CN108155027A - A kind of method of the pre- embedding lithium of lithium ion super capacitor cathode - Google Patents
A kind of method of the pre- embedding lithium of lithium ion super capacitor cathode Download PDFInfo
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- CN108155027A CN108155027A CN201611098898.6A CN201611098898A CN108155027A CN 108155027 A CN108155027 A CN 108155027A CN 201611098898 A CN201611098898 A CN 201611098898A CN 108155027 A CN108155027 A CN 108155027A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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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 present invention relates to a kind of method of the pre- embedding lithium of lithium ion super capacitor cathode, including anode, diaphragm, cathode and the electrolyte between positive electrode and negative electrode；The positive electrode includes active material and pre- embedding lithium additive；Wherein, the mass ratio of pre- embedding lithium additive and negative material is 1：100~10：1；Anode, diaphragm, cathode are assembled into lithium ion super capacitor, added in after electrolyte to the pre- embedding lithium of battery charging.The cyclical stability of the lithium-ion capacitor of less pre- embedding lithium is more preferable, safe and reliable, at low cost.
Description
Technical field
The present invention relates to electrochemical energy storage fields.
Background technology
Lithium ion super capacitor has safe as a kind of energy storage device, and service life is long, and power height etc. is excellent
Point, it combines the advantage of common double layer capacitor and lithium ion battery, so in mobile communication, startup power supply, spare
There is better application prospect in the fields such as power supply.
Lithium ion super capacitor has the characteristics that：(1) for lithium ion battery, it is close to possess higher power
Degree, in high current application scenario particularly high energy pulse environment, can better meet power requirement.(2) during charge and discharge cycles
Between very short, far smaller than charge-discharge cycle time of accumulator.(3) battery is long, need not safeguard all the life.(4) operation temperature
Spend wide can work normally in the range of -45~85 DEG C.
Most of lithium ion super capacitor uses carbonaceous material as cathode.In order to improve the cyclicity of capacitor, all
It needs to use pre- embedding lithium technology.
Early in a kind of lithium ion super capacitor that Fuji Heavy in 2006 announces, than energy up to 12-30Wh/kg,
For capacity retention ratio still more than 96%, excellent cyclicity has benefited from pre-embedding lithium processes after 300000 cycles.
Pre- embedding lithium technology is a vital ring in lithium ion super capacitor manufacturing technology, manufactures of high cost and technique
Complexity is generally acknowledged technological difficulties.Available data has been discovered that a variety of manufacturing technologies of lithium ion super capacitor, lithium source
The factors such as selection, tax lithium process implementations, lithium doping amount decide device performance, manufacture cost, reliability.
Fuji Heavy uses multicellular metal foil as collector, and a piece of lithium foil is placed in the opposite position of outermost layer cathode,
Accordingly even when being the monomer containing multi-layered electrode, Li+ can also pass freely through the coating being attached on collector and is laminated in electrode
It is moved in unit, so as to which Li+ is doped in cathode.This pre-embedding lithium method needs to use lithium metal as lithium source, to being made
Environmental requirement is harsh, and has great security risk.
Professor Zheng Jianping of Tongji University is the stable metal lithium powder of 10~200nm, surface with passivating film using grain size
(SLMP) it is lithium source, cathode is made with dry process after being mixed with hard charcoal, activated carbon is assembled into LIC monomers, test knot for anode
Fruit shows that monomer than energy is about 25Wh/kg, 60% when the electric discharges of 44C multiplying powers than energy is about 2.4C, after 600 cycles
The capacitance decrement of monomer is less than 3%.Compared to the structure that Fuji Heavy uses lithium metal foil, the LIC of the structure can be in drying shed
In manufactured, without the harsh environment of glove box, considerably increase operability.
Rich lithium compound of the use such as Wu Feng of Beijing Institute of Technology with certain irreversible de- lithium property, such as cobalt acid lithium,
LiMn2O4 etc. is greatly improved the packaging technology of lithium ion super capacitor, the manufacture cost of capacitor and safety
While having clear improvement, it also can increase a part of unnecessary quality to battery, reduce the energy density of battery, particularly
In the case where the pre- embedding lithium degree of needs is very big.
