CN113346142B - Low-concentration electrolyte for lithium ion secondary battery and lithium ion secondary battery - Google Patents
Low-concentration electrolyte for lithium ion secondary battery and lithium ion secondary battery Download PDFInfo
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- CN113346142B CN113346142B CN202110782843.1A CN202110782843A CN113346142B CN 113346142 B CN113346142 B CN 113346142B CN 202110782843 A CN202110782843 A CN 202110782843A CN 113346142 B CN113346142 B CN 113346142B
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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
- H01M10/0569—Liquid materials characterised by the solvents
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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
- H01M10/056—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
- H01M10/0568—Liquid materials characterised by the solutes
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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
- H01M2300/0028—Organic electrolyte characterised by the solvent
- H01M2300/0037—Mixture of solvents
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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 invention discloses a low-concentration electrolyte for a lithium ion secondary battery, which comprises a lithium salt and an organic solvent, wherein the organic solvent comprises a chain carboxylic ester solvent and a fluorinated carboxylic ester solvent, and the concentration of the lithium salt is 0.01-0.5 mol/L. The electrolyte adopts a mixed solvent of a chain carboxylic ester solvent and a fluorinated carboxylic ester solvent as a solvent system of the electrolyte, and adds a low-concentration lithium salt, so that the formed electrolyte system has low viscosity and good wettability with positive and negative electrodes, can form a stable CEI/SEI layer, relieves the dissolution of transition metals in a circulation process, can reduce the production cost, has considerable application prospect, and has good circulation performance of an assembled battery.
Description
Technical Field
The invention relates to a low-concentration electrolyte for a lithium ion secondary battery and the lithium ion secondary battery, belonging to the field of lithium ion batteries.
Background
The lithium ion battery is widely applied in the fields of portable electronic products, electric automobiles and the like. In order to meet the increasing energy density demand, efforts are made to develop high energy density positive electrode materials and to increase the operating voltage of lithium ion batteries. The existing commercial lithium ion battery anode material is mainly an intercalation type anode material and is divided into a layered oxide anode material (lithium cobaltate and ternary material), a spinel structure (lithium manganate and lithium nickel manganate) and a polyanion type anode material lithium iron phosphate. Lithium ions are extracted and inserted in the charging and discharging process. The intercalation type anode material has good stability and is suitable for commercial lithium ion batteries. However, as the surface of the positive electrode material and the electrolyte undergo side reaction in the circulation process, lithium salt in the electrolyte reacts with trace water generated in the battery preparation process to decompose and generate hydrogen fluoride, and the generated hydrogen fluoride attacks the positive electrode to dissolve transition metal ions into the electrolyte to be deposited on the negative electrode side, so that the SEI layer on the surface of the negative electrode is reconstructed, the impedance of a battery system is increased, the capacity attenuation of the battery is caused, and the further development of the lithium ion battery is hindered.
The existing commercial lithium ion battery electrolyte is a lithium hexafluorophosphate dissolved in an organic solvent, the concentration of the lithium hexafluorophosphate is about 1M, the lithium salt is not used for the transmission of lithium ions in the charging and discharging process, a CEI/SEI interface layer is formed on the interface between a positive electrode and a negative electrode and the electrolyte, and meanwhile, a small amount of lithium salt and water can generate a side reaction to generate hydrogen fluoride to carry out nucleophilic attack on a positive electrode material, so that the dissolution of transition metals is caused. For example, patent CN201710141499 adopts a high-concentration lithium salt electrolyte, the performance of the battery is improved significantly, but the increase of the lithium salt concentration also increases the viscosity of the electrolyte, reduces the conductivity and the wettability thereof at the electrode interface, and in addition, the application cost is greatly increased by the expensive lithium salt.
Disclosure of Invention
The first purpose of the invention is to overcome the defects of the prior art and provide an electrolyte for a lithium ion battery, which can relieve the dissolution of transition metals.
A second object of the present invention is to provide an electrolyte for a lithium ion battery, which can form stable CEI and SEI interfaces on positive and negative electrode surfaces.
A third object of the present invention is to provide an electrolyte for a lithium ion battery having a low viscosity, which has good wettability with a high-loading positive electrode.
The fourth purpose of the invention is to provide the electrolyte for the commercial positive electrode material lithium ion battery with low cost by reducing the addition amount of lithium salt in the existing commercial electrolyte and reducing the production cost.
The fifth object of the present invention is to provide an electrolyte for a lithium ion battery, which is applied to a lithium ion battery using a lithium nickel cobalt manganese oxide or lithium nickel cobalt aluminate, lithium cobalt oxide, lithium iron phosphate, or other commercial materials as a positive electrode.
