CN102386439A - Lithium ion secondary battery - Google Patents
Lithium ion secondary battery Download PDFInfo
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- CN102386439A CN102386439A CN2010102748466A CN201010274846A CN102386439A CN 102386439 A CN102386439 A CN 102386439A CN 2010102748466 A CN2010102748466 A CN 2010102748466A CN 201010274846 A CN201010274846 A CN 201010274846A CN 102386439 A CN102386439 A CN 102386439A
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of batteries, and in particular discloses a lithium ion secondary battery. The lithium ion secondary battery comprises a battery shell, a pole core and an electrolyte, wherein the pole core and the electrolyte are hermetically accommodated in the battery shell; the pole core comprises an anode, a cathode and a diaphragm; the anode and the cathode comprise current collectors and anode and cathode materials; the electrolyte comprises a lithium salt, an organic solvent and an additive; the cathode material comprises a carbon material and a silicon nano wire; and the negative ions in the lithium salt are selected from one or more of perfluoroalkyl negative ions, chelate boron negative ions, organic aluminate negative ions, chelate phosphorus negative ions, perfluoro-phosphine negative ions, imido negative ions and silicon amido negative ions. Compared with the conventional silicon nano wire battery, the lithium ion secondary battery has the advantages that: the cycle performance of the battery is greatly improved, so that the service life of the battery is greatly prolonged.
Description
Technical field
The invention belongs to the battery technology field, relate in particular to a kind of lithium rechargeable battery.
Background technology
At present, the negative pole of lithium rechargeable battery adopts the graphite-like material with carbon element more, but its theoretical specific capacity is low.Silicon materials enjoy industry to pay close attention to its huge theoretical lithium storage content.Lithium can obtain different alloy products with pasc reaction, like Li
12Si
17, Li
13Si
4, Li
7Si
3, Li
22Si
5Deng, the alloy Li that forms when wherein Si embeds lithium
4.4Si, its theoretical capacity reaches more than the 4200mAh/g, and theoretical capacity is the highest in the various alloys of research at present.
But silicon materials are in the charge and discharge cycles process; The reversible generation of Li-Si alloy is accompanied by huge change in volume (reaching 400%) with decomposition; Can cause the mechanical disintegration (producing crack and efflorescence) of alloy; Cause avalanche and the peeling off of electrode material of material structure and electrode material is lost electrically contacting, thereby cause the cycle performance of electrode sharply to descend, cause electrode failure at last.
At present, silicon nanowires is owing to its one-dimentional structure, and it has enough volumetric expansion spaces in embedding lithium process, thereby can bear bigger swelling stress and not efflorescence.In addition, silicon nanowires directly contacts with collector, has guaranteed the continuous of lithium ion radial diffusion, thereby the good electron path is provided and has shortened lithium ion diffusion length.Silicon nanowires can also bear bigger stress and plastic deformation, aspect toughness of material, also improves a lot.But, adopt silicon nanowires as negative material, the cycle performance of battery still is not ideal enough.
Summary of the invention
Technical problem to be solved by this invention is: in the prior art, adopt silicon nanowires as the bad problem of the lithium ion battery cycle performance of negative pole; Provide a kind of cycle performance good lithium rechargeable battery.
A kind of lithium rechargeable battery, it comprises battery case, pole piece and electrolyte, said pole piece and electrolyte sealing are contained in the battery case;
Said pole piece comprises positive pole, negative pole and the barrier film between positive pole and negative pole, and said positive pole comprises collector and load on the positive electrode on the collector that said negative pole comprises collector and loads on the negative material on the collector;
Said electrolyte comprises lithium salts, organic solvent;
Wherein, said negative material comprises material with carbon element and silicon nanowires; Anion is selected from one or more in perfluoroalkyl anion, chelating boron anion, organo-aluminium acidic group anion, chelating phosphorus anion, perfluor phosphine anion, imido grpup anion and the silica-based amido anion in the said lithium salts.
Lithium rechargeable battery provided by the present invention is compared existing silicon nanowires battery, and its cycle performance of battery has had significantly raising, thereby has prolonged the useful life of battery greatly.
