CN107959050A - A kind of high-energy-density highly secure lithium ion battery sulfone-based electrolyte and preparation method thereof - Google Patents
A kind of high-energy-density highly secure lithium ion battery sulfone-based electrolyte and preparation method thereof Download PDFInfo
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- CN107959050A CN107959050A CN201711082365.3A CN201711082365A CN107959050A CN 107959050 A CN107959050 A CN 107959050A CN 201711082365 A CN201711082365 A CN 201711082365A CN 107959050 A CN107959050 A CN 107959050A
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- 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
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H—ELECTRICITY
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- 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
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Abstract
The present invention discloses a kind of high-energy-density highly secure lithium ion battery sulfone-based electrolyte and preparation method thereof, belongs to field of lithium ion battery.The electrolyte is that increase is obtained equivalent to 1.5~2.5 times of general electrolytic liquid lithium salt in general electrolytic liquid；The general electrolytic liquid is made of sulfone class solvent, linear carbonate solvent and electric conducting lithium salt；The electric conducting lithium salt is fluorine-containing serial lithium salts.The present invention improves the cycle performance of sulfone class electrolyte using the lithium salts of high concentration, under the conditions of high concentration lithium salts, in discharge process, optimize graphite cathode skin covering of the surface, suppress the surface-active of electrode, so as to suppress further contacting for electrolyte and electrode active material, reduction decomposition of the electrolyte sulfone class solvent in electrode surface is reduced, so as to improve cyclical stability of the lithium ion battery under sulfone-based electrolyte；And security performance, service life and energy density, specific discharge capacity are improved.
Description
Technical field
The invention belongs to field of lithium ion battery, and in particular to a kind of high-energy-density highly secure lithium ion battery sulfuryl
Electrolyte and preparation method thereof.
Background technology
In secondary cell is commercialized, lithium ion battery it is more best than energy highest, cycle performance, and because of its electrode material
Expect the diversity of selection, there is vast potential for future development as energy-storage battery.But with advances in technology and the continuous of market sends out
Exhibition, it is increasingly urgent to the demand of battery energy density, therefore the energy density for lifting lithium battery becomes another item puzzlement scientific research work
The new problem of author.
The positive electrode of Current commercial lithium ion battery mainly has LiMn2O4, cobalt acid lithium, LiFePO 4 etc., these electricity
Pond material has preferable stability, but the demand of people is had been unable to meet in energy density, and exploitation has high-energy-density
New battery material be a method for solving energy density deficiency, but find the huge fund of new battery material needs
Input, it is of high cost, work efficiency is low；The method of another lifting battery energy density is to improve the operating voltage of battery, because this
Kind of method it is easy and effective, be certainly that to improve battery operating voltage be excellent in all lifting battery energy density methods
Choosing.But although we can obtain high energy density under high voltage system, commercialization carbonates electrolyte is in high pressure
Under unstability seriously affected the cycle performance of battery, shorten the cycle life of battery, with lifting energy density just
Inner feelings contradicts, and obstruction is also encountered and then the method for lifting energy density by improving operating voltage.But comprehensive cost, efficiency etc.
The problem of aspect, improves voltage to lift the method for energy density or advantageous.Therefore battery energy density is lifted again
One method is to find that the electrolyte of high-pressure work can be matched, can be toward adding high voltage bearing addition in carbonates electrolyte
Agent achieves the goal, but this method is palliative, and the electrolyte of sulfuryl was reported first in 1985, sulfone class is due to band
There is strong electron-withdrawing group to roll into a ball and possess higher oxidizing potential [more than 5.0V (vs.Li/Li+)], its wide electrochemical window is with low
The shortening of polymers chain and become wider, be preferable high pressure resistant solvent, high pressure can be fundamentally solved using sulfone-based electrolyte
The problem of unstable.Unfortunately, the most common shortcoming of sulfone class is its incompatibility between graphite electrode, is caused substantial amounts of
Irreversible capacity produces.Although it still cannot effectively be passivated graphite electricity by the use of EMC as cosolvent, the electrolyte of sulfolane base
Pole.Therefore sulfone class solvent and the necessity of graphite cathode compatibility are improved.
The content of the invention
The shortcomings that in order to overcome the prior art and deficiency, primary and foremost purpose of the invention are to provide a kind of high-energy-density height
Safety lithium ion cell sulfone-based electrolyte.The electrolyte is to improve sulfone class by improving the concentration of lithium salts in sulfone class electrolyte
The cyclical stability of solvent, i.e., it is convenient and economical.The electrolysis liquid energy significantly improves the circulation under the conditions of lithium ion battery high-voltage
Stability and service life.
