CN104900916A - Electrolyte solution for high-capacity lithium-ion battery, preparation method and lithium-ion battery - Google Patents
Electrolyte solution for high-capacity lithium-ion battery, preparation method and lithium-ion battery Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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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
- Y02E60/10—Energy storage using batteries
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses an electrolyte solution for a high-capacity lithium-ion battery. The electrolyte solution includes non-aqueous solvent, lithium hexafluorophosphate, negative electrode film forming additive, positive electrode surface activity inhibiting additive and transition metal ion complexant; the negative electrode film forming additive includes organic ester negative electrode film forming additive of 1 to 10wt% of the total electrolyte solution and inorganic lithium salt negative electrode film forming additive of 0.5 to 2wt% of the total electrolyte solution; the positive electrode surface activity inhibiting additive includes fluorinated ether additive of 1 to 5wt% of the total electrolyte solution and nitrile additive of 0.1 to 5wt% of the total electrolyte solution; the transition metal ion complexant is of 0.1 to 1.0wt% of the total electrolyte solution. The electrolyte solution is adaptive to the high-capacity lithium-ion battery and is capable of optimizing the circulating performance and high-temperature storage performance of the lithium-ion battery. The invention further provides a preparation method of the electrolyte solution and the high-capacity lithium-ion battery adopting the electrolyte solution.
Description
Technical field
The present invention relates to electrolyte field, the lithium ion battery of particularly a kind of electrolyte for high-capacity lithium ion cell, and the preparation method of this electrolyte and this electrolyte of employing.
Background technology
Lithium ion battery has been the study hotspots of people at new energy field since coming out from 1999 always.It is high with voltage, capacity is large, memory-less effect and the life-span is long etc. that advantage is widely used in the electronic products such as mobile phone, digital camera and notebook computer.In addition, lithium ion battery also as an alternative the energy storage device of the energy directly apply to electric motor car and hybrid electric vehicle.Along with the development of technology, to lithium battery energy density requirement more and more higher.
In positive electrode the most frequently used at present, when the nickel content in positive electrode is at 70-90%, there is high reversible specific capacity and good cyclical stability, be considered to most possibly substitute LiCoO
2one of positive electrode, and nickel resources enriches, relative low price, so high-nickel material oneself become the study hotspot of anode material for lithium-ion batteries, for the demand of current lithium ion cell high-capacity, the nickelic positive electrode of high gram volume is used to can yet be regarded as a kind of effective means improving capacity of lithium ion battery.
The negative material mainly carbon class material that current business uses, there is cycle performance excellent, the feature that deposit is abundant and cheap, but the capacity of Carbon anode closely its theoretical capacity (372mAh/g), specific capacity potentiality to be exploited is less, and has larger potential safety hazard when over-charging of battery.So develop more high-energy-density negative material become the active demand of current field of lithium ion battery.Wherein silicon-carbon class material receives much concern because it possesses high theoretical capacity, and is more and more used in commercially produced product.
Using high-nickel material as lithium ion cell positive, the specific energy of battery can be promoted significantly using Si-C composite material as negative pole.
High-nickel material be positive pole, Si-C composite material is in the lithium-ion battery system of negative pole, due to the increase of Ni content in high-nickel material, and in charging process, raise with charging voltage, high-nickel material positive electrode surface Ni
3+and Ni
4+content increases, due to Ni
4+there is very strong oxidizability, not only react with electrolyte, destroy the function of electrolyte, and positive electrode may be caused to divide at a lower temperature parse O
2, produce large calorimetric, under hot conditions, electrolyte decomposition produces a large amount of gas, brings safety risks to battery.The stripping of high-nickel material positive pole transition metal ions also can cause the deterioration of battery performance the destruction of the deposition anticathode SEI film of negative pole.Although silicon-carbon composite cathode has higher specific capacity, but because silicon can produce huge bulk effect in removal lithium embedded process, negative terminal surface SEI film constantly destroys and regenerates, silicon grain is because huge stress breaks or efflorescence simultaneously, the active material on silicium cathode is caused to come off, electrical contact between active material and collector is deteriorated, and causes the internal resistance of cell to increase, deterioration of cell properties.