Description of drawings
Fig. 1 is the SEM figure (2 μ m) of one embodiment of the invention negative material.
Fig. 2 is the SEM figure (5 μ m) of one embodiment of the invention negative material.
Embodiment
Clearer for technical problem, technical scheme and beneficial effect that the present invention is solved, below in conjunction with accompanying drawing and embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
A kind of lithium rechargeable battery, it comprises battery case, pole piece and electrolyte, said pole piece and electrolyte sealing are contained in the battery case;
Said pole piece comprises positive pole, negative pole and the barrier film between positive pole and negative pole, and said positive pole comprises collector and load on the positive electrode on the collector that said negative pole comprises collector and loads on the negative material on the collector;
Said electrolyte comprises lithium salts, organic solvent;
Wherein, said negative material comprises material with carbon element and silicon nanowires; Anion is selected from one or more in perfluoroalkyl anion, chelating boron anion, organo-aluminium acidic group anion, chelating phosphorus anion, perfluor phosphine anion, imido grpup anion and the silica-based amido anion in the said lithium salts.
In lithium rechargeable battery of the present invention, positive pole there is not specific (special) requirements, positive pole can be a positive pole common in the lithium rechargeable battery.
In the present invention, the collector in the positive pole is known in those skilled in the art, does not give unnecessary details at this.
Positive electrode also is known in those skilled in the art, generally comprises cobalt nickel manganese series, series of phosphate, titanium series, vanadium series etc.Common positive electrode has: lithium cobalt oxygen LiCoO
2, lithium nickel oxygen LiNiO
2, lithium manganese oxygen LiMnO
2, lithium-nickel-cobalt-oxygen, lithium nickel cobalt manganese oxygen, LiFePO
4, Li
3V
2(PO
4)
3, LiMnPO
4, Li
2FeSiO
4, Li
2MnSiO
4, LiVO
2, Li
2V
2O
4, LiV
3O
8And above-mentioned substance coats or the product of doping.
The present invention preferably includes LiCoO
2, LiMnO
2, LiNiO
2, Li (Ni
0.8Co
0.2) O
2, LiNi
1/3Co
1/3Mn
1/3O
2, LiFePO
4, Li
3V
2(PO
4)
3, LiV
3O
8In one or more.
Binding agent and conductive agent are known in those skilled in the art in the positive pole, do not give unnecessary details at this.
Anodal preparation method mixes positive electrode, conductive agent and binding agent to obtain required anode sizing agent by a certain percentage in solvent, then with this slurry coating on collector, through super-dry, compressing tablet handle promptly get anodal.
The present invention is used for the positive electrode solvent can be selected from the conventional solvent that uses in this area; As can be selected from N-methyl pyrrolidone (NMP), N; Dinethylformamide (DMF), N, one or more in N-DEF (DEF), methyl-sulfoxide (DMSO), oxolane (THF) and water and the alcohols.The consumption of solvent can be coated on the said collector said slurry and gets final product.In general, the consumption of solvent is that to make the concentration of positive electrode in the slurries be 40~90wt%, is preferably 50~85wt%.
In lithium rechargeable battery of the present invention, negative pole comprises collector and loads on the negative material on the collector.This negative material comprises material with carbon element and silicon nanowires, and material with carbon element is graininess, and silicon nanowire distribution is on said material with carbon element;
Wherein, silicon nanowires is a material known in those skilled in the art.It is an one-dimentional structure, can also can oneself prepare through being purchased acquisition.
Silicon nanowires of the present invention can be the silicon nanowires of whole crystal structures, can also be all to be the silicon nanowires of amorphous silicon, more can be that the surface is amorphous silicon, and inside is the silicon nanowires of the nucleocapsid structure of crystal structure.
Under the preferable case, the average diameter of silicon nanowires of the present invention is 10~120nm, and length is 1~20 μ m.More preferably average diameter is 20~80nm, and length is 2~10 μ m.
Wherein, material with carbon element also is a material known in those skilled in the art.
Material with carbon element of the present invention is preferably selected among graphite, hard carbon, soft carbon and the graphitization mesophase-carbon micro-beads MCMB one or more; Graphite more preferably.
The preferred material with carbon element of the present invention is graininess, and silicon nanowires is coated on the material with carbon element.
