CN108987810B - Electrolyte and secondary lithium battery suitable for high-temperature environment - Google Patents

Electrolyte and secondary lithium battery suitable for high-temperature environment Download PDF

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CN108987810B
CN108987810B CN201810578742.0A CN201810578742A CN108987810B CN 108987810 B CN108987810 B CN 108987810B CN 201810578742 A CN201810578742 A CN 201810578742A CN 108987810 B CN108987810 B CN 108987810B
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lithium
electrolyte
lithium salt
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salt
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CN108987810A (en
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耿振
李泓
黄杰
李文俊
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Institute of Physics of CAS
Beijing WeLion New Energy Technology Co ltd
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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
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/058—Construction or manufacture
    • 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
    • H01M2300/004—Three solvents
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention provides an electrolyte and a secondary lithium battery suitable for a high-temperature environment, wherein the electrolyte comprises a lithium salt and an organic solvent, and the electrolyte is characterized in that the lithium salt is composed of two or three of a first lithium salt, a second lithium salt and a third lithium salt, wherein the first lithium salt is fluorine-containing lithium sulfonate or fluorine-containing lithium sulfonyl, the second lithium salt is boric acid lithium, the third lithium salt is a lithium salt which passivates an aluminum current collector and has strong L ewis acidity, and the organic solvent is composed of 1-3 of the first solvent, the second solvent and the third solvent.

Description

Electrolyte and secondary lithium battery suitable for high-temperature environment
Technical Field
The invention belongs to the technical field of materials, and particularly relates to an electrolyte suitable for a high-temperature environment and application thereof in a high-energy-density secondary lithium battery.
Background
The secondary lithium battery is an important electrochemical energy storage device, and has wide application prospects in the fields of consumer electronics, power batteries, industrial energy storage and the like. In the face of increasing market demand, the performance of lithium batteries is in need of further improvement.
Electrolyte improvement and optimization for lithiumThe electrolyte of the lithium ion battery for commercial use at present is mainly composed of lithium salt (L iPF)6) And organic solvents (ethylene carbonate (EC), dimethyl carbonate (DMC), diethyl carbonate (DEC)), but the current electrolyte systems suffer mainly from the following problems (1) L iPF6Has poor thermal stability and can be decomposed to form PF with extremely strong L ewis acidity5In the presence of trace water, the electrolyte can decompose to form HF, corrode electrode materials, current collectors and battery cases, and cause the performance deterioration of the battery (Nature Energy 2(2017)17108-6The SEI film formed by the decomposition of the electrolyte on the surface of the high-capacity negative electrode (such as a silicon negative electrode and a lithium metal surface) has poor stability, the SEI film breaks to cause the negative electrode material to contact with the electrolyte and generate side reactions continuously, which causes the reduction of the coulombic efficiency of the battery and the generation of lithium dendrites, and further causes the deterioration of the battery performance (Adv. Sci.3(2016)1500213-6Lithium batteries with electrolytes have poor performance at high temperatures. The current commercial electrolytes do not meet the requirements of high temperature applications.
Disclosure of Invention
Therefore, the present invention aims to overcome the defect that the current commercial electrolyte has poor thermal stability and cannot meet the requirement of high temperature application of a lithium battery, provide an electrolyte which can be suitable for a high temperature environment and can stabilize a high capacity negative electrode, and apply the electrolyte to a high energy density secondary lithium battery to improve the performance of the battery in the high temperature environment.
In the present invention, the "high temperature environment" refers to a so-called high temperature environment in the field of secondary lithium batteries, and generally refers to an environment of 55 ℃ or higher, for example, an environment of 55 to 80 ℃.
The invention provides an electrolyte suitable for a high-temperature environment, which comprises a lithium salt and an organic solvent, wherein the lithium salt is composed of two or three of a first lithium salt, a second lithium salt and a third lithium salt, the first lithium salt is fluorine-containing lithium sulfonate or fluorine-containing lithium sulfonyl, the second lithium salt is lithium borate, and the third lithium salt is a lithium salt which passivates an aluminum current collector and has strong L ewis acidity.