In view of be positive pole at high-nickel material, Si-C composite material is the strong oxidizing property of high-nickel material in the lithium-ion battery system of negative pole, the easy stripping of transition metal ions and silicon-carbon cathode volumetric expansion cause greatly surperficial SEI film unsteadiness, be necessary to provide a kind of electrolyte that can simultaneously mate with nickelic positive pole and silicon-carbon composite cathode.
Summary of the invention
Main purpose of the present invention is to provide a kind of electrolyte for high-capacity lithium ion cell.This electrolyte is applicable to nickelic positive pole and silicon-carbon composite cathode lithium ion battery, improves cycle performance and the high-temperature storage performance of this lithium ion battery, and the present invention simultaneously also provides the preparation method of this electrolyte and adopts the high-capacity lithium ion cell of this electrolyte.
Technical scheme provided by the invention is: a kind of electrolyte for high-capacity lithium ion cell, described electrolyte comprises nonaqueous solvents and lithium hexafluoro phosphate, and described electrolyte also comprises cathode film formation additive, suppresses positive electrode surface active additive and transition metal ions complexing agent;
Wherein, cathode film formation additive is made up of with the inorganic lithium salt cathode film formation additive accounting for electrolyte total amount 0.5 ~ 2wt% the organosilane ester cathode film formation additive accounting for electrolyte total amount 1 ~ 10wt%;
Positive electrode surface active additive is suppressed to be made up of with the nitrile additive accounting for electrolyte total amount 0.1 ~ 5wt% the fluorine ether additive accounting for electrolyte total amount 1 ~ 5wt%;
Described transition metal ions complexing agent accounts for 0.1 ~ 1.0wt% of electrolyte total amount.
In the present invention, wt% is mass percent.
Preferably, cathode film formation additive is made up of with the inorganic lithium salt cathode film formation additive accounting for electrolyte total amount 0.5 ~ 2wt% the organosilane ester cathode film formation additive accounting for electrolyte total amount 1 ~ 5wt%;
Positive electrode surface active additive is suppressed to be made up of with the nitrile additive accounting for electrolyte total amount 1 ~ 2wt% the fluorine ether additive accounting for electrolyte total amount 1 ~ 5wt%;
Described transition metal ions complexing agent accounts for 0.5 ~ 1.0wt% of electrolyte total amount.
Above-mentioned in the electrolyte of high-capacity lithium ion cell, described nitrile additive is succinonitrile, glutaronitrile, adiponitrile, pimelic dinitrile, 1,3,6-hexane three nitrile, 1,2,3-propane three nitrile, one or more in ethylene glycol bis (propionitrile) ether.
Described fluorine ether additive is 1,1,2,2-tetra-fluoro ethyl-2,2,3,3-tetrafluoro propyl ether, 1H, 1H, 5H-octafluoro amyl group-1,1,2,2-tetrafluoro ethylether, 2H-hexafluoro propyl group 2,2,3,3-tetrafluoro ether, methyl fluoride-1,1,1,3,3,3-hexafluoroisopropyl ether, 1,1,2,2-tetrafluoro ethyl diethyldithiocarbamate ether, 1,2-two (1,1,2,2-tetrafluoro ethyoxyl) ethane, one or more in 1,2,2,2-tetra-fluoro ethyl difluoromethyl ether.
Above-mentioned in the electrolyte of high-capacity lithium ion cell, described organosilane ester cathode film formation additive is vinylene carbonate, fluorinated ethylene carbonate, vinylethylene carbonate, propylene sulfite, 1,3-propane sultone, glycol sulfite, ethyl sulfate, methane-disulfonic acid methylene ester, Isosorbide-5-Nitrae-butane sultones, one or more in 4-methylsulfuric acid vinyl acetate;
Described inorganic lithium salt cathode film formation additive is LiBF4, di-oxalate lithium borate, two fluorine Lithium bis (oxalate) borate, two fluorine sulfimide lithium, one or more in two trifluoromethanesulfonimide lithium.
Above-mentioned in the electrolyte of high-capacity lithium ion cell, described transition metal ions complexing agent is 12-crown ether-4,18-crown ether-6,15-crown ether-5,1-azepine-15-crown ether-5, azepine-18-crown ether-6, diaza 18-crown ether-6, two (pyridine-2-methyl) amine, N-(2-pyridylmethyl)-1-propylamine, N-(2-pyridylmethyl)-2-alkene-1-propylamine, N, N, one or more in N ', N '-four (2-picolyl) ethylenediamine, N-(2-pyridylmethyl)-1-butylamine.
