CN108321434A - A kind of high-voltage lithium-ion battery electrolyte - Google Patents
A kind of high-voltage lithium-ion battery electrolyte Download PDFInfo
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- CN108321434A CN108321434A CN201810246177.8A CN201810246177A CN108321434A CN 108321434 A CN108321434 A CN 108321434A CN 201810246177 A CN201810246177 A CN 201810246177A CN 108321434 A CN108321434 A CN 108321434A
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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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
Abstract
The present invention relates to a kind of high-voltage lithium ion electrolyte, and in particular to it is a kind of containing fluorinated ethylene carbonate, two nitrile of fluoro and flurosulphonic acid lactone compound high-voltage lithium ion electrolyte and using the electrolyte lithium ion battery.The high-voltage lithium ion electrolyte is made of electrolyte lithium salt, non-aqueous organic solvent and additive.The additive includes fluorinated ethylene carbonate, fluoro dinitrile compound and flurosulphonic acid lactone compound, the fluorinated ethylene carbonate can form finer and close SEI films, the cycle performance of battery can be significantly improved, the fluoro dinitrile compound can both stablize the structure of positive electrode, can also reduce electrolysis fluid viscosity.The flurosulphonic acid lactone compound, can both form a film on cathode, while can improve the viscosity of sultone compounds, increase the wellability of electrolyte.The synergistic effect of these three additives can improve high-voltage battery cycle performance and high-temperature storage performance.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of high-voltage lithium ion electrolyte.
Background technology
With popularizing for the electronic digitals product such as multifunction smart mobile phone, tablet computer, consumer is to lithium ion battery
Energy density require it is higher and higher.Commercialization 4.4V lithium ion batteries energy density maximum is also just in 700Wh/L or so at present,
It is still difficult to meet the requirements of consumers.There are mainly two types of modes for the energy density of promotion battery at present：First, selection high power capacity
With high-pressure solid positive and negative pole material；Second is that improving the operating voltage of battery, that is, use high-voltage anode material.And use high power capacity just
Pole material or high-voltage anode material are the most effective approach for promoting lithium ion battery energy density.However in same voltage conditions
Under, the capacity of positive electrode and compacting have promoted the state for comparing the limit.So everybody approach promotion energy density
It all focuses in the charging voltage for promoting positive electrode.
But raising simply, while positive electrode charging voltage, the dissolution of cathode metal ion can increase, electrolyte
Oxygenolysis phenomenon can aggravate, so that battery performance can be caused to become very poor.Especially under prolonged high temperature storage, just
The dissolution of pole metal ion can aggravate.This seriously constrains the application of high-voltage anode material.Although positive electrode business men is also transported
Improve the stability of cathode material structure with various be mixed with, but if being applied using current commercialized electrolyte
It cannot still be solved in high voltage (such as 4.4V or more) positive electrode system under the oxygenolysis and high temperature storage of electrolyte just
The dissolution of pole metal ion.Therefore develop it is a be used for 4.4V and the above high-voltage lithium ion electrolyte, solve electrode with electricity
The electrolyte for solving the compatibility at liquid interface, high temperature storage and good cycle has more great meaning.
Studies have shown that fluorinated ethylene carbonate has good filming performance and oxidation resistent susceptibility, it can effectively improve electricity
Pond cycle performance.But easily decompose at high temperature, it may appear that serious flatulence phenomenon.Method commonplace at present is in the electrolytic solution
Add nitrile and sultone compounds.However common nitrile and sultone compounds addition lacked can not have it is apparent
Effect, additive amount is more, can influence the interface interaction of the conductivity and electrode and electrolyte of electrolyte.
Invention content
In order to solve the above technical problems, the present invention provides one kind containing fluorinated ethylene carbonate, two nitrile of fluoro and fluorine
The lithium ion battery of electrolyte for sultone compounds combination and the 4.4V or more using the electrolyte, to improve height
Voltage battery high temperature storage and cycle performance.