Invention content
In order to solve the above technical problems, the side the present invention provides the pre- embedding lithium of a kind of lithium ion super capacitor and cathode
Method while this method can prepare electrode and safety in normal lithium battery coating environment, will not increase
The quality in pond is powered up, cost can greatly be reduced.
In order to achieve the above objectives, the specific technical solution of use is as follows,
A kind of method of the pre- embedding lithium of lithium ion super capacitor cathode, including anode, diaphragm, cathode and positioned at anode
Electrolyte between cathode；
The positive electrode includes active material and pre- embedding lithium additive；
The negative material includes native graphite, hard charcoal, mesophase microbeads charcoal, amorphous carbon, silicon, silica, charcoal
It is more than one or two kinds of in silicon compound, lithium titanate；
Wherein, the mass ratio of pre- embedding lithium additive and negative material is 1：100~10：1；
Anode, diaphragm, cathode are assembled into lithium ion super capacitor, added in after electrolyte to the pre- embedding lithium of battery charging.
Battery charging pre-embedding lithium method includes the pre- embedding lithium of constant current or the pre- embedding lithium of constant pressure；
The pre- embedding lithium of battery constant current, electric current are 0.01mA-10A/ per the pre- embedding lithium additives of g, charge cutoff voltage 0.42V-
5V；
The pre- embedding lithium of battery constant pressure, voltage 0.42V-5V, cut-off current are 0.001m A-1m A.
The pre- embedding lithium additive for lithia, lithium peroxide, lithium nitride, charing lithium in it is one or two kinds of more than.
The pre- embedding lithium additive for preferred lithia, lithium peroxide, lithium nitride it is one or two kinds of more than；Pre- embedding lithium
The mass ratio of additive and negative material is 1:5~5:1.
The active material includes absorbent charcoal material, conducting polymer, more than one or two kinds of in oxide.
The absorbent charcoal material includes active carbon powder, activated carbon fibre, carbon aerogels, carbon nanotube, graphene, charcoal
It is more than one or two kinds of in black grade；The conducting polymer includes polyaniline, polythiophene, polypyrrole, polypyridine, polyphenyl
And its more than one or two kinds of in derivative；
The oxide includes manganese dioxide, ruthenium-oxide, more than one or two kinds of in titanium dioxide.
The diaphragm is polyethylene diagrams, polypropylene diaphragm, polyethylene, polypropylene composite materials diaphragm, cellulosic separator, glass
Glass cellulosic separator or ceramic membrane.
Advantageous effect of the present invention：
Provided by the present invention for the cathode pre-embedding lithium method of lithium-ion capacitor, the lithium-ion capacitance of less pre- embedding lithium
The good cycling stability of device, this method can prepare electrode and safety in normal lithium battery coating environment
While, the quality of battery will not be increased, cost can greatly be reduced.
Specific embodiment
With reference to embodiment, the content of invention is more specifically illustrated.The implementation of the present invention is not limited to what dried shrimp was held high
Embodiment.
Embodiment 1
Prepare lithium-ion capacitor cathode.By native graphite, conductive agent, PVDF according to mass ratio be 80:15:5 mixing are equal
After even, NMP (addition of NMP accounts for the 50% of entire slurry) is added in, stirs 12 hours, is coated on copper foil, it is natural after drying
The surface density of graphite is 5mgcm-2。
Prepare lithium-ion capacitor anode.By activated carbon, conductive agent, PVDF, lithium nitride according to mass ratio be 60:10:5:
25 after mixing, adds in NMP (addition of NMP accounts for the 55% of entire slurry) and stirs 12 hours, be coated on aluminium foil, dries
The surface density of activated carbon is 15mgcm afterwards-2。
Above-mentioned positive and negative anodes are sliced into 7.7cm*5cm sizes, thoroughly after drying, anode, cathode, diaphragm are assembled into lamination
The aluminum-plastic packaged interior of corresponding size, fluid injection are packed into after battery.
Under inert conditions, charge to battery pre- embedding lithium, and the electric current of pre- embedding lithium is 0.01Ag-1(based on lithium nitride matter in battery
Amount), charge cutoff voltage 1V.In charging process, ensure that battery is in open state, to be conducive to nitrogen discharge.
