CN105742703A - High-voltage functional electrolyte containing LiDFOB additive and preparation and application thereof - Google Patents
High-voltage functional electrolyte containing LiDFOB additive and preparation and application thereof 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
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- 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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Abstract
The invention discloses a high-voltage functional electrolyte containing a LiDFOB additive and preparation and application thereof, belonging to the field of a lithium ion battery. The electrolyte is prepared by adding a functional additive into an ordinary electrolyte, wherein the ordinary electrolyte comprises an annular carbonic ester solvent, a linear carbonic ester solvent and a conductive lithium salt, and the functional additive is LiDFOB. In the electrolyte, the LiDFOB additive is taken as a high-voltage film formation additive of the lithium ion electrolyte, a layer of compact and stable SEI membrane can be formed on the surfaces of a positive electrode and a negative electrode during the initial charging and discharging process, the membrane on the surfaces of the positive electrode and the negative electrode is optimized, the resistance between the positive electrode and the electrolyte is reduced, the surface activity of the electrode is suppressed, thus, further contact between the electrolyte and an electrode active substance is prevented, and the oxidative decomposition of a main body solvent on the surface of the electrode is reduced. The cycle performance and the rate performance of the lithium ion battery containing the electrolyte additive can be improved at 3-4.5V.
Description
Technical field
The invention belongs to field of lithium ion battery, particularly to a kind of high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive and preparation method thereof and application.
Background technology
The advantage that lithium ion battery has that energy density is big, running voltage is high and has extended cycle life etc..The positive electrode of Current commercial lithium ion battery has LiMn2O4, cobalt acid lithium, LiFePO4, ternary material, and these are several, charge cutoff voltage is generally no more than 4.2V, along with the development of scientific and technological progress and market, the energy density promoting lithium battery seems important and urgent day by day.Except the improvement of current material and battery production technology, high voltage (> 4.5V) positive electrode is one of popular research direction of comparison, realizes the high-energy-density of battery mainly by the depth of charge promoting positive electrode active materials.
Along with the progress of science and technology, the requirement of energy storage device is improved by the field such as electronic product, electric automobile, armarium and space flight and aviation day by day, and energy density is high, volume is little, the lithium ion battery that has extended cycle life is used widely.At present, the positive electrode of business lithium ion battery mainly has LiMn2O4, cobalt acid lithium, ternary material, LiFePO 4 several, and its charge cutoff voltage is usually no more than 4.2V.Along with progress and the development in market of science and technology, promote the energy density of lithium battery and day by day seem important and urgent.What therefore promote lithium ion battery uses voltage thus the energy density improving battery is the emphasis of research at present.
But, while improving positive electrode voltage, the electrical properties such as the charge and discharge cycles of battery are but declining, and reason is that cobalt acid lithium material structure is not sufficiently stable the matching problem with electrolyte on the one hand, is that transition metal ions can deposit to negative pole and destroy negative pole granule on the other hand.Conventional commercial electrolyte liquid easily decomposes at anode surface oxidation under high voltages, and the oxidative decomposition of electrolyte self also can promote the pernicious reactions such as the change of positive electrode pattern, structure collapses simultaneously.Therefore must develop a kind of resistant to (> 4.2V) high-tension electrolyte, and then realize the excellent performance of lithium battery performance, improve lithium battery cycle life.It is improve the method that the most convenient of performance of lithium ion battery is most economical by adding a small amount of electrolysis additive in conventional lithium-ion battery electrolytes.
Summary of the invention
In order to overcome shortcoming and the deficiency of prior art, the primary and foremost purpose of the present invention is in that to provide a kind of high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.This electrolyte is by adding functional additive difluorine oxalic acid boracic acid lithium (LiDFOB); when being applied to lithium ion battery; the surface activity of positive electrode can be reduced; suppress the oxidation Decomposition of electrolyte; protection positive electrode granule is not subjected to destroy; suppress the dissolution of transition metal ions, simultaneously can at negative terminal surface reduction protection negative pole granule, it is possible to improve high-voltage lithium ion batteries cycle performance at normal temperatures.This electrolyte can significantly improve cyclical stability when lithium ion battery high-voltage.
The preparation method that another object of the present invention is to provide the described high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.
It is still another object of the present invention to provide the application of the described high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.
