CN107195463A - One kind contains Li2MoO3The preparation method of coating positive plate - Google Patents
One kind contains Li2MoO3The preparation method of coating positive plate Download PDFInfo
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- CN107195463A CN107195463A CN201610619940.8A CN201610619940A CN107195463A CN 107195463 A CN107195463 A CN 107195463A CN 201610619940 A CN201610619940 A CN 201610619940A CN 107195463 A CN107195463 A CN 107195463A
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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
- H01G11/04—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 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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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 provides a kind of containing Li2MoO3The preparation method of coating positive plate.Including following steps：Step（1）By Li2CO3And MoO3Mixing, is put into Muffle reaction in furnace after being well mixed, reaction obtains Li after terminating2MoO4Material；Step（2）Li will be obtained2MoO4The Muffle reaction in furnace of hydrogen nitrogen mixed gas atmosphere protection is put into, reaction obtains Li after terminating2MoO3Material；Step（3）By Li2MoO3Material, conductive agent, binding agent, which are added in NMP, is mixed into slurry, is then coated with containing active material positive plate, is obtained after drying containing Li2MoO3Coating positive plate.The present invention has the advantages that：（1）Contain Li2MoO3The positive plate of coating makes negative pole to add the pre- embedding lithium technique of lithium piece or complexity for the positive pole of lithium ion super capacitor, simplifies preparation technology, reduces cost.
Description
Technical field
The invention belongs to lithium ion super capacitor technical field, it is related to a kind of system of lithium ion super capacitor positive plate
Preparation Method.
Background technology
In recent years, lithium rechargeable battery has obtained very big development, and this GND is typically using the charcoals such as graphite element
Material, positive pole contains lithium metal oxide using cobalt acid lithium, LiMn2O4 etc..After this battery pack is filled with, negative pole is to positive pole during charging
Lithium ion is provided, and the lithium ion of positive pole returns to negative pole in electric discharge, therefore it is referred to as " rocking chair type battery ".With using metal
The lithium battery of lithium is compared, the characteristics of this battery has high security and high circulation life-span.
But, due to the deformation of positive electrode easy recurring structure during removal lithium embedded, therefore, lithium ion secondary electricity
The cycle life in pond is still restricted.Therefore in recent years, the body that lithium rechargeable battery and double layer capacitor are combined together
System's research turns into new focus.
The carbon materials such as lithium-ion capacitor general anode material selection graphite, hard carbon, positive electrode is special from electric double layer
Property absorbent charcoal material, by negative material carry out lithium ion pre-doping, negative pole current potential is significantly declined, so as to improve
Energy density.A kind of lithium-ion capacitor is disclosed in patent CN200580001498.2, what this lithium-ion capacitor was used
Plus plate current-collecting body and negative current collector are respectively provided with through the hole of positive and negative, respectively by positive active material and negative electrode active material shape
Into electrode layer, by carrying out electrochemical contact to negative pole, lithium ion is carried in negative pole in advance.Patent
A kind of preprocess method of electrochemical capacitor negative pole is disclosed in CN200780024069.6, passes through vapor phase method or liquid phase
Method forms lithium layer on substrate, and then the lithium layer is transferred to the electrode layer of negative pole.The work that the method for these pre-doping is related to
Skill is more complicated, and raw material are needed to carry out specially treated, and certain difficulty is brought to manufacturing process.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of lithium ion super capacitor positive plate, the party
Positive plate prepared by method can provide lithium source in lithium-ion capacitor, without being carried out again to negative pole at complicated pre- embedding lithium
Reason adds lithium piece in lithium-ion capacitor, simplifies the technical process of lithium-ion capacitor preparation, reduces its technique
Cost.
The preparation method for the lithium ion super capacitor positive plate that the present invention is provided is：
Step（1）By Li2CO3And MoO31-2 in molar ratio:1 ratio mixing, 500-700 in Muffle furnace is put into after being well mixed
DEG C reaction 3-8 hour, react terminate after obtain Li2MoO4Material.