After charging, battery seal test, 1A.g-1After 10000 cycles of (being calculated based on cell active materials) test
Capacity retention ratio and capacitance pool energy density (being based on active material), and be reported in Table 1 below.
Comparative example 1
Prepare lithium-ion capacitor cathode.By native graphite, conductive agent, PVDF according to mass ratio be 80:15:5 mixing are equal
After even, NMP (addition of NMP accounts for the 50% of entire slurry) is added in, stirs 12 hours, is coated on copper foil, it is natural after drying
The surface density of graphite is 5mgcm-2。
Prepare lithium-ion capacitor anode.By activated carbon, conductive agent, PVDF according to mass ratio be 85:10:5 are uniformly mixed
Afterwards, it adds in NMP (addition of NMP accounts for the 50% of entire slurry) to stir 12 hours, be coated on aluminium foil, activated carbon after drying
Surface density is 15mgcm-2。
Above-mentioned positive and negative anodes are sliced into 7.7cm*5cm sizes, thoroughly after drying, anode, cathode, diaphragm are assembled into lamination
The aluminum-plastic packaged interior of corresponding size, fluid injection are packed into after battery.
Under inert conditions, charge to battery pre- embedding lithium, and the electric current of pre- embedding lithium is 0.01Ag-1(being based on active material), charging
Blanking voltage is 1V.In charging process, ensure that battery is in open state, to be conducive to nitrogen discharge.
After charging, battery seal test, 1A.g-1After 10000 cycles of (being calculated based on cell active materials) test
Capacity retention ratio and capacitive energy density (being based on active material), and be reported in Table 1 below.
By result as can be seen that stable circulation is much better than the capacitor of not embedding lithium, and the energy density of capacitance is basic
Do not influence.
Embodiment 2
Prepare lithium-ion capacitor cathode.By native graphite, conductive agent, PVDF according to mass ratio be 80:15:5 mixing are equal
After even, NMP (addition of NMP accounts for the 50% of entire slurry) is added in, stirs 12 hours, is coated on copper foil, it is natural after drying
The surface density of graphite is 3mgcm-2。
Prepare lithium-ion capacitor anode.By activated carbon, conductive agent, PVDF, lithia according to mass ratio be 50:10:5:
35 after mixing, adds in NMP (addition of NMP accounts for the 55% of entire slurry) and stirs 12 hours, be coated on aluminium foil, dries
The surface density of activated carbon is 15mgcm afterwards-2。
Under inert conditions, charge to battery pre- embedding lithium, and the electric current of pre- embedding lithium is 0.01Ag-1(based on lithia matter in battery
Amount), charge cutoff voltage 3.5V.In charging process, ensure that battery is in open state, to be conducive to nitrogen discharge.
After charging, battery seal test, 1A.g-1After 10000 cycles of (being calculated based on cell active materials) test
Capacity retention ratio and capacitive energy density (being based on active material), and be reported in Table 1 below.Embodiment 3
Prepare lithium-ion capacitor cathode.By hard charcoal, conductive agent, PVDF according to mass ratio be 80:15:5 after mixing,
NMP (addition of NMP accounts for the 50% of entire slurry) is added in, stirs 12 hours, is coated on copper foil, native graphite after drying
Surface density is 5mgcm-2。
Prepare lithium-ion capacitor anode.By activated carbon, conductive agent, PVDF, lithium nitride according to mass ratio be 60:10:5:
25 after mixing, adds in NMP (addition of NMP accounts for the 55% of entire slurry) and stirs 12 hours, be coated on aluminium foil, dries
The surface density of activated carbon is 12mgcm afterwards-2。
Above-mentioned positive and negative anodes are sliced into 7.7cm*5cm sizes, thoroughly after drying, anode, cathode, diaphragm are assembled into lamination
The aluminum-plastic packaged interior of corresponding size, fluid injection are packed into after battery.
Under inert conditions, charge to battery pre- embedding lithium, and the electric current of pre- embedding lithium is 0.001Ag-1(based on lithium nitride matter in battery
Amount), charge cutoff voltage 1V.In charging process, ensure that battery is in open state, to be conducive to nitrogen discharge.