The purpose of the present invention is achieved through the following technical solutions:
A kind of high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive, this electrolyte adds functional additive in general electrolytic liquid and prepares；Described general electrolytic liquid is made up of cyclic carbonate solvents, linear carbonates solvent and electric conducting lithium salt；Described functional additive is difluorine oxalic acid boracic acid lithium (LiDFOB).
Described high pressure refers to the charge cutoff voltage high voltage more than 4.2V；
The interpolation of described functional additive optimizes positive pole/electrolyte interface, reduces the surface activity of positive pole, it is suppressed that the oxidation Decomposition of electrolyte, so the present invention can improve high voltage (> 4.2V) cobalt acid lithium material is the circulation of the lithium battery of positive electrode.
The content of described functional additive is the 0.5～10% of general electrolytic liquid quality；It is preferably 1%～4%.
As preferably, shown in the solvent burden ratio of described general electrolytic liquid: the mass ratio of cyclic carbonate solvents and linear carbonates solvent is (1:3)～(3:2)；
The described electric conducting lithium salt final concentration of 0.8～1.2mol/L in general electrolytic liquid；
Described cyclic carbonate solvents is preferably ethylene carbonate (EC) or Allyl carbonate (PC)；
Described linear carbonates solvent includes dimethyl carbonate (DMC), Ethyl methyl carbonate (EMC), diethyl carbonate (DEC) and at least one in methyl propyl carbonate (MPC)；
Described electric conducting lithium salt is selected from lithium hexafluoro phosphate (LiPF6), LiBF4 (LiBF4), dioxalic acid Lithium biborate (LiBOB), trifluoromethyl sulfonic acid lithium (LiSO3CF3), lithium perchlorate (LiClO4), hexafluoroarsenate lithium (LiAsF6), bis trifluoromethyl sulfimide lithium (Li (CF3SO2)2And LiC (CF N)3SO2)3In at least one；
The preparation method of the described high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive, comprises the steps:
(1) cyclic carbonate solvents and linear carbonates solvent are mixed, clarification, dewater；
(2) at ambient temperature, electric conducting lithium salt is added in the solvent that step (1) is obtained, obtain general electrolytic liquid；
(3) in the general electrolytic liquid that step (2) obtains, add functional additive, obtain the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive；Described functional additive is difluorine oxalic acid boracic acid lithium；
Cyclic carbonate solvents described in step (1) and linear carbonates solvent be (1:3)～(3:2) mixing in mass ratio preferably；
Described cyclic carbonate solvents is preferably ethylene carbonate (EC) or Allyl carbonate (PC)；
Described linear carbonates solvent includes dimethyl carbonate (DMC), Ethyl methyl carbonate (EMC), diethyl carbonate (DEC) and at least one in methyl propyl carbonate (MPC)；
Clarification described in step (1), dewatering processes preferably by any one or a few in molecular sieve, activated carbon, calcium hydride, lithium hydride, anhydrous calcium oxide, calcium chloride, phosphorus pentoxide, alkali metal or alkaline-earth metal；
Described molecular sieve can adoptType,Type orType, it is desirable to selectType orType.
The temperature of the room temperature described in step (2) is 25～40 DEG C；
The consumption of the electric conducting lithium salt described in step (2) is preferably the final concentration of 0.8～1.2mol/L in described general electrolytic liquid；
Described electric conducting lithium salt is selected from lithium hexafluoro phosphate (LiPF6), LiBF4 (LiBF4), dioxalic acid Lithium biborate (LiBOB), trifluoromethyl sulfonic acid lithium (LiSO3CF3), lithium perchlorate (LiClO4), hexafluoroarsenate lithium (LiAsF6), bis trifluoromethyl sulfimide lithium (Li (CF3SO2)2And LiC (CF N)3SO2)3In at least one；
The described high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive is applied to manufacture lithium ion battery, and the battery obtained has good charge-discharge performance.
A kind of lithium ion battery containing the above-mentioned high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive, including positive plate and negative plate, electrolyte, barrier film；Described positive plate is made up of cobalt acid lithium material, and negative plate is made up of graphite material, and the barrier film being interval in positive plate and negative plate is made up of polyethylene film, and described electrolyte is the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive described above.