Above-mentioned in the electrolyte of high-capacity lithium ion cell, described nonaqueous solvents accounts for 52 ~ 85wt% of electrolyte total amount, and described nonaqueous solvents is the mixture of at least one at least one in ethylene carbonate, propene carbonate and dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, methyl formate, Ethyl formate, methyl acetate, ethyl acetate, propyl acetate, ethyl propionate.
Above-mentioned in the electrolyte of high-capacity lithium ion cell, described lithium hexafluoro phosphate concentration is in the electrolytic solution 1.0 ~ 2.0mol/L.
The invention also discloses the preparation method of the above-mentioned electrolyte for high-capacity lithium ion cell, in argon atmosphere, in nonaqueous solvents, add transition metal ions complexing agent, cathode film formation additive and suppress positive electrode surface active additive, finally add lithium hexafluoro phosphate and mixture is uniformly mixed.
The invention also discloses the lithium ion battery adopting the above-mentioned electrolyte for high-capacity lithium ion cell, described lithium ion battery comprises positive pole, negative pole, electrolyte, barrier film, and the positive active material in the positive pole of described lithium ion battery is LiNi
0.8co
0.1mn
0.1o
2or LiNi
0.8co
0.15al
0.05o
2.As the design that this area is conventional, lithium ion battery also comprises battery case etc., to form a complete lithium ion battery.
In above-mentioned lithium ion battery, the negative electrode active material in the negative pole of described lithium ion battery is silicon-carbon cathode composite material, and in Si-C composite material, total Si mass percent is less than 12%.
The maximum operating voltage of lithium ion battery of the present invention is 4.2V-4.5V.
Beneficial effect of the present invention is as follows:
1, the present invention passes through the conbined usage of fluorine ether additive and nitrile additive, forms interfacial film at high-nickel material positive electrode surface Preferential adsorption, stops direct contact of electrolyte and nickelic positive electrode surface Ni active site, suppresses electrolyte at positive polar decomghtion.
2, the present invention passes through the conbined usage of organosilane ester cathode film formation additive and inorganic lithium salt cathode film formation additive, the skin covering of the surface that shrinkage is good, resistance to elevated temperatures is good is formed on silicon-carbon cathode surface, improve negative material structural stability, improve the electrical contact performance between active material and collector, improve the stability of the internal resistance of cell, alleviate deterioration of cell properties.
3, the present invention uses complexing of metal ion agent simultaneously, by the transition metal ions complexing of nickelic positive electrode stripping in the electrolytic solution, and be not deposited on negative pole, in case anticathode SEI film damages, stablize negative terminal surface SEI film further, transition metal ions stripping in high-nickel material is suppressed the destruction of the deposition anticathode SEI film of negative pole, to improve battery performance.
Comprehensive, the present invention reduces the adverse effect because the oxidizability of nickelic positive pole, Si-C composite material Volumetric expansion and the stripping of positive pole transition metal ions cause battery by the mode adopting the stability that improves both positive and negative polarity skin covering of the surface and complexed transition metal ion and do not act at cathode deposition simultaneously.In utilize the electrolyte of mentality of designing of the present invention to be applied in high-nickel material is positive pole, Si-C composite material is negative pole lithium ion battery, ensure that battery has good cycle performance and high-temperature storage performance.
Accompanying drawing explanation
Fig. 1 is the test result figure of embodiments of the invention 1, comparative example 1, comparative example 2;
Fig. 2 is the test result figure of embodiments of the invention 2, comparative example 3, comparative example 4;
Fig. 3 is the test result figure of embodiments of the invention 3, comparative example 5;
Fig. 4 is the test result figure of embodiments of the invention 4, comparative example 6;
Fig. 5 is the test result figure of embodiments of the invention 5, comparative example 7;
Fig. 6 is the test result figure of embodiments of the invention 6, embodiment 7, embodiment 8;
Fig. 7 is embodiments of the invention 9, embodiment 10, the test result figure of embodiment 11.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in further detail, but does not form any limitation of the invention.