Aiming at the technical problems that the conventional electrolyte solution is easy to react with the transition metal of the anode material to cause dissolution, the cost of the conventional modification mode is increased, and the wettability of the electrolyte and the electrode is poor, the invention makes a great deal of attempts to provide a novel electrolyte system, and the electrolyte system not only can solve the technical problems, but also can realize the purpose, and adopts the following technical scheme:
the low-concentration electrolyte for the lithium ion secondary battery comprises a lithium salt and an organic solvent, wherein the organic solvent comprises a chain carboxylic ester solvent and a fluorinated carboxylic ester solvent, and the concentration of the lithium salt is 0.01-0.5 mol/L. The inventors have surprisingly found that when a mixed solvent of a chain carboxylate solvent and a fluorocarboxylate solvent is used as a solvent system of an electrolyte, the addition of a low concentration of a lithium salt not only significantly alleviates the dissolution of a transition metal in an electrode, but also has a much lower effect on the discharge capacity of a battery than expected, and also significantly improves the cycle performance of the battery.
Research finds that the wettability of the electrolyte affects the performance of the battery, and the wettability of the electrolyte is in negative correlation with the concentration of lithium salt in the electrolyte besides being related with the components of the electrolyte; the lithium salt and the solvent react at the positive and negative electrode interfaces to generate a CEI/SEI interface which influences the electrochemical performance of the battery.
Preferably, the chain carboxylic acid ester solvent includes one or more of propylene carbonate, ethylene carbonate, diethyl carbonate, ethyl methyl carbonate and propylene carbonate.
Preferably, the fluorocarboxylic acid ester solvent is one or more selected from the group consisting of fluoropropylene carbonate, fluoroethylene carbonate and fluoroethylene carbonate.
Preferably, the volume percentage of the chain carboxylic ester solvent in the solvent is 30-90%, and more preferably 50-70%; the fluorinated carboxylic ester solvent is 10 to 70% by volume, and more preferably 30 to 50% by volume.
Preferably, the lithium salt is one or two or more selected from the group consisting of lithium hexafluorophosphate, lithium perchlorate, lithium bis (oxalato) borate, lithium difluoro (oxalato) borate and lithium tetrafluoroborate.
As one general inventive concept, there is also provided a lithium ion secondary battery including a cathode, an anode, a separator, and the aforementioned low-concentration electrolyte for a lithium ion secondary battery.
The positive electrode comprises a positive electrode current collector and a positive electrode material compounded on the surface of the positive electrode current collector, wherein the positive electrode material is obtained by curing slurry mixed by a positive electrode active material, a conductive agent, a binder and a solvent.
In the positive active material, the positive active material includes but is not limited to LiNi with a molecular formula satisfying the structural formulaxCoyMnzO2Or LiNixCoyAlzO2Ternary layered oxide, lithium cobaltate LiCoO, wherein x + y + z =12Layered oxide positive electrode material, lithium iron phosphate LiFePO4Spinel lithium manganate LiMn2O4Spinel lithium nickel manganese oxide LiMn1.5Ni0.5O4One or more combinations of materials.
The negative electrode is metal lithium or a negative electrode obtained by solidifying slurry of a negative electrode active material, a conductive agent, a binder and a solvent.
The negative active material includes, but is not limited to, one or more of graphite, mesocarbon microbeads, hard carbon, silicon, silica, tin, cobaltosic oxide, ferroferric oxide, and the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the mixed solvent of the chain carboxylic ester solvent and the fluorinated carboxylic ester solvent is used as a solvent system of the electrolyte, and 0.01-0.5 mol/L of low-concentration lithium salt is added, so that the formed electrolyte system has low viscosity and good wettability with positive and negative electrodes, can form a stable CEI/SEI layer, relieves the dissolution of transition metal in a circulation process, can reduce the production cost, and has a considerable application prospect.
(2) The lithium ion battery assembled by the electrolyte provided by the invention has stable cycle performance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention.
Fig. 1 is a graph showing the comparative cycle performance of a ternary material lithium ion battery assembled by the electrolyte provided in example 1 of the present invention and a ternary material lithium ion battery assembled by a commercial electrolyte of a comparative example.
Fig. 2 is a graph comparing the wetting performance of the electrolyte provided in example 1 of the present invention and the commercial electrolyte of the comparative example on a high loading ternary positive electrode material.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
The lithium ion battery electrolyte consists of lithium hexafluorophosphate, fluoroethylene carbonate and dimethyl carbonate serving as solvents, wherein the volume ratio of the fluoroethylene carbonate to the dimethyl carbonate in the electrolyte is 1:1, and the concentration of the lithium hexafluorophosphate is 0.4 mol/L.
A lithium ion button cell is prepared by the following method:
(1) electrolyte preparation: in a glove box under argon atmosphere (H)2O＜0.1ppm，O2Less than 0.1 ppm), uniformly mixing fluoroethylene carbonate with dimethyl carbonate in the same volume, adding lithium hexafluorophosphate to ensure that the concentration of the electrolyte is 0.4mol per liter, and stirring until the electrolyte is dissolved to obtain the electrolyte.
(2) Preparation of the positive electrode: reacting LiNi0.8Co0.1Mn0.1O2Mixing acetylene black and PVDF according to a ratio of 8:1:1, adding a proper amount of N-methyl pyrrolidone, mixing to obtain uniform anode slurry with stable components, coating the slurry on an aluminum foil, and drying in a vacuum oven at 120 ℃ until the N-methyl pyrrolidone is completely volatilized.