To achieve the above object, technical solution provided by the invention is：A kind of lithium ion battery high-voltage electrolyte, packet
Include non-aqueous organic solvent, electrolyte lithium salt and functional electrolysis additive, which is characterized in that the functionality electrolyte addition
Agent includes fluorinated ethylene carbonate, fluoro dinitrile compound and at least one flurosulphonic acid lactone compound as shown in structural formula I
Object：
Wherein, n is respectively the integer of 0-3.
The non-aqueous organic solvent accounts for the 25-80% of solvent gross mass；
The LiPF6 of a concentration of 1.1-1.6mol/L of electrolyte lithium salt；
The fluorinated ethylene carbonate accounts for the 1-10% of solvent gross mass；
Two nitrile compounds of the fluoro account for the 0.5-8% of solvent gross mass；
The flurosulphonic acid lactone compound accounts for the 0.1-8% of solvent gross mass；
The non-aqueous organic solvent is carboxylate, alpha-fluorocarboxylate ester or carbonic ester.
The carboxylate is selected from one or more of propyl acetate, propyl propionate, ethyl propionate, ethyl butyrate；It is described
Alpha-fluorocarboxylate ester is selected from one or more of difluoroacetic acid propyl ester, trifluoroacetic acid propyl ester, hyptafluorobutyric acid ethyl ester.
The carbonic ester be selected from ethylene carbonate, propylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate,
One or more of dipropyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, ethyl propyl carbonic acid ester.
The electrolyte lithium salt is lithium hexafluoro phosphate, LiBF4, difluorophosphate, double fluorine Lithium bis (oxalate) borates, two
One or more of (trimethyl fluoride sulfonyl) imine lithium, imidodisulfuryl fluoride lithium salt.
The flurosulphonic acid lactone compound as shown in structural formula I is 1,2,3- tri- fluoro- 1,3-propane sultone, 1,3-
Any one of two fluoro- 2- methyl fluorides -1,3-propane sultone, 1,3-, bis- fluoro- 2- fluoro ethyls -1,3-propane sultone.
Remaining described additive further includes sulfuric acid vinyl ester, ethylene sulfite, propylene sulfite, ethylene carbonate Asia second
Ester it is one or more, these additives each account for solvent gross mass 0.1-3% in the electrolytic solution.
A kind of high-voltage lithium ion batteries, including anode, cathode, diaphragm and above-described contain fluoro ethylene carbonate
The high-voltage electrolyte of ester, fluoro two nitriles and flurosulphonic acid lactone, it is described anode used by active material configuration formula be
LiCoxM1-xO2, wherein M Al, Sr, Mg, Ti, Ca, Zr, Si or Fe, 0 x≤1 ＜, the lithium ion battery charge cutoff voltage
It is less than 4.5V more than or equal to 4.4V.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) in the present invention one of additive fluorinated ethylene carbonate, fine and close flexible and low-resistance can be formed in negative terminal surface
Anti- SEI films, while fluorinated ethylene carbonate can reduce electrolyte surface tension and increase electrolyte under high voltages resistance to
The high-voltage battery of oxidation susceptibility, preparation has excellent cycle performance.
(2) present invention in additive two two nitrile compounds of fluoro, itrile group functional group-CN can be with positive-active material
Complexing occurs for the transition metal ion in material, reduces electrolyte and is catalytically decomposed and inhibits digestion of metallic ion, stablizes high electricity
Press the crystal structure of positive electrode.The fluorine functional group of institute's band can also reduce surface tension simultaneously, increase electrode and electrolyte interface
Compatibility, the high-voltage battery of preparation has excellent high temperature storage and cycle performance.