Embodiment 1
Battery makes:
Prepared by positive pole: positive electrode proportioning is: LiNi
0.8co
0.15al
0.05o
2(lithium nickel cobalt alumina), acetylene black (conductive agent), polyvinylidene fluoride (PVDF, binding agent) mass ratio is 95:2.5:2.5.PVDF is joined in N-methyl-pyrrolidon (NMP), high-speed stirred is even, acetylene black is added in solution, stir, then add lithium nickel cobalt alumina and to stir formation anode sizing agent, by anode sizing agent coating with on aluminium foil, positive plate is toasted, compacting, cut-parts, welding electrode ear.
Prepared by negative pole: negative material proportioning is Si-C composite material, acetylene black, carboxymethyl cellulose (CMC), fourth third rubber (SBR), mass ratio 95:1.0:1.5:2.5.Be added to the water by CMC, high-speed stirred makes it dissolve completely, then adds acetylene black, continue to be stirred to evenly, continue to add Si-C composite material (Si content is 5%) powder, stir after dispersion, add SBR, be dispersed into uniform cathode size, by cathode size coating with on Copper Foil, negative plate is toasted, compacting, cut-parts, welding electrode ear.
Prepared by electrolyte: (moisture < 10ppm in the glove box being full of argon gas, oxygen divides < 1ppm), get the ethylene carbonate accounting for gross mass 77.5%, dimethyl carbonate, methyl ethyl carbonate mixed liquor, ethylene carbonate, dimethyl carbonate, methyl ethyl carbonate mass ratio is 1:1:1, additive vinylene carbonate is added successively in mixed liquor, two fluorine Lithium bis (oxalate) borate, 1, 3, 6-hexane three nitrile, 1, 1, 2, 2-tetra-fluoro ethyl-2, 2, 3, 3-tetrafluoro propyl ether, 12-crown ether-4, addition accounts for 1.0% of gross mass respectively, 1.0%, 1.0%, 5.0%, 0.5%.Slowly add the lithium hexafluoro phosphate accounting for gross mass 14.0% (about 1.12mol/L) in the most backward mixed liquor, after stirring, obtain the electrolyte A1 of embodiment 1.
The preparation of battery: by the positive plate obtained, negative plate, polyethylene diagrams is wound into battery core in order, and load in cylindrical battery shell, above-mentioned electrolyte is injected battery, 18650 type cylindrical batteries are made in sealing.Obtain sample lithium ion battery S1.
Embodiment 2
Embodiment 1 electrolyte method is adopted to prepare electrolyte A2, be fluorinated ethylene carbonate, LiBF4, succinonitrile, 1H unlike the additive added, 1H, 5H-octafluoro amyl group-1,1,2,2-tetrafluoro ethylether, 18-crown ether-6, addition accounts for 4.0%, 0.5%, 2.0%, 4.0%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare S2 according to the method for embodiment 1.
Embodiment 3
Embodiment 1 electrolyte method is adopted to prepare electrolyte A3, be fluorinated ethylene carbonate, di-oxalate lithium borate, oneself two eyeballs, 2H-hexafluoro propyl group 2 unlike the additive added, 2,3,3-tetrafluoro ether, 1-azepine-15-crown ether-5, addition accounts for 5.0%, 1.0%, 1.0%, 2.0%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare S3 according to the method for embodiment 1.
Embodiment 4
Embodiment 1 electrolyte method is adopted to prepare electrolyte A4, be 1 unlike the additive added, 3-propane sultone, two fluorine sulfimide lithium, heptan two eyeball, 1,2,2,2-tetra-fluoro ethyl difluoromethyl ether, azepine-18-crown ether-6, addition accounts for 2.0%, 1.0%, 2.0%, 3.0%, 1.0% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare S4 according to the method for embodiment 1.
Embodiment 5
Embodiment 1 electrolyte method is adopted to prepare electrolyte A5, be methane-disulfonic acid methylene ester, two trifluoromethanesulfonimide lithium, 1 unlike the additive added, 2,3-propane three nitrile, 1,1,2,2-tetrafluoro ethyl diethyldithiocarbamate ether, diaza 18-crown ether-6, addition accounts for 1.0%, 2.0%, 1.0%, 3.0%, 1.0% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare S5 according to the method for embodiment 1.
Embodiment 6
Adopt embodiment 1 electrolyte method to prepare electrolyte A6, be ethylene carbonate, dimethyl carbonate, methyl ethyl carbonate, ethyl acetate unlike nonaqueous solvents, mass ratio is 2:1:2:1.Additive is glycol sulfite, di-oxalate lithium borate, 1,3,6-hexane three nitrile, 1H, 1H, 5H-octafluoro amyl group-1,1,2,2-tetrafluoro ethylether, N-(2-pyridylmethyl)-1-propylamine, addition accounts for 1.5%, 1.0%, 1.0%, 4.0%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 15.0% (about 1.20mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare S6 according to the method for embodiment 1.
