CN112117492A - Organic ester electrolyte additive, electrolyte containing additive, lithium metal battery and application - Google Patents
Organic ester electrolyte additive, electrolyte containing additive, lithium metal battery and application Download PDFInfo
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- CN112117492A CN112117492A CN202011109254.9A CN202011109254A CN112117492A CN 112117492 A CN112117492 A CN 112117492A CN 202011109254 A CN202011109254 A CN 202011109254A CN 112117492 A CN112117492 A CN 112117492A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses an organic ester electrolyte additive, an electrolyte containing the additive, a lithium metal battery and application of the additive. The electrolyte comprises electrolyte lithium salt, a non-aqueous organic solvent and the additive, the concentration of the additive is 1% -50%, and the lithium metal battery comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte. The invention adds a certain amount of organic ester electrolyte additives on the basis of the traditional lithium ion battery electrolyte to improve the cycling stability of the battery in the charging and discharging process and inhibit the generation of lithium dendrites in the cycling process of the lithium metal battery, thereby improving the safety of the lithium metal battery.
Description
Technical Field
The invention belongs to the technical field of lithium metal batteries, and particularly relates to an organic ester electrolyte additive, an electrolyte containing the additive, a lithium metal battery and application of the additive.
Background
The rapid development of electric vehicles and power grids puts higher demands on battery energy storage systems. The ultra-high theoretical specific capacity (3860mA · h/g) and the extremely low negative potential (-3.04V vs. standard hydrogen electrode) of lithium metal are "holy cup" electrodes among all potential anode materials of next generation high energy density rechargeable Lithium Ion Batteries (LIBs). However, problems such as severe corrosion of liquid electrolytes, non-uniform lithium deposition, huge volume expansion, and unstable solid electrolyte interfacial film (SEI) often cause instability of lithium metal anodes, thereby hindering practical applications thereof. Wherein, the uneven deposition of lithium can cause the generation of moss-shaped or dendritic lithium, and the growth of lithium dendrites can cause the internal short circuit of the battery, thereby possibly leading to thermal runaway and causing the risk of potential ignition and explosion. Therefore, it is necessary to develop a series of strategies for protecting the lithium metal anode to inhibit the growth of lithium dendrites during the cycling of the lithium metal battery, thereby improving the cycle life and safety performance of the lithium metal battery.
Over the last several decades, a number of new strategies have been developed to inhibit dendritic growth of metallic lithium negative electrodes, such as designing alloying structures, employing electrolyte additives, using solid-state electrolytes, and negative electrode structural designs of metallic lithium. Since the modification of the electrolyte does not require a great change in the electrode and battery manufacturing processes, and is economically feasible, a great deal of research work is being conducted on the electrolyte to find the optimum electrolyte composition. Such as Vinylene Carbonate (VC), fluoroethylene carbonate (FEC), and Ethylene Sulfite (ES), which have been used in lithium ion batteries. These conventional additives, which have been applied in lithium ion battery electrolytes, have been transferred to rechargeable lithium metal batteries having intercalation-type cathodes, in hopes of maintaining the beneficial properties exhibited in lithium ion batteries. In addition, zwitterionic compounds, lithium halide salts, surfactants, ionic liquids, and the like have also been used in lithium metal battery electrolytes. For this reason, screening and testing of electrolyte additives are still the most sought after efforts by researchers, and their effects mainly include stabilizing lithium metal anodes and increasing discharge capacity. Therefore, in order to overcome the dilemma of the rechargeable lithium metal battery as described above, a great effort in the electrolyte additive is necessary.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an organic ester electrolyte additive, an electrolyte containing the additive, a lithium metal battery and application.
The invention is realized by the following technical scheme:
the organic ester electrolyte additive is one or more of tetraethyl titanate, tetrabutyl titanate, tetraisopropyl titanate and tetraethyl silicate.
The electrolyte comprises electrolyte lithium salt, a non-aqueous organic solvent and the organic ester electrolyte additive.
Preferably, the concentration of the organic ester electrolyte additive in the electrolyte is 1-50%.
Preferably, the electrolyte lithium salt is one or more of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium trifluorochloroborate, lithium tetracyanoborate, lithium difluorooxalato borate, lithium dioxalate borate, lithium difluorosulfate borate, lithium difluorosulfonimide, lithium trifluoromethylsulfonimide and lithium fluoroalkyl phosphonate.