Another object of the present invention is to provide above-mentioned high-energy-density highly secure lithium ion battery sulfone-based electrolyte
Preparation method.
Another object of the present invention is to be to provide above-mentioned high-energy-density highly secure lithium ion battery sulfone-based electrolyte
Application.
The purpose of the present invention is achieved through the following technical solutions：
A kind of high-energy-density highly secure lithium ion battery sulfone-based electrolyte, the electrolyte are in general electrolytic liquid
Increase what is obtained equivalent to 1.5~2.5 times of general electrolytic liquid lithium salt；The general electrolytic liquid is by sulfone class solvent, line
Type carbonate solvent and electric conducting lithium salt are formed；
For high concentration lithium salts as the condition for improving sulfone class electrolyte cyclical stability, the electric conducting lithium salt is fluorine-containing series
Lithium salts, concentration of the electric conducting lithium salt in general electrolytic liquid is preferably 1M；As shown in Equation 1 one that the sulfone class solvent refers to
One kind in series compound or at least two；
Wherein, the R1And R2For any one in following situations：Free hydrogen, the alkyl of carbon number 1~20, carbon are former
The cycloalkyl of subnumber 3~20, the aryl of carbon number 6~30, the aralkyl of carbon number 6~30, part hydrogen or whole hydrogen quilts
The straight chained alkyl that the carbon number of halogen substitution is 1~6.
It is furthermore preferred that the sulfone class solvent is sulfolane；
Preferably, the electrolyte be in general electrolytic liquid increase equivalent to general electrolytic liquid lithium salt 1.5~
2.0 times obtain.
It is furthermore preferred that the electrolyte is to increase in general electrolytic liquid equivalent to the 2.0 of general electrolytic liquid lithium salt
Obtain again.
The sulfone class solvent and the mass ratio of linear carbonate solvent are preferably：Sulfone class solvent accounts for total solvent mass ratio
More than 30%；More preferably 40%.
The linear carbonate solvent is preferably dimethyl carbonate (DMC), methyl ethyl carbonate (EMC), diethyl carbonate
(DEC) and one kind or at least two in methyl propyl carbonate (MPC)；
The electric conducting lithium salt is preferably lithium hexafluoro phosphate (LiPF6), LiBF4 (LiBF4), difluorine oxalic acid boracic acid lithium
(LiDFOB), trifluoromethyl sulfonic acid lithium (LiSO3CF3), hexafluoroarsenate lithium (LiAsF6), per-fluoroalkyl sulfonyl lithium methide (LiC
(CF3SO2)3) and bis trifluoromethyl sulfimide lithium (Li (CF3SO2)2N one kind in) or at least two；
The preparation method of above-mentioned high-energy-density highly secure lithium ion battery sulfone-based electrolyte, includes the following steps：
(1) sulfone class solvent and linear carbonate solvent are mixed, clarification, water removal, obtain mixed solvent；
(2) electric conducting lithium salt is added into step (1) obtained in the mixed solvent, obtains general electrolytic liquid；
(3) added in the general electrolytic liquid that step (2) is prepared equivalent to 1.5~2.5 times of general electrolytic liquid concentration
Electric conducting lithium salt；Obtain the sulfone-based electrolyte.
Clarification described in step (1), water removal are preferably by molecular sieve, activated carbon, calcium hydride, lithium hydride, anhydrous
In calcium oxide, calcium chloride, phosphorus pentoxide, alkali or alkaline earth metal any one or at least two handled；
The molecular sieve can beType,Type orType, is preferablyType orType；
High-energy-density highly secure lithium ion battery sulfone-based electrolyte is applied to manufacture lithium ion battery, obtains
Battery there is good charge-discharge performance.
The present invention is had the following advantages relative to the prior art and effect：
(1) present invention improves the cycle performance of sulfone class electrolyte using the lithium salts of high concentration, in high concentration lithium salts condition
Under, in discharge process, Li ions slough solvation shell, the component PF of solvation shell on graphite electrode surface6 -In electrode table
Face reduction generation F-The LiF combined to form with lithium ion participates in constructing to form one layer of densification, the SEI films of stabilization jointly, optimizes
Graphite cathode skin covering of the surface, suppresses the surface-active of electrode, so as to suppress further contacting for electrolyte and electrode active material, subtracts
Lack reduction decomposition of the electrolyte sulfone class solvent in electrode surface, so that it is steady to improve circulation of the lithium ion battery under sulfone-based electrolyte
It is qualitative,
(2) present invention improves the cyclical stability of sulfone class electrolyte using the lithium salts of high concentration, due in enrichment PF6 -'s
Under the conditions of, the LiF formed in cyclic process is the pith for constructing high quality SEI, can effectively suppress electrolyte point
Solution, effectively protects graphite electrode, promotes the utilization of sulfone class electrolyte.