The microscopic appearance of material with carbon element can be spherical, type sphere or laminar structured.
Under the preferable case, the median particle diameter D of material with carbon element of the present invention
50Be 2~20 μ m, 5~15 μ m more preferably.
The mass ratio of silicon nanowires and material with carbon element is 1: 99~50: 50 among the present invention, more preferably 2: 98~20: 80.Can make the capacity and the cycle performance of battery all be in higher level like this.
Also comprise the negative pole binding agent in the negative pole, the negative pole binding agent is a negative pole binding agent conventionally known to one of skill in the art.Negative pole binding agent of the present invention can be selected from polythiophene, polypyrrole, polytetrafluoroethylene, Kynoar, polyethylene, polypropylene, polyacrylamide, ethylene-propylene-diene copolymer resins, styrene butadiene ribber, polybutadiene, fluorubber, gather in oxireme, polyvinylpyrrolidone, mylar, acrylic resin, phenolic resins, epoxy resin, polyvinyl alcohol, carboxy-propyl cellulose and the ethyl cellulose one or more.
Negative pole of the present invention can also optionally contain the common conductive agent that contains in the prior art negative pole.Because conductive agent is used to increase the conductivity of electrode, reduce the internal resistance of battery, so the present invention preferably contains conductive agent.The content of said conductive agent and kind are conventionally known to one of skill in the art, for example, are benchmark with the negative material, and the content of conductive agent is generally 0.1~12wt%.Said conductive agent can be selected from one or more in conductive carbon black, CNT, nickel powder, the copper powder.
According to the difference of used binding agent kind, be benchmark with the weight of negative material, the content of negative pole binding agent is 0.01~10wt%, is preferably 0.02~5wt%; The content of conductive agent is 0~12wt%, is preferably 2~10wt%.
The preparation technology of negative pole mixes negative material, binding agent to obtain required cathode size by a certain percentage in solvent, then with this slurry coating on collector, handle promptly to get negative pole through super-dry, compressing tablet.The normal solvent that adopts is N-methyl pyrrolidone (NMP), water, ethanol, acetone etc., is benchmark with the negative material, and the consumption of solvent is 50-400%.
In lithium rechargeable battery of the present invention, barrier film is arranged between positive pole and the negative pole, has electrical insulation capability and liquid retainability ability.Said barrier film can be selected from and well known to a person skilled in the art various barrier films used in the lithium rechargeable battery, for example polyolefin micro porous polyolefin membrane (PP), polyethylene felt (PE), glass mat or ultra-fine fibre glass paper or PP/PE/PP.Said barrier film also can be a polyimide film.Said polyimide film can be polyimide film known in those skilled in the art, and preferably its porosity is 20%~55%, and average pore diameter is 30~120nm.
In lithium rechargeable battery of the present invention, contain lithium salts, organic solvent in the electrolyte.
Wherein, the anion of lithium salts is selected from the anion one or more in the electrolyte:
Alkyl sulfonic acid anion, perfluoroalkyl anion, chelating boron anion, organo-aluminium acidic group anion, chelating phosphorus anion, perfluor phosphine anion, imido grpup anion and silica-based amido anion.
Under the preferable case, lithium salts of the present invention is selected from LiB (C
2O
4)
2, Li
2Al (CSO
3Cl
4), LiP (C
6H
4O
2)
3, LiPF
3(C
2F
5)
3And LiN (SiC
3H
9)
2In one or more.
The concentration of the preferred lithium salts of the present invention is for being 0.3~3mol/L, more preferably 0.5~1.5mol/L.
Organic solvent in the electrolyte of the present invention can adopt this area solvent commonly used, for example EC (vinyl carbonate), PC (propylene carbonate), FEC (fluorinated ethylene carbonate), DEC (diethyl carbonate), DMC (dimethyl carbonate), EMC (ethyl-methyl carbonic ester), DME (dimethoxy-ethane), GBL (gamma-butyrolacton), DMC (dimethyl carbonate), MF (methyl formate), MA (methyl acrylate), MB (methyl butyrate), EP (ethyl acetate), ES (ethylene sulfite), PS (propylene sulfite), DMS (methyl sulfide), DES (diethyl sulfite) etc.