(3) Assembling the button cell: and punching the prepared positive electrode into a circular sheet with the diameter of 12mm, and assembling the circular sheet into a button cell by taking a metal lithium sheet as a negative electrode and Celgard2500 as a diaphragm in an argon atmosphere glove box. And standing the prepared battery at room temperature for 6 hours, and then carrying out charge-discharge cycle test on the battery in a blue electricity testing system under the test conditions of constant current charge-discharge, current of 1C and charge-discharge interval of 2.8-4.3V, and circulating for 100 times.
Comparative examples 1 to 3
Compared with example 1, the difference is only in the electrolyte composition, and the electrolyte composition of each comparative example is shown in table 1. The cell of this comparative example was prepared in the same manner as in example 1.
TABLE 1 electrolyte composition for lithium ion batteries of comparative examples 1 to 3
Examples 2 to 8
Examples 2 to 8 differ from example 1 only in the electrolyte composition, and the electrolyte composition formulations in examples 2 to 8 are shown in table 2. The method for preparing the batteries of examples 2-8 is the same as that of example 1.
TABLE 2 electrolyte Components for lithium ion batteries of examples 2 to 8
Electrochemical tests are carried out on the button cells assembled by the electrolytes in examples 1-9 and comparative examples 1-3, the obtained electrochemical performance parameters are listed in table 3, the cycle performance of the button cells assembled by the electrolytes in example 1 and comparative example 1 is shown in figure 1, and as can be seen from figure 1, the cycle performance of the cells assembled by the electrolytes in example 1 is obviously improved.
TABLE 3 results of electrochemical tests of examples 1 to 9 and comparative examples 1 to 3
It can be known from the data in table 3 and fig. 1 that the lithium ion battery prepared by using the electrolyte of the present invention can greatly improve the cycle stability of the battery although the capacity of the battery decreases by 2 to 5 ma hour/g due to the decrease of the ionic conductivity, and the electrolyte of the present invention can better meet the requirement of people on the long cycle life of the lithium ion battery.
In order to investigate the influence of the electrolyte of the present invention on the dissolution process of transition metal ions, the electrode plates in each charged state were immersed in the electrolytes of examples and comparative examples for 28 days, respectively, and the influence of the electrolyte on the dissolution of transition metals was determined by detecting the content of transition metal ions in the electrolyte, and the specific test results are listed in table 4.
TABLE 4 transition Metal dissolution test results for examples 1-4 and comparative examples 1-3
Analysis of the content of the transition metal dissolved in the electrolyte in table 4 shows that the electrolyte in each example can effectively alleviate the problem of dissolution of the transition metal ions.
When the electrolyte of example 1 and the electrolyte of comparative example 1 were subjected to a contact angle test, images of contact with a commercial pole piece were obtained by a computer at the same time and the contact angle was calculated, as shown in fig. 2, it can be seen from fig. 2 that the contact angle of the electrolyte of the present invention was significantly increased compared to the existing commercial electrolyte, indicating that the wettability of the electrolyte to the electrode was significantly improved.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (6)
1. The low-concentration electrolyte for the lithium ion secondary battery comprises a lithium salt and an organic solvent, and is characterized in that the organic solvent comprises a chain carbonate solvent and a fluoro carbonate solvent, and the concentration of the lithium salt is 0.01-0.4 mol/L; the chain carbonate solvent comprises one or two of diethyl carbonate and methyl ethyl carbonate; the fluorinated carbonate solvent is one or more than two of fluorinated propylene carbonate, fluorinated ethylene carbonate, fluorinated diethyl carbonate and fluorinated ethyl methyl carbonate; the lithium salt is selected from any one of lithium hexafluorophosphate, lithium perchlorate, lithium bis (oxalate) borate, lithium difluoro (oxalate) borate and lithium tetrafluoroborate.
2. The low-concentration electrolyte solution for a lithium-ion secondary battery according to claim 1, wherein the solvent contains 30 to 90% by volume of the chain carbonate solvent and 10 to 70% by volume of the fluoro carbonate solvent.
3. A lithium ion secondary battery comprising a positive electrode, a negative electrode, a separator and the low-concentration electrolyte solution for lithium ion secondary batteries according to any one of claims 1 to 2.
4. The lithium ion secondary battery according to claim 3, wherein the active material of the positive electrode is selected from one or more of lithium nickel cobalt manganese oxide, lithium nickel cobalt aluminate, lithium cobalt oxide, and lithium iron phosphate.
5. The lithium ion secondary battery according to claim 3, wherein the negative electrode is metallic lithium or a negative electrode obtained by curing a slurry of a negative electrode active material, a conductive agent, a binder, and a solvent.
6. The lithium ion secondary battery of claim 5, wherein the negative active material is selected from one or more combinations of graphite, mesocarbon microbeads, hard carbon, silicon, silica, tin, tricobalt tetroxide, and triiron tetroxide.
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