Step（2）Li will be obtained2MoO4Material is put into the Muffle of the hydrogen nitrogen mixed gas atmosphere protection of the hydrogen containing volumetric concentration 5%
500-900 DEG C is reacted 5-10 hours in stove, and reaction obtains Li after terminating2MoO3Material.
Step（3）By Li2MoO3Material, conductive agent, binding agent are according to 80-90:5-10:5-10 mass ratio is added to
Slurry is mixed into NMP, is then coated with containing active material positive plate, is obtained after drying containing Li2MoO3Coating positive pole
Piece.
It is as follows that the present invention provides a kind of preparation technology flow of lithium ion super capacitor：
（1）By activated carbon or graphene anode material, conductive agent, binding agent according to 90:5:5 ratio is added in NMP and mixed
Synthetic slurry, is then coated with plus plate current-collecting body aluminium foil, positive plate is obtained after drying.
（2）By Li2MoO3Material, conductive agent, binding agent are according to 80-90:5-10:5-10 mass ratio is added in NMP
Slurry is mixed into, is then coated with containing active material positive plate, is obtained after drying containing Li2MoO3Coating positive plate.
（3）By graphite or hard charcoal negative material, conductive agent, binding agent according to mass ratio 90:5:5 ratio is added to
Slurry is mixed into NMP, is then coated with negative current collector copper foil paper tinsel, negative plate is obtained after drying.
（4）According to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate the group by way of lamination
Into battery core, electrolyte is then injected in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
Volume ratio with DME is 1:1), seal, obtain lithium ion super capacitor.
Use positive electrode of the present invention to prepare the technique of lithium ion super capacitor and prepare work for general lithium ion battery
Skill, enormously simplify the preparation technology of lithium ion super capacitor.
Prepared by the present invention contains Li2MoO3When the positive plate of coating is used as lithium ion super capacitor positive electrode,
Li2MoO3Material provides lithium source, and in initial charge, lithium ion deviates from Li2MoO3Material is inserted into graphite cathode, so as to drag down
Negative pole current potential, therefore need not be using metal lithium sheet or the pre- embedding lithium technique of complexity in negative pole；While Li2MoO3Material is sloughed
Li is formed after lithium ion2-xMoO3Material is electrochemicaUy inert material, does not influence the normal of battery to use.
The present invention has the advantages that：（1）Contain Li2MoO3The positive plate of coating is lithium ion super capacitor
Positive pole makes negative pole to add the pre- embedding lithium technique of lithium piece or complexity, simplifies preparation technology, reduces cost.
Brief description of the drawings
Fig. 1 is lithium ion super capacitor positive plate structural representation of the present invention.
In figure, 1-plus plate current-collecting body, 2-active material positive plate, 3-Li2MoO3Coating.
Embodiment
Below in conjunction with the accompanying drawings, the preferably embodiment to the present invention is described in further detail：
Embodiment 1
（1）By Li2CO3And MoO3In molar ratio 1:1 ratio mixing, is put into 500 DEG C of reactions 3 in Muffle furnace small after being well mixed
When, reaction obtains Li after terminating2MoO4。
（2）Li will be obtained2MoO4It is put into the Muffle furnace containing volumetric concentration for the hydrogen nitrogen mixed gas atmosphere protection of 5% hydrogen
500 DEG C are reacted 5 hours, and reaction obtains Li after terminating2MoO3Material.
（3）By absorbent charcoal material, conductive agent Ketjen black, binding agent PVDF according to mass ratio 90:5:5 ratio is added to
Slurry is mixed into NMP, is then coated with the aluminium foil of plus plate current-collecting body 1, positive plate is obtained after drying.
（4）By Li2MoO3Material, conductive agent Ketjen black, binding agent PVDF are according to mass ratio 80: 10:10 mass ratio
It is added in NMP and is mixed into slurry, is then coated with containing active material positive plate 2, is obtained after drying containing Li2MoO3Apply
3 positive plate of layer.
