CN111900478A - Electrolyte additive, electrolyte containing electrolyte additive and lithium metal battery containing electrolyte - Google Patents
Electrolyte additive, electrolyte containing electrolyte additive and lithium metal battery containing electrolyte Download PDFInfo
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- CN111900478A CN111900478A CN202010843835.9A CN202010843835A CN111900478A CN 111900478 A CN111900478 A CN 111900478A CN 202010843835 A CN202010843835 A CN 202010843835A CN 111900478 A CN111900478 A CN 111900478A
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- lithium
- electrolyte
- additive
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- polyoxometallate
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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
-
- 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
-
- 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 an electrolyte additive, an electrolyte containing the electrolyte additive and a lithium metal battery containing the electrolyte, wherein the additive is polyoxometallate, the electrolyte comprises electrolyte lithium salt, a non-aqueous organic solvent and the additive, the concentration of the additive is 2-8mmol/L, and the lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte. The polyoxometallate is a large anion, can absorb a large amount of lithium ions around the polyoxometallate, and soluble polyoxometallate containing elements in a high oxidation state can be used as an electrolyte additive to perform redox reaction with lithium metal, so that a lithium-rich layer is formed around a polyacid compound, and a lithium-rich passivation film is further formed on the surface of the lithium metal in situ, and on one hand, the passivation film can inhibit the formation of lithium dendrites and improve the safety performance of the battery; on the other hand, under the condition of high rate, the electrochemical performance and the cycling stability of the battery can be improved.
Description
Technical Field
The invention relates to the technical field of lithium metal batteries, in particular to an electrolyte additive, an electrolyte containing the electrolyte additive and a lithium metal battery containing the electrolyte.
Background
In recent years, lithium metal batteries have become a focus of attention in the field of energy storage because of their high energy density. Lithium metal batteries use lithium metal as the negative electrode, replacing the graphite negative electrode in conventional lithium ion batteries. However, when lithium metal is used as a negative electrode of a lithium secondary battery, lithium is likely to form lithium dendrites during repeated plating and stripping processes, and if severe, it is likely to pierce through a separator to cause short-circuiting inside the battery, causing fire or even explosion. Therefore, inhibiting the growth of lithium dendrites is key to achieving high energy density lithium metal battery scale-up applications.
In order to inhibit the growth of lithium dendrites, finding an effective strategy to improve the safety and the cycling stability of the lithium metal battery is the key to realizing the large-scale application of the high-energy density lithium metal battery. And among many strategies, the use of electrolyte additives is considered to be the most feasible, economical and efficient way to solve the problems that have hindered their development as innovative energy storage technologies. Therefore, researchers have proposed a method for improving the electrochemical performance of lithium metal batteries based on the conventional lithium ion battery electrolyte. In 2004, MacFarlane et al introduced a zwitterionic compound as a promoter to dissociate lithium ions from the polymer backbone, thereby improving the ionic conductivity of the electrolyte. Archer et al found that lithium halide salts are good additives for improving long-term cycling of rechargeable Lithium Metal Batteries (LMB) at Room Temperature (RT). Also an additive AlCl3Has proven effective for Li metal negative electrode protection. AlCl3Reaction with trace amounts of water inevitably present in the electrolyte forms Al (OH)3Nano colloidal particles to form stable Al-rich particles on Li surface2O3SEI film of (a), and the like. Although the above-mentioned research idea can inhibit the growth of lithium dendrites under certain specific conditions, the inhibition effect is often unsatisfactory when the current density of the battery is increased.
Disclosure of Invention
One of the purposes of the invention is to provide an electrolyte additive.
The second purpose of the invention is to provide an electrolyte containing the electrolyte additive.
It is another object of the present invention to provide a lithium metal battery comprising the above electrolyte.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: an electrolyte additive, which is a polyoxometallate.
Preferably, the polyoxometallate is selected from one or more of polymetallic molybdate, polymetallic tungstate, polymetallic vanadate, polymetallic niobate, polymetallic tantalate and polymetallic titanate.
The invention also provides electrolyte, which comprises electrolyte lithium salt, a non-aqueous organic solvent and an additive, wherein the additive is the electrolyte additive, and the concentration of the additive in the electrolyte is 2-8 mmol/L.
Preferably, the electrolyte lithium salt is selected from lithium hexafluorophosphate (LiPF)6) Lithium tetrafluoroborate (LiBF)4) Lithium trifluoroborate (LiBF)3Cl), lithium tetracyanoborate (LiB (CN)4) Lithium difluorooxalato borate (LiDFOB), lithium dioxalate borate (LiBOB), lithium difluorosulfatato borate (LiBF)2SO4) One or more of lithium bis-fluorosulfonylimide (LiFSI), lithium trifluoromethanesulfonylimide (LiTFSI), and lithium fluoroalkylphosphonate (LiFAP).
Preferably, the non-aqueous organic solvent is selected from a mixed solvent consisting of one of cyclic Ethylene Carbonate (EC), Propylene Carbonate (PC) and Butylene Carbonate (BC) and one or two of chain dimethyl carbonate (DMC), diethyl carbonate (DEC), Ethyl Methyl Carbonate (EMC) and Ethyl Acetate (EA).
Wherein the volume content of the annular organic solvent accounts for 25-50% of the total volume of the electrolyte.
Preferably, the concentration of the electrolytic lithium salt in the electrolytic solution is 0.8 to 1.5 mol/L.