(3) high-voltage lithium-ion battery electrolyte described in is applied to manufacture lithium ion battery, obtained lithium ion battery
Security performance, service life and energy density, specific discharge capacity is improved.
Brief description of the drawings
Fig. 1 is half electricity of graphite that sulfuryl lithium-ion battery electrolytes prepared by embodiment 1,2,3 and comparison example make
Pond charge and discharge cycles figure.
Fig. 2 is that the graphite half-cell battery charging and discharging that electrolyte of the different salinity using DMC as one-part solvent makes follows
Ring figure.
Fig. 3 is that the graphite half-cell battery charging and discharging that electrolyte of the 1ML lithium salts using sulfolane as one-part solvent makes is bent
Line.
Embodiment
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) sulfolane (SL), linear carbonate solvent diethyl carbonate (DMC) SL in mass ratio：DMC=1：1.5 mixing,
Using molecular sieveCalcium hydride, lithium hydride clarification, water removal, obtain mixed solvent；
(2) by electric conducting lithium salt LiPF6The in the mixed solvent that step (1) obtains is dissolved in, stirs evenly, is made into general electrolytic
Liquid；Wherein electric conducting lithium salt LiPF6Final concentration of 1mol/L in general electrolytic liquid；
(3) 1.5 times that lithium salt is general electrolytic liquid are increased in the general electrolytic liquid that step (2) is prepared；
To sulfuryl lithium-ion battery electrolytes.
Embodiment 2
(1) sulfolane (SL), linear carbonate solvent diethyl carbonate (DMC) SL in mass ratio：DMC=1：1.5 mixing,
Using molecular sieveCalcium hydride, lithium hydride clarification, water removal, obtain mixed solvent；
(2) by electric conducting lithium salt LiPF6The in the mixed solvent that step (1) obtains is dissolved in, stirs evenly, is made into general electrolytic
Liquid；Wherein electric conducting lithium salt LiPF6Final concentration of 1mol/L in general electrolytic liquid；
(3) 2 times that lithium salt is general electrolytic liquid are increased in the general electrolytic liquid that step (2) is prepared；Obtain
Sulfuryl lithium-ion battery electrolytes.
Embodiment 3
(1) sulfolane (SL), linear carbonate solvent diethyl carbonate (DMC) SL in mass ratio：DMC=1：1.5 mixing,
Using molecular sieveCalcium hydride, lithium hydride clarification, water removal, obtain mixed solvent；
(2) by electric conducting lithium salt LiPF6The in the mixed solvent that step (1) obtains is dissolved in, stirs evenly, is made into general electrolytic
Liquid；Wherein electric conducting lithium salt LiPF6Final concentration of 1mol/L in general electrolytic liquid；
(3) it is 2.5 times of general electrolytic liquid to increase lithium salt in the general electrolytic liquid that step (2) is prepared；Obtain
Sulfuryl lithium-ion battery electrolytes.
Embodiment 4
(1) sulfolane (SL), linear carbonate solvent diethyl carbonate (DMC) SL in mass ratio：DMC=1：1.5 mixing,
Using molecular sieveCalcium hydride, lithium hydride clarification, water removal, obtain mixed solvent；
(2) electric conducting lithium salt LiDFOB is dissolved in the in the mixed solvent that step (1) obtains, stirs evenly, be made into common electricity
Solve liquid；Final concentration of 1mol/Ls of the wherein electric conducting lithium salt LiDFOB in general electrolytic liquid；
(3) 2.5 times that lithium salt is general electrolytic liquid are increased in the general electrolytic liquid that step (2) is prepared；
To sulfuryl lithium-ion battery electrolytes.
Embodiment 5
(1) sulfolane (SL), linear carbonate solvent diethyl carbonate (DMC) SL in mass ratio：DMC=1：1.5 mixing,
Using molecular sieveCalcium hydride, lithium hydride clarification, water removal, obtain mixed solvent；
(2) by electric conducting lithium salt LiAsF6The in the mixed solvent that step (1) obtains is dissolved in, stirs evenly, is made into common electricity
Solve liquid；Wherein electric conducting lithium salt LiAsF6Final concentration of 1mol/L in general electrolytic liquid；
(3) 2.5 times that lithium salt is general electrolytic liquid are increased in the general electrolytic liquid that step (2) is prepared；
To sulfuryl lithium-ion battery electrolytes.