（5）By graphite cathode material, conductive agent Ketjen black, binding agent PVDF according to mass ratio 90:5:5 ratio is added to
Slurry is mixed into NMP, is then coated with negative current collector copper foil, negative plate is obtained after drying.
（6）According to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate the group by way of lamination
Into battery core, electrolyte is then injected in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
Volume ratio with DME is 1:1), seal, obtain lithium ion super capacitor.
Embodiment 2
（1）By Li2CO3And MoO3In molar ratio 2:1 ratio mixing, is put into 700 DEG C of reactions 8 in Muffle furnace small after being well mixed
When, reaction obtains Li after terminating2MoO4。
（2）Li will be obtained2MoO4It is put into the Muffle furnace containing volumetric concentration for the hydrogen nitrogen mixed gas atmosphere protection of 5% hydrogen
900 DEG C are reacted 10 hours, and reaction obtains Li after terminating2MoO3Material.
（3）By absorbent charcoal material, conductive agent, binding agent according to mass ratio 90:5:5 ratio, which is added in NMP, to be mixed into
Slurry, is then coated with the aluminium foil of plus plate current-collecting body 1, positive plate is obtained after drying.
（4）By Li2MoO3Material, conductive agent Ketjen black, binding agent PVDF are according to mass ratio 90:5:5 mass ratio is added
Slurry is mixed into NMP, is then coated with containing active material positive plate 2, is obtained after drying containing Li2MoO3Coating 3 is just
Pole piece.
（5）By hard charcoal negative material, conductive agent Ketjen black, binding agent PVDF according to mass ratio 90:5:5 ratio is added to
Slurry is mixed into NMP, is then coated with negative current collector copper foil paper tinsel, negative plate is obtained after drying.
（6）According to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate the group by way of lamination
Into battery core, electrolyte is then injected in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
Volume ratio with DME is 1:1), seal, obtain lithium ion super capacitor.
Embodiment 3
（1）By Li2CO3And MoO3In molar ratio 1.3:1 ratio mixing, is put into 600 DEG C of reactions 7 in Muffle furnace after being well mixed
Hour, reaction obtains Li after terminating2MoO4。
（2）Li will be obtained2MoO4It is put into 700 in the Muffle furnace of the hydrogen nitrogen mixed gas atmosphere protection of the hydrogen containing volumetric concentration 5%
DEG C reaction 8 hours, reaction terminate after obtain Li2MoO3Material.
（3）By absorbent charcoal material, conductive agent Ketjen black, binding agent PVDF according to mass ratio 90:5:5 ratio is added to
Slurry is mixed into NMP, is then coated with the aluminium foil of plus plate current-collecting body 1, positive plate is obtained after drying.
（4）By Li2MoO3Material, conductive agent Ketjen black, binding agent PVDF are according to 85:7:8 mass ratio is added to NMP
In be mixed into slurry, be then coated with containing active material positive plate 2, obtained after drying containing Li2MoO3The positive plate of coating 3.
（5）By graphite cathode material, conductive agent Ketjen black, binding agent PVDF according to mass ratio 90:5:5 ratio is added to
Slurry is mixed into NMP, is then coated with negative current collector copper foil, negative plate is obtained after drying.
（6）According to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate the group by way of lamination
Into battery core, electrolyte is then injected in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
Volume ratio with DME is 1:1), seal, obtain lithium ion super capacitor.
Embodiment 4
（1）By Li2CO3And MoO3In molar ratio 1.5:1 ratio mixing, is put into 650 DEG C of reactions 5 in Muffle furnace after being well mixed
Hour, reaction obtains Li after terminating2MoO4。
（2）Li will be obtained2MoO4It is put into the Muffle furnace containing volumetric concentration for the hydrogen nitrogen mixed gas atmosphere protection of 5% hydrogen
600 DEG C are reacted 8 hours, and reaction obtains Li after terminating2MoO3Material.
（3）By absorbent charcoal material, conductive agent Ketjen black, binding agent PVDF according to 90:5:5 ratio is added in NMP and mixed
Synthetic slurry, is then coated with the aluminium foil of plus plate current-collecting body 1, positive plate is obtained after drying.