After charging, battery seal test, 1A.g-1After 10000 cycles of (being calculated based on cell active materials) test
Capacity retention ratio and capacitive energy density (being based on active material), and be reported in Table 1 below.Embodiment 4
Prepare lithium-ion capacitor cathode.By hard charcoal, conductive agent, PVDF according to mass ratio be 80:15:5 after mixing,
NMP (addition of NMP accounts for the 50% of entire slurry) is added in, stirs 12 hours, is coated on copper foil, native graphite after drying
Surface density is 5mgcm-2。
Prepare lithium-ion capacitor anode.By activated carbon, conductive agent, PVDF, lithium nitride according to mass ratio be 55:10:5:
30 after mixing, adds in NMP (addition of NMP accounts for the 53% of entire slurry) and stirs 12 hours, be coated on aluminium foil, dries
The surface density of activated carbon is 18mgcm afterwards-2。
Above-mentioned positive and negative anodes are sliced into 7.7cm*5cm sizes, thoroughly after drying, anode, cathode, diaphragm are assembled into lamination
The aluminum-plastic packaged interior of corresponding size, fluid injection are packed into after battery.
Under inert conditions, charge to battery pre- embedding lithium, and the electric current of pre- embedding lithium is 0.02Ag-1(based on lithium nitride matter in battery
Amount), charge cutoff voltage 1V.In charging process, ensure that battery is in open state, to be conducive to nitrogen discharge.
After charging, battery seal test, 1A.g-1After 10000 cycles of (being calculated based on cell active materials) test
Capacity retention ratio and capacitive energy density (being based on active material), and be reported in Table 1 below.Embodiment 5
Prepare lithium-ion capacitor cathode.By hard charcoal, conductive agent, PVDF according to mass ratio be 80:15:5 after mixing,
NMP (addition of NMP accounts for the 50% of entire slurry) is added in, stirs 12 hours, is coated on copper foil, native graphite after drying
Surface density is 5mgcm-2。
Prepare lithium-ion capacitor anode.By activated carbon, conductive agent, PVDF, lithium peroxide according to mass ratio be 40:10:
5:45 after mixing, adds in NMP (addition of NMP accounts for the 53% of entire slurry) and stirs 12 hours, be coated on aluminium foil, dries
The surface density of activated carbon is 15mgcm after dry-2。
Above-mentioned positive and negative anodes are sliced into 7.7cm*5cm sizes, thoroughly after drying, anode, cathode, diaphragm are assembled into lamination
The aluminum-plastic packaged interior of corresponding size, fluid injection are packed into after battery.
Under inert conditions, charge to battery pre- embedding lithium, and the electric current of pre- embedding lithium is 0.02Ag-1(based on lithium peroxide in battery
Quality), charge cutoff voltage 4V.In charging process, ensure that battery is in open state, to be conducive to nitrogen discharge.
After charging, battery seal test, 1A.g-1After 10000 cycles of (being calculated based on cell active materials) test
Capacity retention ratio and capacitive energy density (being based on active material), and be reported in Table 1 below.
Table 1
| Capacity retention ratio after 10000 cycles | Energy density (is based on active material) | |
| Embodiment 1 | 93% | 125Wh/kg |
| Comparative example 1 | 60% | 126Wh/kg |
| Embodiment 2 | 92% | 127Wh/kg |
| Embodiment 3 | 90% | 124Wh/kg |
| Embodiment 4 | 87% | 128Wh/kg |
| Embodiment 5 | 88% | 130Wh/kg |
Claims (7)
1. a kind of method of the pre- embedding lithium of lithium ion super capacitor cathode, including anode, diaphragm, cathode and positioned at anode with
Electrolyte between cathode；It is characterized in that：
The positive electrode includes active material and pre- embedding lithium additive；
The negative material includes native graphite, hard charcoal, mesophase microbeads charcoal, amorphous carbon, silicon, silica, charcoal silicon and answers
Close object, more than one or two kinds of in lithium titanate；
Wherein, the mass ratio of pre- embedding lithium additive and negative material is 1：100~10：1；
Anode, diaphragm, cathode are assembled into lithium ion super capacitor, added in after electrolyte to the pre- embedding lithium of battery charging.