According to the electrolyte provided by the invention, the molar concentration of the first lithium salt can be 0.01-8 mol/l. The molar concentration of the second lithium salt may be 0.01 to 3 mol/l. The molar concentration of the third lithium salt may be 0.01 to 1 mol/l.
According to the electrolyte provided by the present invention, preferably, the lithium salt is composed of a first lithium salt, a second lithium salt and a third lithium salt.
The electrolyte provided by the invention is characterized in that the first lithium salt is bis (trifluoromethylsulfonyl) imide lithium (L iTFSI), bis (fluorosulfonyl) imide lithium (L iFSI) and lithium (L iCF) trifluoromethanesulfonate3SO3) And lithium bis (perfluoroethylsulfonyl) imide (L iBETI), wherein the second lithium salt is lithium bis (oxalato) borate (L iBOB), lithium difluoro (oxalato) borate (L iDFOB), lithium tetrafluoroborate (L iBF)4) And the third lithium salt is lithium hexafluorophosphate (L iPF)6) Lithium perchlorate (L iClO)4) And lithium hexafluoroarsenate (L iAsF)6) One or more of (a).
According to the technical scheme, the first lithium salt is used as a main salt to improve the overall thermal stability of the electrolyte, the second lithium salt is used for relieving corrosion of the second lithium salt on a current collector, meanwhile, the borate participates in the construction of an SEI film to improve the stability of the SEI film, and the third lithium salt is used as an auxiliary salt to inhibit corrosion of the main salt on a battery, has strong L ewis acidity and can catalyze organic solvent crosslinking polymerization.
According to the electrolyte provided by the invention, 1-3 of a first solvent, a second solvent and a third solvent are preferably used as the organic solvent, wherein the first solvent is one or more of Ethylene Carbonate (EC), Propylene Carbonate (PC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC), the second solvent is one or more of fluoroethylene carbonate (FEC), diethyl fluoro carbonate (FDEC) and perfluoroether (HFE), and the third solvent is one or more of Vinylene Carbonate (VC), Ethylene Sulfite (ES), ethylene carbonate (VEC) and 1, 3-dioxolane (DO L).
Preferably, the organic solvent consists of a first solvent, a second solvent and an optional third solvent, wherein the proportion of the first solvent, the second solvent and the third solvent is 1:1: 0-8 vol%.
According to the electrolyte provided by the invention, the organic solvent is high in thermal stability and can be crosslinked, the selected organic solvent has the effects of participating in the construction of a high-stability SEI film, improving the thermal stability of the electrolyte by utilizing the good stability of the organic solvent, and in addition, the crosslinkable solvent can carry out polymerization reaction at the temperature of 25-80 ℃ under the acid action of L ewis of lithium salt, so that a gel-state electrolyte is formed in situ, wherein the polymerization temperature can be 25-80 ℃, and the polymerization time can be 12-48 h.
The invention also provides a secondary lithium battery, which comprises a battery shell, an electrode group and electrolyte, wherein the electrode group and the electrolyte are sealed in the battery shell, the electrode group comprises a positive electrode, a diaphragm and a negative electrode, and the electrolyte is the electrolyte suitable for high-temperature environment provided by the invention.
The invention provides a secondary lithium battery, wherein the cathode material used for the cathode comprises polyanion cathode material with an orthogonal structure, such as L iFePO4Oxide-based positive electrodes of layered structure, e.g. L iCoO2Nickel cobalt manganese ternary (NCM), Nickel Cobalt Aluminium (NCA), lithium rich manganese based positive electrode materials, spinel structured materials, e.g. L iMn2O4And L iNi0.5Mn1.5O4。
According to the present invention, there is provided a secondary lithium battery, wherein a negative electrode material for a negative electrode includes: the composite cathode material comprises a carbon-based cathode material, a silicon-based cathode material, an oxide-based cathode material, lithium titanate and a composite cathode material containing metal lithium.