(3) present invention in additive three flurosulphonic acid lactone compound, sultones is in lithium-ion battery electrolytes
As common film for additive, it can significantly improve the service life of lithium secondary battery, but it is low with conductivity, viscosity is big
Disadvantage, if after two addition fluorine functional groups, the interface impedance of electrolyte and electrode, the height of making can also be reduced by neither influencing film forming
Voltage lithium ion battery has excellent cycle and high-temperature storage performance.
Specific implementation mode
With reference to specific embodiment, the invention will be further described, but is not to be construed as to the scope of the present invention
Restriction.
High-voltage lithium-ion battery electrolyte includes following component：Non-aqueous organic solvent, electrolyte matter lithium salts, fluoro carbonic acid
Vinyl acetate, two nitrile of fluoro, flurosulphonic acid lactone and remaining additive.Wherein, non-aqueous organic solvent accounts for the 25- of solvent gross mass
80%；The LiPF6 of a concentration of 1.1-1.6mol/L of electrolyte lithium salt；Fluorinated ethylene carbonate accounts for the 1-10% of solvent gross mass；
Two nitrile compounds of fluoro account for the 0.5-8% of solvent gross mass；Flurosulphonic acid lactone compound accounts for the 0.1- of solvent gross mass
8%；
Remaining described additive further includes sulfuric acid vinyl ester, ethylene sulfite, propylene sulfite, ethylene carbonate Asia second
Ester it is one or more, these additives each account for solvent gross mass 0.1-3% in the electrolytic solution.
Embodiment 1
Prepare electrolyte step：In the glove box full of argon gas, by ethylene carbonate, propene carbonate, propyl propionate
In mass ratio 2:1:3 are mixed, be then slowly added into mixed solution a concentration of 1.2mol/L lithium hexafluoro phosphate and
Double fluorine sulfimide lithiums of 0.1mol/L are eventually adding fluorinated ethylene carbonate, 4%2- fluorine based on electrolyte gross mass 4%
For adiponitrile, 3%1,2,3- tri- fluoro- 1,3-propane sultone and 0.5% vinylethylene carbonate are implemented after stirring evenly
The high-voltage lithium-ion battery electrolyte of example 1
The preparation process of positive plate：In nmp solvent by weight by LiCoO2 and conductive agent (carbon black), bonding agent (PVDF)
Than 98:1:1 weight ratio is uniformly mixed, and anode sizing agent is made in vacuum stirring；By slurry even application on 10 μm of aluminium foil, system
Standby pole piece；Pole piece is dried under 130 DEG C of environment, and positive plate is made through roll-in slitting.
The preparation process of negative plate：By graphite and conductive agent (carbon black), thickener (CMC), bonding agent in H2O solvents
(SBR) by weight 96:1:1:2 ratio is uniformly mixed, and negative electrode slurry is made in vacuum stirring；By slurry even application at 8 μm
Copper foil on, prepare pole piece；Pole piece is dried under 120 DEG C of environment, and negative plate is made through roll-in slitting.
The preparation process of battery：The polyethylene that positive plate, negative plate and the thickness that the above method is prepared are 12 μm
Diaphragm, which stacks gradually, is wound into a rectangular core, and (material is plastic-aluminum by core loading polymer soft-package battery shell
Film), then vacuum bakeout injects the electrolyte of above-mentioned preparation, and through standing, being melted into after encapsulation, degasification obtains after aging and partial volume
Polymer soft bag lithium ionic cell.