Preferably, the concentration of the electrolyte lithium salt in the electrolyte is 0.8-1.5 mol/L.
Preferably, the non-aqueous organic solvent is a mixed solvent of a cyclic organic solvent and a chain organic solvent.
Preferably, the cyclic organic solvent is one of ethylene carbonate, propylene carbonate and butylene carbonate, and the chain organic solvent is one or two of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate and ethyl acetate.
Preferably, the volume content of the cyclic organic solvent accounts for 25-50% of the total volume of the electrolyte.
A lithium metal battery comprises a metal lithium anode, a metal lithium cathode, a battery diaphragm and the electrolyte.
An application of organic ester electrolyte additive in preparing lithium metal battery.
The invention has the following beneficial effects:
1. according to the invention, the organic ester electrolyte additive is introduced into the lithium metal battery electrolyte, and a stable SEI film can be formed in the circulation process, so that the uniform deposition of lithium ions is realized, the lithium metal anode is protected, and the cycle life of the lithium metal battery is prolonged.
2. The organic ester electrolyte additive introduced by the invention can be used as a catalyst for ester exchange reaction, can enhance the adhesion of rubber and plastics on the metal surface, and a hydrolysate can be used for optical coating. Therefore, the electrolyte has strong feasibility when being applied to the electrolyte of the lithium metal battery.
Drawings
FIG. 1(a) shows a lithium symmetric cell assembled using the electrolyte prepared in comparative example 1 at 2mA/cm2Current density of 1mA · h/cm2Time-voltage graph of 140h cycle at fixed capacity;
FIG. 1(b) shows the electrolyte prepared in comparative example 1 at 2mA/cm for an assembled lithium symmetric cell2Current density of 1mA · h/cm2Time-voltage plots for the 55 th to 60 th of the cycle at fixed capacity of (a);
FIG. 2(a) shows the electrolyte prepared in example 1 at 2mA/cm for a lithium symmetric battery2Current density of 1mA · h/cm2Time-voltage graph of 140h cycle at fixed capacity;
FIG. 2(b) shows the electrolyte prepared in example 1 at 2mA/cm for a lithium symmetric battery2Current density of 1mA · h/cm2Time-voltage plots for the 55 th to 60 th of the cycle at fixed capacity of (a);
FIG. 3 shows the electrolyte prepared in comparative example 1 at 2mA/cm for a lithium symmetric cell2Current density of 1mA · h/cm2Electron microscopy images of the surface of the lithium metal anode after 50 weeks of cycling at fixed capacity of (a);
FIG. 4 shows an electrolyte prepared in example 1The assembled lithium symmetric battery is at 2mA/cm2Current density of 1mA · h/cm2Electron microscopy images of the surface of the lithium metal anode after 50 weeks of cycling at fixed capacity of (a);
FIG. 5(a) shows the electrolyte prepared in comparative example 2 at 2mA/cm for a lithium symmetric cell assembled with the electrolyte2Current density of 1mA · h/cm2Time-voltage graph of cycle 120h at fixed capacity;
FIG. 5(b) shows the electrolyte prepared in comparative example 2 at 2mA/cm for an assembled lithium symmetric cell2Current density of 1mA · h/cm2Time-voltage graph of 50 th to 55 th of cycle at fixed capacity of
FIG. 6(a) shows the electrolyte prepared in example 2 at 2mA/cm for a lithium symmetric battery2Current density of 1mA · h/cm2Time-voltage graph of cycle 120h at fixed capacity;
FIG. 6(b) shows the electrolyte prepared in example 2 at 2mA/cm for a lithium symmetric battery2Current density of 1mA · h/cm2Time-voltage plots of 50 th to 55 th of the cycle at a fixed capacity.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples. The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention. In the following examples, unless otherwise specified, the starting materials and reagents used were commercially available in analytical purity and above.
An organic ester electrolyte additive, wherein the organic ester is one or more of tetraethyl titanate (IV), tetrabutyl titanate (TBT), tetraisopropyl titanate and tetraethyl silicate (TEOS).
The electrolyte comprises electrolyte lithium salt, a non-aqueous organic solvent and the electrolyte additive, wherein the concentration of the electrolyte additive in the electrolyte is 1-50%.