According to the invention, by utilizing the synergistic effect between the lithium salt and the solvent, the SEI with an organic-inorganic composite structure is constructed on the negative electrode side, so that the volume expansion of the negative electrode and the generation of lithium dendrites are effectively inhibited, particularly the silicon negative electrode and the metal lithium negative electrode are combined with the good thermal stability of the electrolyte, and thus, a battery using the electrolyte shows good performance in a high-temperature environment. The electrolyte and the lithium battery thereof can be applied to the fields of consumer electronics, power batteries, industrial energy storage, military, national defense and the like, and are not limited to the fields.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 shows an electrolyte prepared by using the electrolyte of example 8 of the present invention and a commercial product L iPF6A comparison graph of the high-temperature cycle performance of the battery of the electrolyte;
FIG. 2 shows an electrolyte prepared by using the electrolyte of example 8 of the present invention and a commercial product L iPF6And comparing the appearance of the lithium metal cathode after battery circulation of the electrolyte.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
Sequentially adding Propylene Carbonate (PC) and fluoroethylene carbonate (FEC) according to the volume ratio of 1:1, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing lithium bis (trifluoromethylsulfonyl) imide (L iTFSI), lithium difluorooxalato borate (L iDFOB) and lithium hexafluoroarsenate (L iAsF)6) The electrolyte with the concentration of 8mol/l, 3mol/l and 1mol/l respectively is continuously stirred for 24 hours and then transferred into an aluminum packaging bottle filled with inert gas for storage.
Example 2
Adding fluoroethylene carbonate (FEC) and diethyl Fluorocarbonate (FDEC) in sequence according to the volume ratio of 1:1, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing lithium bis (fluorosulfonyl) imide (L iFSI), lithium bis (oxalato) borate (L iBOB) and lithium hexafluoroarsenate (L iAsF)6) The electrolyte with the concentration of 8mol/l, 0.01mol/l and 1mol/l respectively is continuously stirred for 24 hours and then transferred into an aluminum packaging bottle filled with inert gas for storage.
Example 3
Sequentially adding Propylene Carbonate (PC), Ethylene Carbonate (EC) and Ethylene Sulfite (ES) according to the volume ratio of 1:1:1, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing lithium bis (trifluoromethylsulfonyl) imide (L iTFSI), lithium difluorooxalato borate (L iDFOB) and lithium hexafluorophosphate (L iPF)6) The electrolyte with the concentration of 8mol/l, 3mol/l and 0.01mol/l respectively is continuously stirred for 24 hours and then transferred into an aluminum packaging bottle filled with inert gas for storage.
Example 4
Sequentially adding Propylene Carbonate (PC) and Ethylene Carbonate (EC) according to the volume ratio of 1:1, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing lithium bis (fluorosulfonyl) imide (L iFSI), lithium difluoro (L iDFOB) oxalate and lithium perchlorate (L iClO)4) The electrolyte with the concentration of 8mol/l, 0.01mol/l and 1mol/l is continuously stirred for 24 hours and then transferred into an aluminum packaging bottle filled with inert gas for storage.
Example 5
Sequentially adding Propylene Carbonate (PC) and Ethylene Carbonate (EC) according to the volume ratio of 1:1, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing lithium bis (trifluoromethylsulfonyl) imide (L iTFSI) and lithium tetrafluoroborate (L iBF)4) And lithium perchlorate (L iClO)4) The electrolyte with the concentration of 0.01mol/l, 3mol/l and 0.01mol/l respectively is continuously stirred for 24 hours and then transferred into an aluminum packaging bottle filled with inert gas for storage.