Electrochemical property test：
1) 0.7C recycles discharge test：At 25 DEG C, the battery after chemical conversion is charged to 4.45V by 0.7C constant current constant voltages, is cut
Only electric current 0.02C, after then shelving 10min, by 0.7C constant-current discharges to 3.0V.Charge-discharge cycle calculates the 500th cycle after 500 weeks
Circulation volume conservation rate.Calculation formula is as follows：
500th week circulation volume conservation rate (%)=(the 500th week cyclic discharge capacity/store warm up discharge capacity for the first time) *
100%；
2) 85 DEG C/4h of the full electric states of 4.45V storage tests：The battery after chemical conversion is charged to 4.45V by 0.5C at room temperature, is ended
Electric current 0.02C, after shelving 10min, 0.5C is put to 3.0V, records initial capacity D1, then be charged to 4.45V with 0.5C constant current constant voltages,
Cut-off current 0.02C tests thickness T1, voltage and the internal resistance of battery；The battery of full electric state is placed in 85 DEG C of insulating boxs and is stored
4h measures the hot thickness of battery and is denoted as T2, tests cold thickness T3, voltage and the internal resistance of battery after normal temperature shelf 2h, then put by 0.5C
It is recorded to 3.0V and keeps capacity D2, shelved and be charged to 4.45V with 0.5C constant current constant voltages after 10min, cut-off current 0.02C is shelved
After 10min, put to 3.0V with 0.5C, record restores capacity D3.
Battery coefficient of thermal expansion (%)=(T2-T1)/T1*100%；
Battery capacity conservation rate (%)=D2/D1*100%；
Capacity resuming rate (%)=D3/D1*100%.
In embodiment 2-9, other than each component content of electrolyte is by addition shown in table 1, remaining is same as Example 1.
Table 1 is each component content table of electrolyte and electric performance test result of embodiment 1-9：
Table 1：
In above-mentioned table 1, it is as follows that each chemical substance letter writes a Chinese character in simplified form corresponding title：
EC (ethylene carbonate), DEC (diethyl carbonate), PP (propyl propionate), LiFSi (double fluorine sulfimide lithiums),
LiPF6 (lithium hexafluoro phosphate), FEC (fluorinated ethylene carbonate), VEC (vinylethylene carbonate).
Known to comparative example 1 and 4：The room temperature 0.7C cycles of the less fluorine-containing sultones of sultones containing fluoro are held
Amount conservation rate wants slightly worse, and cell expansion is slightly smaller after 85 DEG C of storage 4h, and capacity is kept and response rate is slightly larger.Fluorine i.e. of the present invention
Having for sultones improves the cycle and high-temperature storage performance of high-voltage battery.
Comparative example 1-3 it is found that with flurosulphonic acid lactone content increase, 85 degree of 4h storage performances improve, room temperature
The variation of 0.7C circulation volume conservation rates is little.Interface impedance shadow of the flurosulphonic acid lactone i.e. of the present invention to electrolyte and electrode
Sound is smaller.
Comparative example 1 and 5 is it is found that fluorinated ethylene carbonate can promote room temperature 0.7C circulation volume conservation rates, but 85 degree
4h storage performances reduce.Fluorinated ethylene carbonate i.e. of the present invention can be effectively improved the cycle performance of high-voltage battery, but energy
Reduce by 85 degree of storage performances.
Comparative example 1 it is found that fluoro two nitriles pair, 85 degree of 4h storage performances are helpful, not too much influences room temperature with 6
0.7C circulation volume conservation rates.Two nitrile compounds of fluoro i.e. of the present invention on the interface impedance of electrolyte and electrode influence compared with
It is small.
In conclusion the present invention passes through fluorinated ethylene carbonate, two nitrile of fluoro and fluoro with good filming performance
The synergistic effect of sulphonic acid ester lactone reduces the impedance of electrolyte and interface in positive and negative anodes surface filming, reduces side reaction, improves
The cycle performance and high-temperature storage performance of high-voltage lithium ion batteries.Compared to conventional sultones, flurosulphonic acid lactone is logical
The introduction of F elements is crossed, its filming performance is neither influenced, and electrolyte and interelectrode interface impedance can be improved, to make
Obtaining lithium ion battery has good cycle and high-temperature storage performance.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, any ripe
Professional and technical personnel is known, without departing from the scope of the present invention, according to the technical essence of the invention, to above real
Apply any simple modification, equivalent replacement and improvement etc. made by example, still fall within technical solution of the present invention protection domain it
It is interior.