Embodiment 7
Adopt embodiment 1 electrolyte method to prepare electrolyte A7, be ethylene carbonate, dimethyl carbonate, methyl ethyl carbonate, ethyl acetate unlike nonaqueous solvents, mass ratio is 1:1:1:1.Additive is fluorinated ethylene carbonate, two fluorine sulfimide lithium, succinonitrile, 1,1,2,2-tetra-fluoro ethyl-2,2,3,3-tetra-fluoropropyl ether, azepine-18-crown ether-6, and addition accounts for 4.0%, 1.5%, 2.0%, 3.0%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 15.0% (about 1.20mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare S7 according to the method for embodiment 1.
Embodiment 8
Adopt embodiment 1 electrolyte method to prepare electrolyte A8, be ethylene carbonate, propene carbonate, dimethyl carbonate, methyl ethyl carbonate unlike nonaqueous solvents, mass ratio is 3:2:9:9.Additive is vinylethylene carbonate, LiBF4, adiponitrile, 1,1,2,2-tetrafluoro ethyl diethyldithiocarbamate ether, 15-crown ether-5, and addition accounts for 2.0%, 1.0%, 2.0%, 3.0%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 16.0% (about 1.28mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare S8 according to the method for embodiment 1.
Embodiment 9
Embodiment 1 electrolyte method is adopted to prepare electrolyte A9, be 1 unlike additive, 4-butane sultones, two trifluoromethayl sulfonic acid imine lithium, ethylene glycol bis (propionitrile ether), 1,2,2,2-tetra-fluoro ethyl difluoromethyl ether, N-(2-pyridylmethyl)-1-butylamine, addition accounts for 1.5%, 1.5%, 2.0%, 3.5%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 16.0% (about 1.28mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Adopt above-mentioned electrolyte to prepare S9 according to the method for embodiment 1, prepare used positive electrode for LiNi unlike battery
0.8co
0.1mn
0.1o
2(lithium nickel cobalt manganese oxygen).
Embodiment 10
Adopt embodiment 1 electrolyte method to prepare electrolyte A10, be ethylene carbonate, dimethyl carbonate, diethyl carbonate unlike nonaqueous solvents, mass ratio is 2:2:1.Additive is fluorinated ethylene carbonate, LiBF4, adiponitrile, 1,2,2,2-tetra-fluoro ethyl difluoromethyl ether, 1-azepine-15-crown ether-5, and addition accounts for 8%, 0.5%, 4.0%, 1%, 0.2% of gross mass respectively; Lithium hexafluoro phosphate accounts for electrolyte gross mass 23% (about 1.84mol/L); Remaining component is nonaqueous solvents.
Adopt above-mentioned electrolyte to prepare S10 according to the method for embodiment 1, prepare used negative material for Si-C composite material (Si content is 8%) unlike battery.
Embodiment 11
Adopt embodiment 1 electrolyte method to prepare electrolyte A11, be ethylene carbonate, dimethyl carbonate, ethyl acetate unlike nonaqueous solvents, mass ratio is 2:2:1.Additive is fluorinated ethylene carbonate, di-oxalate lithium borate, 1,3,6-hexane three nitrile, 1,1,2,2-tetrafluoro ethyl diethyldithiocarbamate ether, N-(2-pyridylmethyl)-1-propylamine, addition accounts for 6%, 0.5%, 4.0%, 2%, 0.2% of gross mass respectively; Lithium hexafluoro phosphate accounts for electrolyte gross mass 18.5% (about 1.48mol/L); Remaining component is nonaqueous solvents.
Adopt above-mentioned electrolyte to prepare S11 according to the method for embodiment 1, prepare unlike battery and used prepare used positive electrode for LiNi unlike battery
0.8co
0.1mn
0.1o
2(lithium nickel cobalt manganese oxygen), negative material is Si-C composite material (Si content is 8%).