Example 6
Sequentially adding Propylene Carbonate (PC) and Ethylene Carbonate (EC) according to the volume ratio of 1:1, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing the lithium bis (fluorosulfonyl) imide (L iFSI) and the lithium tetrafluoroborate (L iBF)4) And lithium perchlorate (L iClO)4) The electrolyte with the concentration of 0.01mol/l, 3mol/l and 1mol/l respectively is continuously stirred for 24 hours and then transferred into an aluminum packaging bottle filled with inert gas for storage.
Example 7
Sequentially adding Propylene Carbonate (PC) and Ethylene Carbonate (EC) according to the volume ratio of 1:1, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing the bis (trifluoromethyl)Sulfonyl) imide lithium (L iTFSI), lithium bis (oxalato) borate (L iBOB) and lithium perchlorate (L iClO)4) The electrolyte with the concentration of 0.6mol/l, 0.4mol/l and 0.1mol/l respectively is continuously stirred for 24 hours and then transferred into an aluminum packaging bottle filled with inert gas for storage.
Example 8
Sequentially adding Propylene Carbonate (PC) and Ethylene Carbonate (EC) according to the volume ratio of 1:1, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing lithium bis (trifluoromethylsulfonyl) imide (L iTFSI), lithium difluorooxalato borate (L iDFOB) and lithium hexafluorophosphate (L iPF)6) The electrolyte with the concentration of 0.8mol/l, 0.2mol/l and 0.01mol/l respectively is continuously stirred for 24 hours and then transferred into an aluminum packaging bottle filled with inert gas for storage.
The surface capacity is 2.5mAh/cm2L iCoO of2As a positive electrode and lithium metal as a negative electrode, a button cell was assembled using the electrolyte solutions of the 8 examples, and the current density was 1.2mA/cm in an environment of 80 deg.C2The cyclability test was carried out under the conditions shown in Table 1. FIG. 1 shows the use of the electrolyte prepared in example 8 with a commercial L iPF6Comparative battery performance of the electrolyte. As shown in table 1 and fig. 1, the electrolyte prepared by the present invention was effective in improving the high-temperature cycle performance of the battery.
FIG. 2 shows the electrolyte prepared using example 8 and commercial L iPF6The appearance of the lithium metal cathode after the battery of the electrolyte is circulated is obviously shown, and the electrode solution prepared by the method has the effect of effectively inhibiting lithium dendrites.
TABLE 1
Figure BDA0001687844730000061
Example 9
Sequentially adding Propylene Carbonate (PC), Ethylene Carbonate (EC) and 1, 3-dioxolane (DO L) according to the volume ratio of 1:1:8, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing lithium bis (trifluoromethylsulfonyl) imide (L iTFSI), lithium difluorooxalato borate (L iDFOB) and lithium perchlorate (L iClO)4) The concentrations of the electrolyte are 1mol/l, 1mol/l and 0.2mol/l respectivelyAnd (5) continuously stirring the solution for 24 hours, and then transferring the solution into a packaging bottle filled with inert gas for sealed storage. The surface capacity is 2.5mAh/cm2L iCoO of2The button cell was assembled by injecting the electrolyte solution into a positive electrode and a negative electrode made of lithium metal. The cell was allowed to stand at 25 ℃ for 48h and then cooled to room temperature.
Example 10
Adding fluoroethylene carbonate (FEC), Ethylene Carbonate (EC) and 1, 3-dioxolane (DO L) in a volume ratio of 1:1:4 in sequence, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing lithium bis (trifluoromethylsulfonyl) imide (L iTFSI), lithium difluorooxalato borate (L iDFOB) and lithium perchlorate (L iClO)4) The electrolyte with the concentration of 2mol/l, 0.5mol/l and 0.1mol/l respectively is continuously stirred for 24 hours and then is transferred into a packaging bottle filled with inert gas for sealed storage. The surface capacity is 2.5mAh/cm2L iCoO of2The button cell was assembled by injecting the electrolyte solution into a positive electrode and a negative electrode made of lithium metal. The cell was allowed to stand at 40 ℃ for 24h and then cooled to room temperature.