In optimal ethylene carbonic ester of the present invention, propylene carbonate, fluorinated ethylene carbonate, diethyl carbonate, dimethyl carbonate, the ethyl-methyl carbonic ester one or more.
Also preferably contain additive in the electrolyte of the present invention, additive can be selected additive known in those skilled in the art for use.
The preparation method of lithium rechargeable battery of the present invention carries out according to method as well known to those skilled in the art.In general, this method comprises reels positive pole, negative pole and the barrier film between positive pole and negative pole or range upon range of formation pole piece successively, and pole piece is inserted in the battery case; Add electrolyte; Sealing then, wherein, the method for coiling and sealing is that those skilled in the art are known.The consumption of electrolyte is a conventional amount used.
Inventor of the present invention is through a large amount of experimental studies and analyze discovery; Cause that the bad reason of silicon nanowires cycle performance of battery mainly is in the prior art: the surface of silicon nanowires inevitably exists the oxide of certain silicon; The oxide of silicon can change the surface state character and the surface charge of silicon nanowires, thus guaranteed silicon nanowires can stable existence in air.But the oxide of this silicon can react with the anion of lithium salts in the electrolyte of the prior art, thereby lithium salts is decomposed.With the most frequently used LiPF
6Be example, LiPF
6In battery, there is following balance:
LiPF
6=LiF+PF
5,
And 2PF
5+ SiO
2=SiF
4↑+2PF
3O
Thereby cause LiPF
6And the lasting decomposition reaction of other similar inorganic lithium salts, from influencing the performance of electrolyte.Simultaneously, when changing into since above-mentioned reaction continue carry out, be unfavorable for forming the SEI film on the surface of silicon nanowires.Thereby have a strong impact on the cycle performance of silicon nanowires battery.Secondly, the factor that influences the silicon nanowires cycle performance of battery also has: the electronic conductivity of silicon nanowires itself is low, and silicon nanowires easy caking in charge and discharge process, can aggravate electronic conductivity and reduce.
Inventor of the present invention is unexpected to be found: silicon nanowire material is distributed in the material with carbon element, adopts lithium salts of the present invention, the cycle performance of battery to have significantly in the electrolyte and improve.
The reason that inventor of the present invention infers is: the organic anion of lithium salts has better chemical stability among the present invention for silicon nanowires; Thereby can effectively suppress the boundary response between silicon nanowires and the electrolyte, and help on silicon nanowires, forming stable interfacial film SEI film.Simultaneously, organic anion has bigger ionic radius, can anionic electric charge carry out delocalizationization, thereby reduces lattice energy, reduces the interaction between the ion, has guaranteed dissolubility and conductivity.Silicon nanowire distribution of the present invention on material with carbon element, the caking phenomenon of silicon nanowires in the time of on the one hand can effectively suppressing to discharge and recharge; On the other hand, material with carbon element is good electronic conductor, can remedy the problem of the electronic conductivity of silicon nanowires.Thereby the conductivity that makes negative material has had significantly raising.Finally cause the raising of cycle performance of battery.
Below in conjunction with specific embodiment the present invention is done further elaboration.
Embodiment 1
(1) making of positive pole:
With 940gLiCoO
2, 30g PVDF, 30g conductive agent acetylene black join among the 600g solvent NMP, in de-airing mixer, stirs then, forms the anode sizing agent of stable uniform.This slurry intermittently is coated on the two sides of aluminium foil (aluminium foil is of a size of: width 160mm, thickness 16 μ m) equably, 120 ℃ of oven dry then, behind the roll squeezer compressing tablet, the pole piece of cutting out to being of a size of 480mm*45mm promptly gets anode pole piece.
(2) making of negative pole:
Earlier the 1000g deionized water is joined in the 60g silicon nanowires, ultrasonic dispersing 60min adds 940g graphite (Japanese NCK, D then while stirring to the disappearance of floccule mass aggressiveness
50=15 μ m), treat that graphite all adds after, add binding agent CMC solution (wherein CMC content is 60g); Stir simultaneously and ultrasonic dispersing 120min, add certain amount of solvent and regulate slurry viscosity to 2000~3000cp, promptly get electrode slurry.This slurry intermittently is coated on the two sides of Copper Foil (aluminium foil is of a size of: width 160mm, thickness 16 μ m) equably, 120 ℃ of oven dry then, behind the roll squeezer compressing tablet, the pole piece of cutting out to being of a size of 480mm*45mm promptly gets cathode pole piece.