The functional additive that the present invention uses is in the discharge and recharge system of 3～4.5V; the film with defencive function one layer stable can be defined at positive pole and negative terminal surface; the oxidation Decomposition protection positive electrode inhibiting high-voltage electrolyte on the one hand is not subjected to destroy; protection negative pole pole material on the other hand, it is possible to improve the cycle performance of high-voltage lithium ion.
The present invention, relative to prior art, has such advantages as and effect:
The present invention uses difluorine oxalic acid boracic acid lithium additive as the high pressure film for additive of lithium-ion electrolyte, there is relatively low oxidizing potential and higher reduction potential due to such additive, first charge-discharge process can form one layer of densification, stable SEI film at positive pole and negative terminal surface, optimize both positive and negative polarity skin covering of the surface, reduce the resistance between positive pole and electrolyte, suppress the surface activity of electrode, thus suppressing electrolyte to contact with the further of electrode active material, reduce the electrolyte bulk solvent oxidation Decomposition at electrode surface.The lithium ion battery containing this electrolysis additive cycle performance under 3～4.5V and high rate performance improve.
Accompanying drawing explanation
Fig. 1 is the discharge and recharge comparison diagrams of lithium ion battery circulation 250 circle of the electrolyte making that the embodiment of the present invention 1 is prepared with comparative example.
Fig. 2 is the lithium ion battery coulombic efficiency comparison diagram of the electrolyte making that the embodiment of the present invention 1 is prepared with comparative example.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, and adopt molecular sieve, calcium hydride, lithium hydride clarification, dewater；
(2) at ambient temperature, by electric conducting lithium salt LiPF6It is dissolved in the solvent that step (1) obtains, final concentration of 1.0mol/L, stir, obtain general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2), add consumption is general electrolytic liquid quality the 1% of difluorine oxalic acid boracic acid lithium；Obtain the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.
Embodiment 2
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, and adopt molecular sieve, calcium hydride, lithium hydride clarification, dewater；
(2) at ambient temperature, by electric conducting lithium salt LiPF6It is dissolved in the solvent that step (1) obtains, final concentration of 1.0mol/L, stir, be made into general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2), add consumption is general electrolytic liquid quality the 2% of difluorine oxalic acid boracic acid lithium；Obtain the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.
Embodiment 3
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, adopt molecular sieve, calcium hydride, lithium hydride clarification, dewater；
(2) at ambient temperature, by electric conducting lithium salt LiPF6It is dissolved in the solvent that step (1) obtains, final concentration of 1.0mol/L, stir, be made into general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2), add consumption is general electrolytic liquid quality the 3% of difluorine oxalic acid boracic acid lithium；Obtain the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.
Embodiment 4
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, adopt molecular sieve, calcium hydride, lithium hydride clarification, dewater；
(2) at ambient temperature, by electric conducting lithium salt LiPF6It is dissolved in the solvent that step (1) obtains, final concentration of 1.0mol/L, stir, be made into general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2), add consumption is general electrolytic liquid quality the 4% of difluorine oxalic acid boracic acid lithium；Obtain the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.
Embodiment 5
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, adopt molecular sieve, calcium hydride, lithium hydride clarification, dewater；
(2) at ambient temperature, by electric conducting lithium salt LiAsF6It is dissolved in the solvent that step (1) obtains, final concentration of 1mol/L, stir, be made into general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2), add consumption is general electrolytic liquid quality the 1% of difluorine oxalic acid boracic acid lithium；Obtain the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.
Embodiment 6
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, adopt molecular sieve, calcium hydride, lithium hydride clarification, dewater；
(2) at ambient temperature, by electric conducting lithium salt Li (CF3SO2)2N is dissolved in the solvent that step (1) obtains, and final concentration of 1.0mol/L stirs, is made into general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2), add consumption is general electrolytic liquid quality the 2% of difluorine oxalic acid boracic acid lithium；Obtain the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.
Embodiment 7
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, adopt molecular sieve, calcium hydride, lithium hydride clarification, dewater；
(2) at ambient temperature, by electric conducting lithium salt LiC (CF3SO2)3It is dissolved in the solvent that step (1) obtains, final concentration of 1.0mol/L, stir, be made into general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2), add consumption is general electrolytic liquid quality the 3% of difluorine oxalic acid boracic acid lithium；Obtain the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.