Example 11
Adding fluoroethylene carbonate (FEC), diethyl Fluorocarbonate (FDEC) and 1, 3-dioxolane (DO L) in a volume ratio of 1:1:2 in sequence, slowly adding lithium salt when the temperature is reduced to about 25 ℃, and preparing lithium bis (trifluoromethylsulfonyl) imide (L iTFSI), lithium difluorooxalato borate (L iDFOB) and lithium hexafluoroarsenate (L iAsF)6) The electrolyte with the concentration of 0.5mol/l, 2mol/l and 0.3mol/l respectively is continuously stirred for 24 hours and then is transferred into a packaging bottle filled with inert gas for sealed storage. The surface capacity is 2.5mAh/cm2L iCoO of2The button cell was assembled by injecting the electrolyte solution into a positive electrode and a negative electrode made of lithium metal. The cell was allowed to stand at 80 ℃ for 12h and then cooled to room temperature.
The electrolyte of the embodiment 9-11 is injected into a battery, the battery is kept stand for 12-48 hours at a certain temperature (25-80 ℃), the solvent with polymerization property can generate cross-linking polymerization reaction under the action of strong L ewis acidic lithium salt, and the liquid electrolyte is converted into gel electrolyte in situ in the battery, and the 80 ℃ cyclic test shows that the battery using the electrolyte has high initial capacity which is 2.1～2.5mAh/cm2Meanwhile, the composite material has good circulation stability, and the capacity retention rate is 85-95% after 100-week circulation.
The invention has various specific embodiments, and all technical solutions produced by adopting equivalents or equivalent substitutions are within the protection scope of the invention.

Claims (5)

1. The electrolyte is suitable for a high-temperature environment and comprises a lithium salt and an organic solvent, and is characterized in that the lithium salt is composed of a first lithium salt, a second lithium salt and a third lithium salt, wherein the first lithium salt is fluorine-containing lithium sulfonate or fluorine-containing lithium sulfonyl, the second lithium salt is lithium borate, the third lithium salt is a lithium salt which passivates an aluminum current collector and has strong L ewis acidity, the organic solvent is composed of a first solvent, a second solvent and an optional third solvent, the first solvent is one or more of ethylene carbonate, propylene carbonate, diethyl carbonate and ethyl methyl carbonate, the second solvent is one or more of fluoroethylene carbonate, diethyl fluoro carbonate and perfluoro ether, and the third solvent is one or more of vinylene carbonate, ethylene sulfite, ethylene carbonate and 1, 3-dioxolane.
2. The electrolyte of claim 1, wherein the first lithium salt has a molar concentration of 0.01 to 8 mol/l; the molar concentration of the second lithium salt is 0.01-3 mol/l; the molar concentration of the third lithium salt is 0.01-1 mol/l.
3. The electrolyte of claim 1 or 2, wherein the first lithium salt is one or more of lithium bis (trifluoromethylsulfonyl) imide, lithium bis (fluorosulfonyl) imide, lithium trifluoromethylsulfonate, and lithium bis (perfluoroethylsulfonyl) imide; the second lithium salt is one or more of lithium bis (oxalate) borate, lithium difluoro (oxalate) borate and lithium tetrafluoroborate; the third lithium salt is one or more of lithium hexafluorophosphate, lithium perchlorate and lithium hexafluoroarsenate.
4. The electrolyte of claim 1, wherein the first, second, and third solvents are present in a ratio ranging from 1:1:0 to 8 vol%.
5. A secondary lithium battery comprising a battery case, an electrode group and an electrolyte sealed in the battery case, the electrode group comprising a positive electrode, a separator and a negative electrode, wherein the electrolyte is the electrolyte suitable for a high temperature environment according to any one of claims 1 to 4.
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