(3) preparation of electrolyte
Is that the mixing of 4: 6 ratios is as solvent, then with electrolyte lithium salt LiN (SiC with EC: DEC with volume ratio
3H
9)
2Be dissolved in the solvent, add certain quantity of additive, preparation electrolyte.Wherein, the concentration of lithium salts is 1mol/L in the electrolyte.
(4) making of battery
Between the positive plate of above-mentioned preparation, negative plate, the PP/PE/PP barrier film is set after reel, sheath body, inject above-mentioned electrolyte, seal, change into etc. makes battery, note is made A1.
Embodiment 2
Different is with embodiment 1: electrolyte lithium salt is LiPF
3(C
2F
5)
3, the lithium salt in the electrolyte is 1.5mol/L, other parts are with embodiment 1.The battery of processing, note is made A2.
Embodiment 3
Different is with embodiment 1: electrolyte lithium salt is LiBC
2O
4F
2, the lithium salt in the electrolyte is 0.5mol/L, other parts are with embodiment 1.The battery of processing, note is made A3.
Embodiment 4
Different is with embodiment 1: electrolyte lithium salt is LiB (C
2O
4)
2, the lithium salt in the electrolyte is 0.8mol/L, he is partly with embodiment 1.The battery of processing, note is made A4.
Embodiment 5
Different is with embodiment 1: electrolyte lithium salt is LiN (SiC
3H
9)
2And LiB (C
2O
4)
2, LiN (SiC in the electrolyte
3H
9)
2Concentration be 0.6mol/L, LiB (C
2O
4)
2Be 0.4mol/L.Other parts are with embodiment 1.The battery of processing, note is made A5.
Embodiment 6
Different is with embodiment 5: the amount of the silicon nanowires in the negative material is 100g, and graphite is 900g.Other parts are with embodiment 1.The battery of processing, note is made A6.
Embodiment 7
Different is with embodiment 5: the amount of the silicon nanowires in the negative material is 150g, and graphite is 850g.Other parts are with embodiment 1.The battery of processing, note is made A7.
Embodiment 8
Different is with embodiment 5: the amount of the silicon nanowires in the negative material is 40g, and graphite is 960g.Other parts are with embodiment 1.The battery of processing, note is made A8.
Comparative Examples 1
Different is with embodiment 1:
The making of step (2) negative pole: earlier the 1000g solvent deionized water is joined in the 200g silicon nanowire material, ultrasonic dispersing 60min disappears to the floccule mass aggressiveness, interpolation CMC (binding agent) solution, and wherein the amount of CMC is 20g; Stirring and ultrasonic dispersing are carried out 120min simultaneously, add certain amount of solvent and regulate slurry viscosity to 2000~3000cp, promptly get electrode slurry.This slurry intermittently is coated on the two sides of Copper Foil (aluminium foil is of a size of: width 160mm, thickness 16 μ m) equably, 120 ℃ of oven dry then, behind the roll squeezer compressing tablet, the pole piece of cutting out to being of a size of 480mm*45mm promptly gets cathode pole piece.
Other parts are with embodiment 1.The battery of processing, note is made AC1.
Comparative Examples 2
Different is with embodiment 1: use LiPF
6Replacement LiN (SiC
3H
9)
2, lithium salt is constant.Other parts are with embodiment 1.The battery of processing, note is made AC2.
Performance Detection:
With the battery of A1-A8 and AC1-AC2 respectively get 50 change into, partial volume, holding up on day BS-9300 secondary cell device for detecting performance, under 23 ± 2 ℃ of conditions, battery is carried out charge and discharge cycles test with 0.2C.Step is following: shelve 10min; Constant voltage charge ends to 4.2V/0.05C; Shelve 10min; Constant-current discharge is to 3.0V; The circulation above-mentioned steps.Getting its mean value inserts in the table 1.
