative anodes area specific resistance is respectively 2.28 Ω cm2With 0.35 Ω cm2。
Manufactured lithium-ion capacitor sample initial capacity is 168mAh.
Embodiment 4
With embodiment 1, positive conductive slurry is changed to trade mark T-602, and material formula is changed to active carbon by anode: conductive agent: viscous
Tie agent=80:12:8.Positive coating thickness 230um tests positive electrode specific capacity about 0.65mAh/cm2。
With embodiment 1, cathode specific capacity 4.03mAh/cm2。
Pole piece testing impedance shows that positive and negative anodes the area specific impedance is respectively 2.06 Ω cm2With 0.35 Ω cm2。
Manufactured lithium-ion capacitor sample initial capacity is 185mAh.
Embodiment 5
With embodiment 4, positive coating thickness 170um measures positive electrode specific capacity about 0.45mAh/cm2。
With 1 cathode production method of embodiment, cathode coating thickness 90um measures cathode specific capacity about 2.9mAh/cm2。
Pole piece testing impedance shows that positive and negative anodes the area specific impedance is respectively 1.83 Ω cm2With 0.28 Ω cm2。
Manufactured lithium-ion capacitor sample initial capacity is 134mAh.
Embodiment 6
With embodiment 4, positive coating thickness 200um measures positive electrode specific capacity about 0.55mAh/cm2。
With embodiment 5, cathode coating thickness 90um measures positive electrode specific capacity about 2.9mAh/cm2。
Pole piece testing impedance shows that positive and negative anodes the area specific impedance is 1.96 Ω cm respectively2With 0.35 Ω cm2。
Manufactured lithium-ion capacitor sample initial capacity is 156mAh.
Embodiment 7
With embodiment 4, positive coating thickness 230um measures positive electrode specific capacity about 0.65mAh/cm2。
With the conductive coating coating method of embodiment 1, on the aperture copper foil for being pre-coated with electrocondution slurry, according to 90:5:5's
Ratio is coated with silicon charcoal cathode.Cathode coating thickness is 100um, measures cathode specific capacity about 4.6mAh/cm2。
Pole piece testing impedance shows that positive and negative anodes area specific resistance is 2.06 Ω cm respectively2With 0.48 Ω cm2。
Manufactured lithium-ion capacitor sample initial capacity is 189mAh.
Comparative example 1
It with embodiment 1, is coated in perforated aluminum foil in advance without using electrocondution slurry, and is directly coated with anode sizing agent.Anode coating
Thickness 230um, the positive electrode specific capacity measured about 0.68mAh/cm2。
It with embodiment 1, is coated on perforated copper foil in advance without using electrocondution slurry, and is directly coated with negative electrode slurry.Cathode coating
Thickness 126um, the cathode specific capacity measured about 4.0mAh/cm2。
Pole piece testing impedance shows that positive and negative anodes area specific resistance is 4.25 Ω cm respectively2With 0.43 Ω cm2。
Manufactured lithium-ion capacitor sample initial capacity is 193mAh.
Comparative example 2
It with embodiment 5, is coated in advance without using electrocondution slurry in perforated aluminum foil and perforation copper foil, directly coating anode and cathode slurry
On a current collector.
Positive coating thickness 170um measures positive electrode specific capacity about 0.42mAh/cm2。
Cathode coating thickness 90um measures cathode specific capacity about 2.88mAh/cm2。
Pole piece testing impedance shows that positive and negative anodes area specific resistance is 2.87 Ω cm respectively2With 0.40 Ω cm2。
Manufactured lithium-ion capacitor sample initial capacity is 128mAh.
Carrying out capacity, internal resistance, cryogenic property, high temperature durability, cycle charge-discharge etc. to lithium-ion capacitor obtained is
Column test, test result are as shown in table 1.
As known from Table 1, lithium-ion capacitor of the invention has high power charging-discharging ability, and has extended cycle life.
Claims (10)
1. a kind of manufacturing method of the lithium-ion capacitor with the high power charging-discharging ability long-life, which is characterized in that including
The anode of active carbon with high specific surface area, the cathode of artificial graphite or silicon carbon cathode material, electrolyte, diaphragm, aluminum plastic film, tab end
Son, positive pole aluminium foil and negative copper foil as collector, and act on the system of the conductive coating on positive pole aluminium foil/negative copper foil
Standby, preparation step is as follows:
Step 1, anode preparation:
The anode includes active carbon, conductive agent and the binder of high-specific surface area, and active carbon, conductive agent and binder are according to matter
Amount is mixed and made into slurry than 70~95:3~20:3~15, is coated uniformly on surface and is coated on the aluminium foil of conductive coating；The work
The specific surface area of property charcoal is in 600~3500m2/ g, control positive electrode specific capacity are not less than 0.25mAh/cm2, positive the area specific impedance is not
More than 12 Ω cm2；
Step 2, cathode preparation:
The cathode includes artificial graphite or silicon carbon cathode material, conductive agent and binder, artificial graphite or silicon carbon cathode material,
Conductive agent, binder are mixed and made into slurry according to 70~98:0 of mass ratio~15:2~15, are coated uniformly on surface and are coated with conduction
On the copper foil of coating；The artificial graphite with mesophase pitch, coal tar, petroleum coke, needle coke etc. for raw material, by pyrocarbon
Change obtains, and D50 partial size is no more than 10um；Or natural graphite, artificial graphite with D90 no more than 3um etc. passes through secondary granulation
Technique obtains the artificial graphite that D50 partial size is no more than 15um；It controls cathode specific capacity and is not less than 1.2mAh/cm2, cathode areas
Specific impedance is no more than 5 Ω cm2；The ratio N/P ratio of cathode specific capacity and positive electrode specific capacity is not less than 2, positive the area specific impedance
It is not less than 2.5 with the ratio of cathode areas specific impedance；
Step 3, electrolyte preparation:
The electrolyte includes the LiPF of about 0.8~1.5M6And organic solvent, the organic solvent include 10 by weight percentage
~40% ethylene carbonate (EC), 0~20% propene carbonate (PC), 0~50% dimethyl carbonate (DMC), 10~
60% methyl ethyl carbonate (EMC), 0~10% adiponitrile (ADN), 0~5% vinylene carbonate (VC) and 0~5%
Ethylene sulfite (ES)；The sum of the weight percent of ethylene carbonate (EC) and propene carbonate (PC) is total organic solvent
20~50%, and propene carbonate accounts for the sum of described 40% or smaller；
Step 4, lithium-ion capacitor sample preparation: the positive and negative electrode cuts into pole piece by certain size, in automatic laminating machine
On battery core built up with " Z-type ", by battery core high temperature drying, the pre- lithium of metal lithium sheet, the ultrasonic welding of tab terminal, aluminum plastic film top
Side seal, injecting electrolytic solution, deairing and sealing and etc., obtain final flexible packing lithium ion electric container products.