Embodiment 6
(1) sulfolane (SL), linear carbonate solvent diethyl carbonate (DMC) SL in mass ratio：DMC=1：1.5 mixing,
Using molecular sieveCalcium hydride, lithium hydride clarification, water removal, obtain mixed solvent；
(2) by electric conducting lithium salt Li (CF3SO2)2N is dissolved in the in the mixed solvent that step (1) obtains, and stirs evenly, and is made into general
Logical electrolyte；Wherein electric conducting lithium salt Li (CF3SO2)2Final concentration of 1mol/Ls of the N in general electrolytic liquid；
(3) 2.5 times that lithium salt is general electrolytic liquid are increased in the general electrolytic liquid that step (2) is prepared；
To sulfuryl lithium-ion battery electrolytes.
Embodiment 7
(1) sulfolane (SL), linear carbonate solvent diethyl carbonate (DMC) SL in mass ratio：DMC=1：1.5 mixing,
Using molecular sieveCalcium hydride, lithium hydride clarification, water removal, obtain mixed solvent；
(2) by electric conducting lithium salt LiC (CF3SO2)3The in the mixed solvent that step (1) obtains is dissolved in, stirs evenly, is made into general
Logical electrolyte；Wherein electric conducting lithium salt LiC (CF3SO2)3Final concentration of 1mol/L in general electrolytic liquid；
(3) 2 times that lithium salt is general electrolytic liquid are increased in the general electrolytic liquid that step (2) is prepared；Obtain
Sulfuryl lithium-ion battery electrolytes.
Comparative example
(1) sulfolane (SL), linear carbonate solvent diethyl carbonate (DMC) SL in mass ratio：DMC=1：1.5 mixing,
Using molecular sieveCalcium hydride, lithium hydride clarification, water removal, obtain mixed solvent；
(2) by electric conducting lithium salt LiPF6The in the mixed solvent that step (1) obtains is dissolved in, stirs evenly, obtains general electrolytic
Liquid；Wherein electric conducting lithium salt LiPF6Final concentration of 1.0mol/L in general electrolytic liquid.
Effect compares：
The sulfuryl lithium-ion battery electrolytes and comparative example that embodiment 1,2,3 is prepared are prepared common
Electrolyte is compared：
(1) Fig. 1 is the lithium ion battery of sulfuryl lithium-ion battery electrolytes making prepared by embodiment 1,2,3 in application electricity
Solution liquid prepares button cell, carries out the test of charge-discharge performance：With the graphite of mass percent 80%, mass percent 10%
PVDF and the conductive carbon black of mass percent 10% are working electrode, and lithium metal is added and implemented as reference electrode and to electrode
30 μ L of general electrolytic liquid prepared by high-voltage lithium-ion battery electrolyte or comparative example prepared by example 1,2,3.In room temperature
With 0.05C, the circle of charge and discharge 3 carries out cell activation processing between 0.005V to 2.5V under 25 DEG C of constant temperature, is then arrived with 0.1C in 0.005V
2.5V charge-discharge test.As shown in Figure 1, comparative example cyclical stability is substantially not as good as embodiment 1,2,3；And embodiment 1,2,
The 3 sulfone Li-like ions battery electrolytes prepared are used for capacity retention ratio after lithium ion battery circulates 125 weeks and are above comparison example,
Illustrate that high concentration lithium salts can improve the cyclical stability of sulfone class electrolyte.
(2) the graphite half-cell battery charging and discharging that electrolyte of Fig. 2 differences salinity using DMC as one-part solvent makes
Can test：With the graphite of mass percent 80%, the PVDF of mass percent 10% and the conductive carbon black of mass percent 10%
For working electrode, lithium metal as reference electrode and to electrode, be separately added into 1,1.5,2, the LiPF of 2.5M6Salt, using DMC to be molten
The 30 μ L of electrolyte of agent composition.With 0.05C, the circle of charge and discharge 3 carries out cell activation between 0.005V to 2.5V under 25 DEG C of constant temperature of room temperature
Processing, then with 0.1C in 0.005V to 2.5V charge-discharge tests.As shown in Fig. 2, with the raising of lithium salt, to graphite half
The cycle performance of battery does not have big influence, and the chemical property showed is different from the electrolyte of sulfuryl, it may be said that bright reality
In example, the effect of DMC solvents mainly reduces the viscosity of sulfone-based electrolyte, and what cycle performance mainly showed is the behavior of SL.