2. according to the method for claim 1, it is characterised in that：
Battery charging pre-embedding lithium method includes the pre- embedding lithium of constant current or the pre- embedding lithium of constant pressure；
The pre- embedding lithium of battery constant current, electric current are 0.01mA-10A/ per the pre- embedding lithium additives of g, charge cutoff voltage 0.42V-5V；
The pre- embedding lithium of battery constant pressure, voltage 0.42V-5V, cut-off current are 0.001m A-1m A.
3. according to the method for claim 1, it is characterised in that：The pre- embedding lithium additive is lithia, lithium peroxide, nitrogen
Change lithium, charing lithium in it is one or two kinds of more than.
4. according to the method for claim 1, it is characterised in that：
The pre- embedding lithium additive for preferred lithia, lithium peroxide, lithium nitride it is one or two kinds of more than；Pre- embedding lithium addition
The mass ratio of agent and negative material is 1:5~5:1.
5. according to the method for claim 1, it is characterised in that：
The active material includes absorbent charcoal material, conducting polymer, more than one or two kinds of in oxide.
6. according to the method for claim 5, it is characterised in that：
The absorbent charcoal material includes active carbon powder, activated carbon fibre, carbon aerogels, carbon nanotube, graphene, carbon black etc.
In it is one or two kinds of more than；The conducting polymer include polyaniline, polythiophene, polypyrrole, polypyridine, polyphenyl and its
It is more than one or two kinds of in derivative；
The oxide includes manganese dioxide, ruthenium-oxide, more than one or two kinds of in titanium dioxide.
7. method in accordance with claim, it is characterised in that：
The diaphragm is polyethylene diagrams, polypropylene diaphragm, polyethylene, polypropylene composite materials diaphragm, cellulosic separator, glass fibers
The plain diaphragm of dimension or ceramic membrane.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109686923A (en) * | 2018-12-17 | 2019-04-26 | 深圳先进技术研究院 | The preparation method of pre- embedding cathode of lithium and pre- embedding cathode of lithium, energy storage device, energy-storage system and the electrical equipment being prepared |
| CN110246699A (en) * | 2019-05-17 | 2019-09-17 | 中国科学院电工研究所 | A kind of anode electrode piece of lithium-ion capacitor, lithium-ion capacitor and its cathode pre-embedding lithium method |
| CN111105938A (en) * | 2018-10-26 | 2020-05-05 | 中国科学院大连化学物理研究所 | Lithium pre-embedding method for negative electrode of lithium ion super capacitor |
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|---|---|---|---|---|
| CN101252043A (en) * | 2007-04-25 | 2008-08-27 | 北京理工大学 | Pre-embedding method of lithium ion super capacitor cathode |
| CN101847516A (en) * | 2010-02-26 | 2010-09-29 | 上海奥威科技开发有限公司 | Capacitor battery of high-specific-energy organic system |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101252043A (en) * | 2007-04-25 | 2008-08-27 | 北京理工大学 | Pre-embedding method of lithium ion super capacitor cathode |
| CN101847516A (en) * | 2010-02-26 | 2010-09-29 | 上海奥威科技开发有限公司 | Capacitor battery of high-specific-energy organic system |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111105938A (en) * | 2018-10-26 | 2020-05-05 | 中国科学院大连化学物理研究所 | Lithium pre-embedding method for negative electrode of lithium ion super capacitor |
| CN109686923A (en) * | 2018-12-17 | 2019-04-26 | 深圳先进技术研究院 | The preparation method of pre- embedding cathode of lithium and pre- embedding cathode of lithium, energy storage device, energy-storage system and the electrical equipment being prepared |
| CN109686923B (en) * | 2018-12-17 | 2020-07-17 | 深圳先进技术研究院 | Preparation method of pre-lithium-intercalated negative electrode, pre-lithium-intercalated negative electrode prepared by preparation method, energy storage device, energy storage system and electric equipment |
| CN110246699A (en) * | 2019-05-17 | 2019-09-17 | 中国科学院电工研究所 | A kind of anode electrode piece of lithium-ion capacitor, lithium-ion capacitor and its cathode pre-embedding lithium method |
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