（4）By Li2MoO3Material, conductive agent Ketjen black, binding agent PVDF are according to 82:9:9 mass ratio is added to NMP
In be mixed into slurry, be then coated with containing active material positive plate 2, obtained after drying containing Li2MoO3The positive plate of coating 3.
（5）By hard charcoal negative material, conductive agent Ketjen black, binding agent PVDF according to mass ratio 90:5:5 ratio is added to
Slurry is mixed into NMP, is then coated with negative current collector copper foil, negative plate is obtained after drying.
（6）According to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate the group by way of lamination
Into battery core, electrolyte is then injected in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
Volume ratio with DME is 1:1), seal, obtain lithium ion super capacitor.
Embodiment 5
（1）By Li2CO3And MoO3In molar ratio 1.7:1 ratio mixing, is put into 600 DEG C of reactions 6 in Muffle furnace after being well mixed
Hour, reaction obtains Li after terminating2MoO4。
（2）Li will be obtained2MoO4It is put into the Muffle furnace containing volumetric concentration for the hydrogen nitrogen mixed gas atmosphere protection of 5% hydrogen
800 DEG C are reacted 6 hours, and reaction obtains Li after terminating2MoO3Material.
（3）By absorbent charcoal material, conductive agent Ketjen black, binding agent PVDF according to mass ratio 90:5:5 ratio is added to
Slurry is mixed into NMP, is then coated with the aluminium foil of plus plate current-collecting body 1, positive plate is obtained after drying.
（4）By Li2MoO3Material, conductive agent Ketjen black, binding agent PVDF are according to 88:6:6 mass ratio is added to NMP
In be mixed into slurry, be then coated with containing active material positive plate 2, obtained after drying containing Li2MoO3The positive plate of coating 3.
（5）By graphite cathode material, conductive agent Ketjen black, binding agent PVDF according to mass ratio 90:5:5 ratio is added to
Slurry is mixed into NMP, is then coated with negative current collector copper foil, negative plate is obtained after drying.
（6）According to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate the group by way of lamination
Into battery core, electrolyte is then injected in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
Volume ratio with DME is 1:1), seal, obtain lithium ion super capacitor.
Its effect is as shown in table 1, as shown in Table 1：Lithium ion super capacitor energy density prepared by the present invention reaches
34.6-37.1 wh/kg, have reached the fluence level of conventional lithium ion super capacitor.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Energy density（wh/kg） | 35.2 | 36.6 | 37.1 | 34.8 | 34.6 |
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert this hair
Bright specific implementation is confined to these explanations.For general technical staff of the technical field of the invention, do not taking off
On the premise of from present inventive concept, some simple deduction or replace can also be made, the protection of the present invention should be all considered as belonging to
Scope.
Claims (10)
1. a kind of preparation method of lithium ion super capacitor positive plate, it is characterised in that including following steps：
Step（1）By Li2CO3And MoO3Mixing, is put into Muffle reaction in furnace after being well mixed, reaction obtains Li after terminating2MoO4
Material；
Step（2）Li will be obtained2MoO4Material is put into the Muffle reaction in furnace of hydrogen nitrogen mixed gas atmosphere protection, and reaction is obtained after terminating
To Li2MoO3Material；
Step（3）By Li2MoO3Material, conductive agent, binding agent, which are added in NMP, is mixed into slurry, is then coated with containing active
On material positive plate, obtained after drying containing Li2MoO3Coating positive plate.
2. the method as described in claim 1, it is characterised in that the step（1）Middle Li2CO3And MoO3Amount 1- in molar ratio
2:1 ratio mixing.
3. the method as described in claim 1, it is characterised in that the step（1）Reaction temperature in Muffle furnace is 500-
700 DEG C, the reaction time is 3-8 hours.
4. the method as described in claim 1, it is characterised in that the step（2）Atmosphere in middle Muffle furnace is containing 5% hydrogen
Hydrogen nitrogen mixed gas.