Claims (10)
1. a kind of high-voltage lithium-ion battery electrolyte, including non-aqueous organic solvent, electrolyte lithium salt and functional electrolyte add
Add agent, which is characterized in that the functionality electrolysis additive includes fluorinated ethylene carbonate, fluoro dinitrile compound and at least
A kind of flurosulphonic acid lactone compound as shown in structural formula I：
Wherein, n is respectively the integer of 0-3.
2. a kind of high-voltage lithium-ion battery electrolyte according to claim 1, which is characterized in that described is non-aqueous organic
Solvent is carboxylate, alpha-fluorocarboxylate ester or carbonic ester.
3. a kind of high-voltage lithium-ion battery electrolyte according to claim 2, which is characterized in that the carboxylate is selected from
One or more of propyl acetate, propyl propionate, ethyl propionate, ethyl butyrate；The alpha-fluorocarboxylate ester is selected from difluoroacetic acid
One or more of propyl ester, trifluoroacetic acid propyl ester, hyptafluorobutyric acid ethyl ester.
4. a kind of high-voltage lithium-ion battery electrolyte according to claim 2, which is characterized in that the carbonic ester is selected from
Ethylene carbonate, propylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, methyl ethyl carbonate,
One or more of methyl propyl carbonate, ethyl propyl carbonic acid ester.
5. a kind of high-voltage lithium ion electrolyte according to claim 1, which is characterized in that the electrolyte lithium salt is
Lithium hexafluoro phosphate, LiBF4, difluorophosphate, double fluorine Lithium bis (oxalate) borates, two (trimethyl fluoride sulfonyl) imine lithiums, double fluorine sulphurs
One or more of acid imide lithium salts.
6. a kind of high-voltage lithium ion electrolyte according to claim 1, which is characterized in that described as shown in structural formula I
Flurosulphonic acid lactone compound be 1,2,3- tri- fluoro- 1,3-propane sultone, bis- fluoro- methyl fluoride -1 2- 1,3-, 3-N-morpholinopropanesulfonic acid
Any one of lactone, 1,3-, bis- fluoro- 2- fluoro ethyls -1,3-propane sultone.
7. a kind of high-voltage lithium ion electrolyte according to claim 1, which is characterized in that the flurosulphonic acid lactone exists
Mass percent in electrolyte is 0.1%-8%；The mass percent of the fluorinated ethylene carbonate in the electrolytic solution is
1%-10%；The fluoro dinitrile compound is any one of fluoro succinonitrile, fluoro glutaronitrile, fluoro adiponitrile or several
Kind, mass percent in the electrolytic solution is 0.5%-8%.
8. a kind of high-voltage lithium-ion battery electrolyte according to claim 1, which is characterized in that the functional electrolysis
Solution additive further includes one kind or more in sulfuric acid vinyl ester, ethylene sulfite, propylene sulfite, vinylethylene carbonate
The mixing of kind, mass percent in the electrolytic solution is 0.1-3%.
9. a kind of high-voltage lithium ion batteries, which is characterized in that including anode, cathode, diaphragm and high electricity described in claim 1
Press lithium-ion battery electrolytes.
10. high-voltage lithium ion batteries according to claim 9, which is characterized in that active matter used by the anode
Matter structural formula is LiCoxM1-xO2, wherein M Al, Sr, Mg, Ti, Ca, Zr, Si or Fe, 0 x≤1 ＜, the lithium ion battery fill
Electric blanking voltage is less than 4.5V more than or equal to 4.4V.
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| CN109473713A (en) * | 2018-12-19 | 2019-03-15 | 珠海光宇电池有限公司 | A kind of high-voltage electrolyte for taking into account high temperature performance and the lithium ion battery using the electrolyte |
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| CN109904522A (en) * | 2019-03-27 | 2019-06-18 | 湖州昆仑动力电池材料有限公司 | High-voltage lithium ion battery electrolyte and additive thereof |
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