Comparative example 1
Embodiment 1 electrolyte method is adopted to prepare electrolyte DA1-1, be two fluorine Lithium bis (oxalate) borates, 1 unlike additive, 3,6-hexane three nitrile, 1,1,2,2-tetra-fluoro ethyl-2,2,3,3-tetrafluoro propyl ether, 12-crown ether-4, addition accounts for 1.0%, 1.0%, 5.0%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare DS1-1 according to the method for embodiment 1.
Comparative example 2
Embodiment 1 electrolyte method is adopted to prepare electrolyte DA1-2, be vinylene carbonate, 1 unlike the additive added, 3,6-hexane three nitrile, 1,1,2,2-tetra-fluoro ethyl-2,2,3,3-tetrafluoro propyl ether, 12-crown ether-4, addition accounts for 1.0%, 1.0%, 5.0%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare DS1-2 according to the method for embodiment 1
Comparative example 3
Embodiment 1 electrolyte method is adopted to prepare electrolyte DA2-1, be fluorinated ethylene carbonate, LiBF4,1H unlike the additive added, 1H, 5H-octafluoro amyl group-1,1,2,2-tetrafluoro ethylether, 18-crown ether-6, addition accounts for 4.0%, 0.5%, 4.0%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare DS2-1 according to the method for embodiment 1.
Comparative example 4
Adopt embodiment 1 electrolyte method to prepare electrolyte DA2-2, be fluorinated ethylene carbonate, LiBF4, succinonitrile, 18-crown ether-6 unlike the additive added, addition accounts for 4.0%, 0.5%, 2.0%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare DS2-2 according to the method for embodiment 1.
Comparative example 5
Adopt embodiment 1 electrolyte method to prepare electrolyte DA3, be fluorinated ethylene carbonate, di-oxalate lithium borate, 1-azepine-15-crown ether-5 unlike the additive added, addition accounts for 5.0%, 1.0%, 0.5% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare DS3 according to the method for embodiment 1.
Comparative example 6
Adopt embodiment 1 electrolyte method to prepare electrolyte DA4, unlike the additive added be heptan two eyeball, 1,2,2,2-tetra-fluoro ethyl difluoromethyl ether, azepine-18-crown ether-6, addition accounts for 2.0%, 3.0%, 1.0% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare DS4 according to the method for embodiment 1.
Comparative example 7
Embodiment 1 electrolyte method is adopted to prepare electrolyte DA5, be methane-disulfonic acid methylene ester, two trifluoromethanesulfonimide lithium, 1 unlike the additive added, 2,3-propane three nitrile, 1,1,2,2-tetrafluoro ethyl diethyldithiocarbamate ether, addition accounts for 1.0%, 2.0%, 1.0%, 3.0% of gross mass respectively.Wherein lithium hexafluoro phosphate accounts for 14.0% (about 1.12mol/L) of electrolyte gross mass, and remaining component is nonaqueous solvents.
Above-mentioned electrolyte is adopted to prepare DS5 according to the method for embodiment 1.
Test experiments
All comparative examples 1 ~ 7 and all embodiments 1 ~ 11 gained battery are tested as follows:
Normal temperature circulation experiment: comparative example 1 ~ 7 and embodiment 1 ~ 11 gained battery are at room temperature carried out charge and discharge cycles test with the charge-discharge magnification of 0.5C/0.5C within the scope of 3.0 ~ 4.35V, record every 10 cyclic discharge capacities, record result is as Fig. 1,2,3,4,5,6,7.
High temperature storage is tested: by the battery of comparative example 1 ~ 7 and embodiment 1 ~ 11 first at room temperature with the charge-discharge magnification of 0.5C/0.5C 3.0 ~ 4.35V discharge and recharge 3 times, then charge to 4.35V with 0.5C, record the 3rd discharge capacity.Battery is placed in 60 DEG C of baking ovens and stores 15 days, treat that battery is cooled to room temperature, more at room temperature with the charge-discharge magnification of 0.5C/0.5C 3.0 ~ 4.35V discharge and recharge 3 times, record the 1st discharge capacity and 3 times discharge in discharge capacity once the highest.Namely obtain capability retention with the 1st discharge capacity after storing divided by front 3rd discharge capacity of storage, with store discharge capacity in rear 3 electric discharges the highest once namely obtain capacity restoration rate divided by storing front 3rd discharge capacity, outcome record is as table 1.