In a preferred embodiment, the electrolyte lithium salt is lithium hexafluorophosphate (LiPF)6) Lithium tetrafluoroborate (LiBF)4) Lithium trifluoroborate (LiBF)3Cl), tetracyanoboronLithium (LiB (CN)4) Lithium difluorooxalato borate (LiDFOB), lithium dioxalate borate (LiBOB), lithium difluorosulfatato borate (LiBF)2SO4) One or more of lithium bis (fluorosulfonyl) imide (LiFSI), lithium trifluoromethyl sulfonyl imide (LiTFSI) and lithium fluoroalkyl phosphonate (LiFAP), wherein the concentration of the electrolyte lithium salt in the electrolyte is 0.8-1.5 mol/L.
In a preferred embodiment, the nonaqueous organic solvent is a mixed solvent of a cyclic organic solvent and a chain organic solvent. Wherein the annular organic solvent is one of Ethylene Carbonate (EC), Propylene Carbonate (PC) and Butylene Carbonate (BC), and the volume content of the annular organic solvent accounts for 25-50% of the total volume of the electrolyte. The chain-like organic solvent is one or two of dimethyl carbonate (DMC), diethyl carbonate (DEC), Ethyl Methyl Carbonate (EMC) and Ethyl Acetate (EA).
Example 1
The specific preparation method of the electrolyte comprises the following steps:
in an argon-filled glove box, lithium hexafluorophosphate (LiPF) was added6) Dissolving in ethylene carbonate by volume ratio: dimethyl carbonate: and (2) in a non-aqueous organic solvent mixed by ethyl methyl carbonate (1: 1: 1), adding tetraethyl titanate (IV) into the nonaqueous organic solvent with the final concentration of lithium hexafluorophosphate being 1mol/L, wherein the concentration of IV in the electrolyte is 5%, stirring, mixing and dissolving, and drying all reagents used in preparation in a glove box for more than 12 hours to prepare the electrolyte.
Comparative example 1
The specific preparation method of the electrolyte comprises the following steps:
in an argon-filled glove box, lithium hexafluorophosphate (LiPF) was added6) Dissolving in ethylene carbonate by volume ratio: dimethyl carbonate: and (2) in a non-aqueous organic solvent mixed by ethyl methyl carbonate (1: 1: 1), stirring and mixing lithium hexafluorophosphate with the final concentration of 1mol/L without using an additive, and drying all reagents used in preparation in a glove box for more than 12 hours to prepare the electrolyte.
Test example 1
Assembling the lithium-lithium symmetrical battery: the assembly of the battery is carried out in a glove box filled with argon protective atmosphere, a pair of metal lithium sheets are used as electrodes to assemble the battery, then the electrolyte prepared in the example 1 and the electrolyte prepared in the comparative example 1 are respectively injected into the battery, and the battery is packaged by a packaging machine, namely the assembly of the lithium-lithium symmetrical battery is completed.
The electrochemical test of the lithium-lithium symmetric battery of the test example is carried out on a LAND test system, and the test temperature is kept constant at 25 ℃.
Testing the room-temperature electrochemical cycle performance: the cell was left standing at room temperature (25 ℃ C.) for 24 hours at 2mA/cm2Constant current charge and discharge tests were performed at the current density of (1). The results are shown in FIG. 1: the electrolyte prepared in comparative example 1 was used at 2mA/cm2At a current density of (a), it was found that the polarization voltage started to increase after 20 hours of cycling and the cell had been damaged after 30 hours of cycling. In contrast, the electrolyte prepared in example 1 was used at 2mA/cm2The time-voltage curve of the lithium metal battery is still stable after 140h of circulation under the current density, as shown in fig. 2, which shows that the addition of 5% of IV has a good effect of improving the circulation stability of the lithium metal battery.
FIG. 3 shows the electrolyte prepared in comparative example 1 at 2mA/cm for a lithium symmetric cell2Current density of 1mA · h/cm2At a fixed capacity of (a) and after 50 weeks of cycling. It is apparent from its morphology that the lithium metal surface produces a large number of dendrites that ultimately lead to battery failure or damage.
FIG. 4 shows the electrolyte prepared in example 1 at 2mA/cm for a lithium symmetric cell2Current density of 1mA · h/cm2At a fixed capacity of (a) and after 50 weeks of cycling. The appearance of the lithium metal battery shows that the surface of the lithium metal battery is relatively flat, which indicates that the tetraethyl titanate additive has a certain effect of inhibiting the generation of lithium dendrites, and finally the cycle life of the lithium metal battery is prolonged.