5. the method as described in claim 1, it is characterised in that the step（2）Reaction temperature in Muffle furnace is 500-
900 DEG C, the reaction time is 5-10 hours.
6. the method as described in claim 1, it is characterised in that the step（3）Middle Li2MoO3Material, conductive agent, binding agent
Mass ratio be 80-90:5-10:5-10.
7. a kind of preparation technology of lithium ion super capacitor, it is characterised in that including following steps：
Step A:Activated carbon or graphene anode material, conductive agent and binding agent are added in NMP and are mixed into slurry, then
It is coated on plus plate current-collecting body aluminium foil, positive plate is obtained after drying；
Step B:By the Li as prepared by claim 12MoO3Material, conductive agent, binding agent, which are added in NMP, is mixed into slurry,
It is then coated with containing active material positive plate, is obtained after drying containing Li2MoO3Coating positive plate;
Step C:Graphite or hard charcoal negative material, conductive agent, binding agent are added in NMP and are mixed into slurry, is then coated with
On negative current collector copper foil paper tinsel, negative plate is obtained after drying；
Step D:Negative plate, barrier film and positive plate are constituted into battery core by way of lamination, electrolysis is then injected in battery case
Liquid, sealing, obtains lithium ion super capacitor.
8. preparation technology as claimed in claim 7, it is characterised in that in the step A, graphene is combined Li2MoO3Material,
Conductive agent, the mass ratio of binding agent are 90:5:5.
9. preparation technology as claimed in claim 7, it is characterised in that in the step B, graphite or hard charcoal negative material,
Conductive agent, the mass ratio of binding agent are 90:5:5.
10. preparation technology as claimed in claim 7, it is characterised in that in the step C, the electrolyte is 1mol/L
LiPF6DOL-DME solution, wherein, DOL and DME volume ratio is 1:1.
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| CN201610619940.8A CN107195463A (en) | 2016-07-31 | 2016-07-31 | One kind contains Li2MoO3The preparation method of coating positive plate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109935831A (en) * | 2017-12-18 | 2019-06-25 | 上海纳晓能源科技有限公司 | Electrode inertness material, combination electrode, production method and lithium ion battery |
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| WO2012043398A1 (en) * | 2010-09-29 | 2012-04-05 | エスペック株式会社 | Method for drying electrode pair, method for manufacturing lithium-ion secondary battery, method for manufacturing electric double-layer capacitor, and method for manufacturing lithium-ion capacitor |
| CN103515110A (en) * | 2012-06-26 | 2014-01-15 | 海洋王照明科技股份有限公司 | Li2MoO3/graphene composite material, preparing method thereof and lithium ion capacitor |
| CN104577088A (en) * | 2013-10-16 | 2015-04-29 | 中国科学院物理研究所 | Lithium molybdate serving as secondary battery electrode material |
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2016
- 2016-07-31 CN CN201610619940.8A patent/CN107195463A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101165827A (en) * | 2007-08-29 | 2008-04-23 | 李青海 | Mixed electrochemical capacitor and its manufacture method |
| WO2012043398A1 (en) * | 2010-09-29 | 2012-04-05 | エスペック株式会社 | Method for drying electrode pair, method for manufacturing lithium-ion secondary battery, method for manufacturing electric double-layer capacitor, and method for manufacturing lithium-ion capacitor |
| CN103515110A (en) * | 2012-06-26 | 2014-01-15 | 海洋王照明科技股份有限公司 | Li2MoO3/graphene composite material, preparing method thereof and lithium ion capacitor |
| CN104577088A (en) * | 2013-10-16 | 2015-04-29 | 中国科学院物理研究所 | Lithium molybdate serving as secondary battery electrode material |
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| CN109935831A (en) * | 2017-12-18 | 2019-06-25 | 上海纳晓能源科技有限公司 | Electrode inertness material, combination electrode, production method and lithium ion battery |
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Application publication date: 20170922 |