Table 1: capacity of lithium ion battery conservation rate, capacity restoration rate test result
| Sample group | Capability retention after high temperature storage | Capacity restoration rate after high temperature storage |
| DS1-1 | 90.3％ | 96.3％ |
| DS1-2 | 89.4％ | 95.7％ |
| S1 | 91.5％ | 96.9％ |
| DS2-1 | 80.5％ | 88.4％ |
| DS2-2 | 85.3％ | 89.5％ |
| S2 | 92.4％ | 96.7％ |
| DS3 | 80.2％ | 85.7％ |
| S3 | 90.2％ | 94.8％ |
| DS4 | 85.0％ | 91.2％ |
| S4 | 88.0％ | 92.0％ |
| DS5 | 84.5％ | 89.5％ |
| S5 | 89.7％ | 93.4％ |
| S6 | 88.7％ | 94.5％ |
| S7 | 91.4％ | 96.7％ |
| S8 | 92.8％ | 97.9％ |
| S9 | 89.9％ | 95.7％ |
| S10 | 90.1％ | 96.5％ |
| S11 | 88.4％ | 93.1％ |
Composition graphs 1 and the display of table 1 result: SD1-1, SD1-2 and S1 contrast, interpolation organosilane ester cathode film formation additive and inorganic lithium salt cathode film formation additive are relative to only adding organosilane ester additive or inorganic lithium additive salt simultaneously, cycle performance of battery significantly improves, and illustrates that the synergy between organosilane ester additive and inorganic lithium salt additive can improve cycle performance of battery better at cathode film formation.
Composition graphs 2 and the display of table 1 result: SD2-1, SD2-2 and S2 contrast, add nitrile and fluorine ethers suppresses positive-active additive relative to a wherein class in both simultaneously, cycle performance of battery and high-temperature storage performance significantly improve, illustrate that the synergy between fluorine ether additive and nitrile additive can suppress positive electrode surface active better, reduce the oxidation activity of electrolyte, improve battery performance.
Composition graphs 3 and the display of table 1 result: contrast SD3 and S3, do not add and suppress the active nitrile additive of positive electrode surface and fluorine ether additive, cycle performance and high temperature storage poor, the direct contact not having anode additive to be preferentially adsorbed on positive electrode surface to suppress electrolyte and positive electrode Ni active site is described, cycle performance of battery and high-temperature storage performance poor.
Composition graphs 4 and the display of table 1 result: contrast SD4 and S4, do not add the battery of cathode film formation additive, cycle performance and high temperature storage are obviously very poor, and illustrate and do not have cathode film formation additive to participate in forming stable negative terminal surface film, cycle performance of battery and high-temperature storage performance are all very poor.。
Composition graphs 5 and the display of table 1 result: contrast SD5 and S5, the cycle performance of battery and the high-temperature storage performance that with the addition of complexing of metal ion agent significantly improve, what complexing of metal ion agent was described adds the deposition that positive pole stripping metal ion can be suppressed at negative pole, suppress the destruction of negative terminal surface film, and then improve battery performance.
Fig. 6, Fig. 7 and the display of table 1 result: S6, S7, S8, S9, S10, S11 with the addition of organosilane ester cathode film formation additive, inorganic lithium salt cathode film formation additive simultaneously, suppress nitrile additive and the fluorine ether additive of positive-active, transition metal ions complexing agent, all shows good cycle performance and high-temperature storage performance.
Can be learnt by above-mentioned analysis, organosilane ester cathode film formation additive, inorganic lithium salt cathode film formation additive in electrolyte of the present invention, suppress nitrile additive and the fluorine ether additive of positive-active, transition metal ions complexing agent is indispensable, mutually work in coordination with between five additive components, be an organic whole, it effectively raises lithium ion battery particularly containing cycle performance and the high-temperature storage performance of the lithium ion battery of nickelic positive pole, Si-C composite material negative pole.
Above-describedly be only preferred embodiment of the present invention, all do within the scope of the spirit and principles in the present invention any amendment, equivalently to replace and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the electrolyte for high-capacity lithium ion cell, described electrolyte comprises nonaqueous solvents and lithium hexafluoro phosphate, it is characterized in that: described electrolyte also comprises cathode film formation additive, suppresses positive electrode surface active additive and transition metal ions complexing agent;
Wherein, cathode film formation additive is made up of with the inorganic lithium salt cathode film formation additive accounting for electrolyte total amount 0.5 ~ 2wt% the organosilane ester cathode film formation additive accounting for electrolyte total amount 1 ~ 10wt%;
Positive electrode surface active additive is suppressed to be made up of with the nitrile additive accounting for electrolyte total amount 0.1 ~ 5wt% the fluorine ether additive accounting for electrolyte total amount 1 ~ 5wt%;
Described transition metal ions complexing agent accounts for 0.1 ~ 1.0wt% of electrolyte total amount.