(3) Fig. 3 is the lithium salts (LiPF using SL as pure solvent6) concentration for 1M composition electrolyte make graphite half-cell
Battery first circle charge and discharge electrograph.As shown in figure 3, using SL as the electrolyte of pure solvent the Li on graphite half-cell+It can only be embedded in almost
It is de- not come out, further verify other researchers conclusion incompatible to graphite to SL.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
- A kind of 1. high-energy-density highly secure lithium ion battery sulfone-based electrolyte, it is characterised in that：The electrolyte is general Increase is obtained equivalent to 1.5~2.5 times of general electrolytic liquid lithium salt in logical electrolyte；The general electrolytic liquid is by sulfone Class solvent, linear carbonate solvent and electric conducting lithium salt are formed；The electric conducting lithium salt is fluorine-containing serial lithium salts.
- 2. high-energy-density highly secure lithium ion battery sulfone-based electrolyte according to claim 1, it is characterised in that：One kind or at least two in a series of compounds as shown in Equation 1 that the sulfone class solvent refers to；Wherein, the R1And R2For any one in following situations：Free hydrogen, the alkyl of carbon number 1~20, carbon number 3 ~20 cycloalkyl, the aryl of carbon number 6~30, the aralkyl of carbon number 6~30, part hydrogen or whole hydrogen is taken by halogen The carbon number in generation is 1~6 straight chained alkyl.
- 3. high-energy-density highly secure lithium ion battery sulfone-based electrolyte according to claim 1, it is characterised in that：Concentration of the electric conducting lithium salt in general electrolytic liquid is 1M.
- 4. high-energy-density highly secure lithium ion battery sulfone-based electrolyte according to claim 1 or 2, its feature exist In：The sulfone class solvent and the mass ratio of linear carbonate solvent are：Sulfone class solvent accounts for total solvent mass ratio more than 30%.
- 5. high-energy-density highly secure lithium ion battery sulfone-based electrolyte according to claim 1, it is characterised in that：The linear carbonate solvent is one in dimethyl carbonate, methyl ethyl carbonate, diethyl carbonate and methyl propyl carbonate Kind or at least two.
- 6. the high-energy-density highly secure lithium ion battery sulfone-based electrolyte according to claim 1 or 3, its feature exist In：The electric conducting lithium salt is lithium hexafluoro phosphate, LiBF4, difluorine oxalic acid boracic acid lithium, trifluoromethyl sulfonic acid lithium, hexafluoro Arsenic acid lithium, per-fluoroalkyl sulfonyl lithium methide and one kind in bis trifluoromethyl sulfimide lithium or at least two.
- 7. the preparation side of claim 1~6 any one of them high-energy-density highly secure lithium ion battery sulfone-based electrolyte Method, it is characterised in that include the following steps：(1) sulfone class solvent and linear carbonate solvent are mixed, clarification, water removal, obtain mixed solvent；(2) electric conducting lithium salt is added into step (1) obtained in the mixed solvent, obtains general electrolytic liquid；(3) equivalent to general electrolytic liquid concentration 1.5~2.5 times are added in the general electrolytic liquid that step (2) is prepared to lead Electric lithium salts；Obtain the sulfone-based electrolyte.
- 8. the preparation method of high-energy-density highly secure lithium ion battery sulfone-based electrolyte according to claim 7, its It is characterized in that：Clarification, water removal described in step (1) pass through molecular sieve, activated carbon, calcium hydride, lithium hydride, anhydrous calcium oxide, chlorine Change calcium, phosphorus pentoxide, in alkali or alkaline earth metal any one or at least two handled.
- 9. the preparation method of high-energy-density highly secure lithium ion battery sulfone-based electrolyte according to claim 8, its It is characterized in that：The molecular sieve isType,Type orType.
- 10. claim 1~6 any one of them high-energy-density highly secure lithium ion battery sulfone-based electrolyte is in manufacture lithium Application in ion battery.
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| US12107227B2 (en) | 2018-09-28 | 2024-10-01 | Contemporary Amperex Technology Co., Limited | Nonaqueous electrolyte, lithium-ion battery, battery module, battery pack, and apparatus |
| CN113161618A (en) * | 2021-03-31 | 2021-07-23 | 厦门大学 | High-voltage electrolyte for lithium secondary battery working in wide temperature range and preparation method and application thereof |
| CN114725509A (en) * | 2022-04-25 | 2022-07-08 | 西安交通大学 | Sulfone-based lithium battery electrolyte and lithium battery |
| CN115458811A (en) * | 2022-09-02 | 2022-12-09 | 哈尔滨工业大学（深圳） | Electrolyte based on sulfone-based eutectic solvent, preparation method of electrolyte and lithium ion battery |
| CN115458811B (en) * | 2022-09-02 | 2023-03-21 | 哈尔滨工业大学（深圳） | Electrolyte based on sulfone-based eutectic solvent, preparation method thereof and lithium ion battery |
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Application publication date: 20180424 |