Table 1
Can find out that from table 1 conservation rate of A1-A8 battery is that 80% o'clock cycle-index is compared AC1-AC2 and had significantly and to improve.Also have the capability retention after the circulation 300 times, also had significantly and improved.This explains cycle performance of battery of the present invention, and comparing the silicon nanowires battery has had significantly raising.
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (11)
1. lithium rechargeable battery, it comprises battery case, pole piece and electrolyte, said pole piece and electrolyte sealing are contained in the battery case;
Said pole piece comprises positive pole, negative pole and the barrier film between positive pole and negative pole, and said positive pole comprises collector and load on the positive electrode on the collector that said negative pole comprises collector and loads on the negative material on the collector;
Said electrolyte comprises lithium salts, organic solvent;
It is characterized in that: said negative material comprises material with carbon element and silicon nanowires; Anion is selected from one or more in perfluoroalkyl anion, chelating boron anion, organo-aluminium acidic group anion, chelating phosphorus anion, perfluor phosphine anion, imido grpup anion and the silica-based amido anion in the said lithium salts.
2. lithium rechargeable battery according to claim 1 is characterized in that: said lithium salts is selected from LiB (C
2O
4)
2, Li
2Al (CSO
3Cl
4), LiP (C
6H
4O
2)
3, LiPF
3(C
2F
5)
3And LiN (SiC
3H
9)
2In one or more.
3. lithium rechargeable battery according to claim 2 is characterized in that: said lithium salts is LiB (C
2O
4)
2And LiN (SiC
3H
9)
2
4. lithium rechargeable battery according to claim 1 is characterized in that: the concentration of said lithium salts is 0.3~3mol/L.
5. lithium rechargeable battery according to claim 1 is characterized in that: the average diameter of said silicon nanowires is 20~120nm, and length is 2~10 μ m.
6. lithium rechargeable battery according to claim 1 is characterized in that: the median particle diameter of said material with carbon element is 2~20 μ m.
7. lithium rechargeable battery according to claim 1 is characterized in that: said material with carbon element is graininess, and said silicon nanowires is coated on the said material with carbon element.
8. lithium rechargeable battery according to claim 1 is characterized in that: said material with carbon element is selected from graphite, hard carbon, soft carbon or the graphitization mesophase-carbon micro-beads one or more.
9. lithium rechargeable battery according to claim 8 is characterized in that: the mass ratio of said silicon nanowires and material with carbon element is 1: 99~50: 50.
10. lithium rechargeable battery according to claim 1 is characterized in that: said positive electrode comprises LiCoO
2, LiMnO
2, LiNiO
2, Li (Ni
0.8Co
0.2) O
2, LiNi
1/3Co
1/3Mn
1/3O
2, LiFePO
4, Li
3V
2(PO
4)
3, LiV
3O
8In one or more.
11. lithium rechargeable battery according to claim 1 is characterized in that: said organic solvent is one or more in vinyl carbonate, propylene carbonate, fluorinated ethylene carbonate, diethyl carbonate, dimethyl carbonate, the ethyl-methyl carbonic ester.
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CN104347857A (en) * | 2013-07-29 | 2015-02-11 | 华为技术有限公司 | Lithium ion secondary cell cathode active material and preparation method thereof, lithium ion secondary cell cathode pole piece and lithium ion secondary cell |
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CN107768640B (en) * | 2017-10-19 | 2020-09-08 | 中国科学院过程工程研究所 | Crystalline/amorphous silicon-carbon nanowire and preparation method and application thereof |
US10818969B2 (en) | 2018-09-27 | 2020-10-27 | University Of Maryland, College Park | Borate compounds as Li super-ionic conductor, solid electrolyte, and coating layer for Li metal battery and Li-ion battery |
CN111834613A (en) * | 2019-04-23 | 2020-10-27 | 四川佰思格新能源有限公司 | High-capacity composite negative electrode material, preparation method and lithium ion battery |
CN114497729A (en) * | 2020-11-12 | 2022-05-13 | 山东海科新源材料科技股份有限公司 | Lithium ion battery and electrolyte for lithium ion battery |
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