2. the electrolyte for high-capacity lithium ion cell according to claim 1, is characterized in that:
Described fluorine ether additive is 1,1,2,2-tetra-fluoro ethyl-2,2,3,3-tetrafluoro propyl ether, 1H, 1H, 5H-octafluoro amyl group-1,1,2,2-tetrafluoro ethylether, 2H-hexafluoro propyl group 2,2,3,3-tetrafluoro ether, methyl fluoride-1,1,1,3,3,3-hexafluoroisopropyl ether, 1,1,2,2-tetrafluoro ethyl diethyldithiocarbamate ether, 1,2-two (1,1,2,2-tetrafluoro ethyoxyl) ethane, one or more in 1,2,2,2-tetra-fluoro ethyl difluoromethyl ether.
3. the electrolyte for high-capacity lithium ion cell according to claim 2, is characterized in that: described nitrile additive is succinonitrile, glutaronitrile, adiponitrile, pimelic dinitrile, 1,3,6-hexane three nitrile, 1,2,3-propane three nitrile, one or more in ethylene glycol bis (propionitrile) ether.
4. the electrolyte for high-capacity lithium ion cell according to claim 1, it is characterized in that: described organosilane ester cathode film formation additive is vinylene carbonate, fluorinated ethylene carbonate, vinylethylene carbonate, propylene sulfite, 1,3-propane sultone, glycol sulfite, ethyl sulfate, methane-disulfonic acid methylene ester, Isosorbide-5-Nitrae-butane sultones, one or more in 4-methylsulfuric acid vinyl acetate;
Described inorganic lithium salt cathode film formation additive is LiBF4, di-oxalate lithium borate, two fluorine Lithium bis (oxalate) borate, two fluorine sulfimide lithium, one or more in two trifluoromethanesulfonimide lithium.
5. the electrolyte for high-capacity lithium ion cell according to claim 1, it is characterized in that: described transition metal ions complexing agent is 12-crown ether-4,18-crown ether-6,15-crown ether-5,1-azepine-15-crown ether-5, azepine-18-crown ether-6, diaza 18-crown ether-6, two (pyridine-2-methyl) amine, N-(2-pyridylmethyl)-1-propylamine, N-(2-pyridylmethyl)-2-alkene-1-propylamine, N, N, one or more in N ', N '-four (2-picolyl) ethylenediamine, N-(2-pyridylmethyl)-1-butylamine.
6. according to the arbitrary described electrolyte for high-capacity lithium ion cell of claim 1 to 5, it is characterized in that: described nonaqueous solvents accounts for 52 ~ 85wt% of electrolyte total amount, described nonaqueous solvents is the mixture of at least one at least one in ethylene carbonate, propene carbonate and dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, methyl formate, Ethyl formate, methyl acetate, ethyl acetate, propyl acetate, ethyl propionate.
7. the electrolyte for high-capacity lithium ion cell according to claim 6, is characterized in that: described lithium hexafluoro phosphate concentration is in the electrolytic solution 1.0 ~ 2.0mol/L.
8. one kind as arbitrary in claim 1 to 7 as described in the preparation method of the electrolyte for high-capacity lithium ion cell, it is characterized in that: in argon atmosphere, in nonaqueous solvents, add transition metal ions complexing agent, cathode film formation additive and suppress positive electrode surface active additive, finally add lithium hexafluoro phosphate and mixture is uniformly mixed.
9. adopt as arbitrary in claim 1 to 7 as described in the lithium ion battery of electrolyte, described lithium ion battery comprises positive pole, negative pole, electrolyte, barrier film, it is characterized in that: the positive active material in the positive pole of described lithium ion battery is LiNi
0.8co
0.1mn
0.1o
2or LiNi
0.8co
0.15al
0.05o
2.
10. lithium ion battery according to claim 9, is characterized in that: the negative electrode active material in the negative pole of described lithium ion battery is Si-C composite material, and in Si-C composite material, total Si mass percent is less than 12%.
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