Comparative example
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate (EMC) and diethyl carbonate (DEC) EC:EMC:DEC=3:5:2 in mass ratio mixing, adopt molecular sieve, lithium hydride clarification, dewater；
(2) at ambient temperature, by electric conducting lithium salt LiPF6It is dissolved in the solvent that step (1) obtains, final concentration of 1.0mol/L, stir, be made into general electrolytic liquid.
Effectiveness comparison:
The high voltage functionality electrolyte (that is to say 1%LiDFOB) containing difluorine oxalic acid boracic acid lithium additive and contrast general electrolytic liquid (that is to say STD) that embodiment 1 are prepared compare:
(1) Fig. 1 is the discharge and recharge comparison diagram of lithium ion battery circulation 200 circle that the embodiment of the present invention 1 makes in electrolyte prepared by comparative example.From the results, it was seen that the electrolyte adding difluorine oxalic acid boracic acid lithium in electrolyte can improve its cycle performance under high voltages for lithium ion battery.
(2) Fig. 2 is the lithium ion coulombic efficiency test comparison figure that the embodiment of the present invention 1 makes in electrolyte prepared by comparative example.As can be seen from the results; after adding difluorine oxalic acid boracic acid lithium in electrolyte, the coulombic efficiency of lithium ion battery significantly improves, and illustrates that this additive can form protecting film on both positive and negative polarity surface; oxidation and the reduction decomposition of electrolyte can be suppressed, improve the chemical property of lithium ion battery.
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are also not restricted to the described embodiments; the change made under other any spirit without departing from the present invention and principle, modification, replacement, combination, simplification; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive, it is characterised in that: this electrolyte adds functional additive in general electrolytic liquid and prepares；Described general electrolytic liquid is made up of cyclic carbonate solvents, linear carbonates solvent and electric conducting lithium salt；Described functional additive is difluorine oxalic acid boracic acid lithium.
2. the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive according to claim 1, it is characterised in that: the content of described functional additive is the 0.5～10% of general electrolytic liquid quality.
3. the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive according to claim 1, it is characterised in that: the mass ratio of described cyclic carbonate solvents and linear carbonates solvent is (1:3)～(3:2)；
The described electric conducting lithium salt final concentration of 0.8～1.2mol/L in general electrolytic liquid.
4. the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive according to claim 1, it is characterised in that: described cyclic carbonate solvents is ethylene carbonate or Allyl carbonate；
Described linear carbonates solvent includes dimethyl carbonate, Ethyl methyl carbonate, diethyl carbonate and at least one in methyl propyl carbonate.
5. the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive according to claim 1, it is characterised in that: described electric conducting lithium salt is selected from LiPF6、LiBF4、LiBOB、LiSO3CF3、LiClO4、LiAsF6、Li(CF3SO2)2N and LiC (CF3SO2)3In at least one.
6. the preparation method of the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive described in any one of Claims 1 to 5, it is characterised in that comprise the steps:
(1) cyclic carbonate solvents and linear carbonates solvent are mixed, clarification, dewater；
(2) at ambient temperature, electric conducting lithium salt is added in the solvent that step (1) is obtained, obtain general electrolytic liquid；
(3) in the general electrolytic liquid that step (2) obtains, add functional additive, obtain the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive.
7. the preparation method of the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive according to claim 6, it is characterised in that: the clarification described in step (1), dewatering is processed by any one or a few in molecular sieve, activated carbon, calcium hydride, lithium hydride, anhydrous calcium oxide, calcium chloride, phosphorus pentoxide, alkali metal or alkaline-earth metal.
8. the preparation method of the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive according to claim 7, it is characterised in that: described molecular sieve adoptsType,Type orType.
9. the application in manufacturing lithium ion battery of the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive described in any one of Claims 1 to 5.
10. the lithium ion battery containing the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive described in any one of Claims 1 to 5, it is characterised in that include positive plate and negative plate, electrolyte, barrier film；Described positive plate is made up of cobalt acid lithium material, negative plate is made up of graphite material, the barrier film being interval in positive plate and negative plate is made up of polyethylene film, and described electrolyte is the high voltage functionality electrolyte containing difluorine oxalic acid boracic acid lithium additive described in any one of Claims 1 to 5.
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