2. a kind of preparation side of the lithium-ion capacitor with the high power charging-discharging ability long-life as described in claim 1
Method, which is characterized in that active carbon with the raw mineral materials such as department of botanys' raw material or coal, petroleum coke, pitch such as coconut husk, apricot shell, rice husk,
It handles to obtain by vapor or highly basic high temperature pore-creating；The aluminium foil can be LITHIUM BATTERY light foil, the processed electricity of surface corrosion
Container Cathode Foil or perforated aluminum foil；Not perforated aluminium foil can obtain after positive coating molding by the mode of mechanical punching
Lithium-ion capacitor anode with through-hole form.
3. a kind of preparation side of the lithium-ion capacitor with the high power charging-discharging ability long-life as described in claim 1
Method, which is characterized in that more preferably positive electrode specific capacity is not less than 0.5mAh/cm2, further positive electrode specific capacity is not less than
0.7mAh/cm2More preferably, but it is no more than 1.5mAh/cm2。
4. a kind of preparation side of the lithium-ion capacitor with the high power charging-discharging ability long-life as described in claim 1
Method, which is characterized in that the lithium-ion capacitor has high isotropism with cathode artificial graphite；The copper foil can be electricity
Pond grade dual light foil, machine glazing foil or two-sided hair foil, two-sided thick foil or perforation copper foil Jing Guo surface roughening treatment；It is non-to wear
Hole copper foil can obtain having the lithium-ion capacitor of through-hole form negative after cathode coating molding by the mode of mechanical punching
Pole.
5. a kind of preparation side of the lithium-ion capacitor with the high power charging-discharging ability long-life as described in claim 1
Method, which is characterized in that more preferably cathode specific capacity is not less than 1.8mAh/cm2, further cathode specific capacity is not less than
2.5mAh/cm2More preferably, but it is no more than 8.4mAh/cm2。
6. a kind of preparation side of the lithium-ion capacitor with the high power charging-discharging ability long-life as described in claim 1
Method, which is characterized in that the ratio N/P ratio of cathode specific capacity and positive electrode specific capacity is more preferably not less than 4, and further N/P ratio is not
More preferably lower than 5.5, but it is no more than 10.
7. a kind of preparation side of the lithium-ion capacitor with the high power charging-discharging ability long-life as described in claim 1
Method, which is characterized in that the ratio of positive the area specific impedance (ASI) and cathode areas specific impedance is not less than 2.5, and more preferably ratio is not
Lower than 4, further more preferably not less than 5, but it is no more than 10.
8. a kind of preparation side of the lithium-ion capacitor with the high power charging-discharging ability long-life as claimed in claim 8
Method, which is characterized in that more preferably positive the area specific impedance is no more than 8 Ω cm2, further ASI is no more than 5 Ω cm2More
It is good；More preferably cathode ASI is no more than 3 Ω cm2, further ASI is no more than 1.5 Ω cm2More preferably.
9. a kind of preparation side of the lithium-ion capacitor with the high power charging-discharging ability long-life as described in claim 1
Method, which is characterized in that the diaphragm includes cellulose paper diaphragm, PET non-woven fabrics+ceramic filler diaphragm, PE+ ceramic coating membrane
One of Deng, the porosity of diaphragm is not less than 40%.
10. a kind of preparation side of the lithium-ion capacitor with the high power charging-discharging ability long-life as described in claim 1
Method, which is characterized in that in the drying shed of control humidity, take a certain amount of lithium piece, the metallic copper for being attached to thickness 30um is online, copper
Net and cathode, which are left white, to be ultrasonically welded together；Positive and negative electrode is left white to be ultrasonically welded together with positive and negative electrode tab terminal respectively.Electricity
The progress of lithium-ion capacitor sample is made after the processes such as top side seal, fluid injection, sealing, aging, secondary sealing in core and aluminum plastic film
Test.Electrolyte selects 1M LiPF6/ (PC+EC+EMC+DMC), additive are adiponitrile (ADN), vinylene carbonate (VC)
With ethylene sulfite (ES).
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| CN111435632A (en) * | 2019-01-11 | 2020-07-21 | 中国石油大学(北京) | Lithium ion capacitor and preparation method thereof |
| CN113138221A (en) * | 2021-04-20 | 2021-07-20 | 合肥国轩高科动力能源有限公司 | Method for optimizing proportion representation SEI film impedance of conductive agent and binder |
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