Example 2
The specific preparation method of the electrolyte comprises the following steps:
in an argon-filled glove box, lithium hexafluorophosphate (LiPF) was added6) Dissolving in propylene carbonate according to volume ratio: diethyl carbonate: dimethyl carbonate 1:1:1 mixtureAnd (3) in the mixed non-aqueous organic solvent, the final concentration of lithium hexafluorophosphate is 1mol/L, then tetraethyl silicate (TEOS) is added into the mixed non-aqueous organic solvent, the concentration of TEOS in the electrolyte is 5%, the lithium hexafluorophosphate and the TEOS are stirred, mixed and dissolved, and all reagents used in preparation are dried in a glove box for more than 12 hours to prepare the electrolyte.
Comparative example 2
The specific preparation method of the electrolyte comprises the following steps:
in an argon-filled glove box, lithium hexafluorophosphate (LiPF) was added6) Dissolving in propylene carbonate according to volume ratio: diethyl carbonate: and (2) in a non-aqueous organic solvent mixed with dimethyl carbonate in a ratio of 1:1:1, wherein the final concentration of lithium hexafluorophosphate is 1mol/L, no additive is used, the mixture is stirred and mixed, and all reagents used in preparation are dried in a glove box for more than 12 hours to prepare the electrolyte.
Test example 2
Assembling the lithium-lithium symmetrical battery: the assembly of the battery is carried out in a glove box filled with argon protective atmosphere, a pair of metal lithium sheets are used as electrodes to assemble the battery, then the electrolyte prepared in the example 2 and the electrolyte prepared in the comparative example 2 are respectively injected into the battery, and the battery is packaged by a packaging machine, namely the assembly of the lithium-lithium symmetrical battery is completed.
The electrochemical test of the lithium-lithium symmetric battery of the test example is carried out on a LAND test system, and the test temperature is kept constant at 25 ℃. As shown in fig. 5, it can be seen from the time-voltage curve of the lithium symmetric battery using the electrolyte prepared in comparative example 2 that the polarization voltage started to increase after 20 hours of cycling and the battery was damaged after 30 hours of cycling. As shown in fig. 6, the time-voltage curve of the lithium symmetric battery added with the electrolyte prepared in example 2 still remained stable after 120h, and thus it can be seen that the electrolyte prepared in example 2 can effectively improve the electrochemical stability of the battery.
The foregoing embodiments and description have been provided merely to illustrate the principles of the invention and various changes and modifications may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (10)
1. The organic ester electrolyte additive is characterized in that the organic ester is one or more of tetraethyl titanate, tetrabutyl titanate, tetraisopropyl titanate and tetraethyl silicate.
2. An electrolyte comprising an electrolytic lithium salt, a non-aqueous organic solvent, and the organic ester electrolyte additive of claim 1.
3. The electrolyte of claim 2, wherein the concentration of the organic ester electrolyte additive in the electrolyte is 1-50%.
4. The electrolyte according to claim 2, wherein the electrolyte lithium salt is one or more of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium trifluorochloroborate, lithium tetracyanoborate, lithium difluorooxalato borate, lithium dioxaoxalato borate, lithium difluorosulfatesulfonylimide, lithium difluorosulfonimide, lithium trifluoromethylsulfonimide, and lithium fluoroalkylphosphonate.
5. The electrolyte of claim 2, wherein the concentration of the electrolyte lithium salt in the electrolyte is 0.8-1.5 mol/L.
6. The electrolyte according to claim 2, wherein the non-aqueous organic solvent is a mixed solvent of a cyclic organic solvent and a chain organic solvent.
7. The electrolyte according to claim 6, wherein the cyclic organic solvent is one of ethylene carbonate, propylene carbonate and butylene carbonate, and the chain organic solvent is one or two of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate and ethyl acetate.
8. The electrolyte as claimed in claim 6, wherein the cyclic organic solvent is present in an amount of 25 to 50% by volume based on the total volume of the electrolyte.
9. A lithium metal battery comprising a metallic lithium positive electrode, a metallic lithium negative electrode, a battery separator, and the electrolyte of any one of claims 2 to 8.
10. The use of the organic ester electrolyte additive of claim 1 in the preparation of a lithium metal battery.
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| US20030190529A1 (en) * | 2002-04-03 | 2003-10-09 | Samsung Sdi Co., Ltd. | Electrolyte for lithium battery and lithium battery comprising same |
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