The invention also provides a lithium metal battery which comprises a positive electrode, a negative electrode, a diaphragm and electrolyte, wherein the positive electrode active material is at least one of oxygen, air and lithium-containing metal oxide, the negative electrode active material is lithium metal or lithium alloy, and the electrolyte is the electrolyte.
The lithium-containing metal oxide is selected from one or more of lithium cobaltate, lithium nickelate, lithium manganate, lithium iron phosphate or lithium nickel cobalt manganate.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, polyoxometallate is introduced into the lithium battery electrolyte for the first time, and the uniform deposition of lithium ions is realized in the circulation process, so that the lithium metal anode is protected, and the circulation life of the lithium metal battery is prolonged.
2. The polyoxometallate is a large anion, can absorb a large amount of lithium ions around the polyoxometallate, and soluble polyoxometallate containing elements in a high oxidation state can be used as an electrolyte additive to perform redox reaction with lithium metal, so that a lithium-rich layer is formed around a polyacid compound, and a passivation film with a stable structure is further formed on the surface of the lithium metal in situ, and on one hand, the passivation film timely supplements the deficiency of the lithium ions on a lithium metal anode, so that the formation of lithium dendrites is inhibited, and the safety performance of the battery is improved; on the other hand, the lithium metal can be protected from being corroded by the electrolyte, and the utilization rate and the cycling stability of the battery are improved. Matching with high voltage anode materials will help to advance the industrialization process.
Drawings
FIG. 1 is a surface of a lithium metal anode of a comparative example 1 lithium-lithium symmetric cell after 30 weeks of cycling in an electrolyte without the addition of a polyoxometalate additive;
FIG. 2 is the surface of the lithium metal anode of the lithium-lithium symmetric cell of example 1 after 30 weeks of cycling in an electrolyte with the addition of a polyoxometalate additive;
fig. 3 is a case where a full cell assembled with a blank electrolyte of comparative example 1 and an electrolyte of example 1 to which a polyacid was added, respectively, was cycled under a rate condition of 3C;
FIG. 4 is a time-voltage curve of a lithium-lithium symmetric cell assembled with the electrolyte of comparative example 2;
fig. 5 is a time voltage curve of a lithium-lithium symmetric battery assembled with the electrolyte of example 2.
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 examples of the present invention, unless otherwise specified, the raw materials and reagents used were commercially available and the purity was analytical purity and above.
Example 1
In an argon-filled glove box, lithium hexafluorophosphate (LiPF) was added6) Dissolving in ethylene carbonate by volume ratio: dimethyl carbonate: ethyl methyl carbonate ═ 1: 1: 1 in a non-aqueous organic solvent mixed with lithium hexafluorophosphate in a final concentration of 1mol/L, and then phosphomolybdovanadophosphoric acid (H) was added thereto5PMo10V2O40) And the concentration of the phosphomolybdovanadophosphoric acid in the electrolyte is 5mmol/L, stirring and mixing, and drying the reagents used in the preparation in a glove box for more than 12 hours to prepare the electrolyte.
Comparative example 1
In an argon-filled glove box, lithium hexafluorophosphate (LiPF) was added6) Dissolving in ethylene carbonate by volume ratio: dimethyl carbonate: ethyl methyl carbonate ═ 1: 1: 1, the final concentration of lithium hexafluorophosphate salt is 1mol/L in the mixed non-aqueous organic solvent, no additive is used, the mixture is stirred and mixed, and the reagents used in the preparation are all dried in a glove box for more than 12 hours to prepare the electrolyte.
Assembling the lithium-lithium symmetrical battery: the battery assembly needs to be 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 prepared electrolyte without the polyoxometallate additive or the electrolyte with the polyoxometallate additive is injected into the battery, and the battery is packaged through a packaging machine, namely the assembly of the lithium-lithium symmetrical battery is completed.
Electrochemical testing of the lithium symmetric battery of this example was performed on a LAND test system, with the test temperature maintained at a constant temperature of 25 ℃.
Testing the room-temperature electrochemical cycle performance: the cell was left standing at room temperature (25 ℃ C.) for 24 hours at 4mA/cm2The constant current charge and discharge test was performed at a current density of (1) and the cycle number was 30 weeks. The results show that: when the electrolyte containing no electrolyte additive is used, the concentration of the electrolyte is 4mA/cm2At current density ofAfter 30 cycles, it can be seen from fig. 1 that a large amount of lithium dendrites are formed on the surface of the lithium metal anode. In contrast, the electrolyte containing the electrolyte additive was at 4mA/cm2After 30 cycles at the current density of (a), it can be seen from fig. 2 that no dendrite is formed on the surface of the lithium metal anode.
Assembling the lithium metal battery: the battery assembly needs to be carried out in a glove box filled with argon protective atmosphere, the battery is assembled by taking metal lithium as a negative electrode and lithium cobaltate as a positive electrode, then the prepared electrolyte without the polyoxometallate additive or the electrolyte with the polyoxometallate additive is injected into the battery, and the battery is packaged by a packaging machine, namely the lithium metal battery assembly is completed.
The electrochemical performance test is carried out on the battery system, the capacity of the lithium battery without the electrolyte additive is attenuated very quickly, and the capacity is almost 0 after 200 cycles; and the capacity retention rate of the full cell assembled by adding the polyoxometallate additive reaches 74% after 200 cycles under the high-rate condition of 3C. It can be seen that the electrolyte additive of the present invention can effectively improve the electrochemical performance of the battery, as shown in fig. 3.
Example 2
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 in a mixed nonaqueous organic solvent with a final concentration of lithium hexafluorophosphate of 1mol/L, and then silicotungstic acid (H) was added thereto4SiW12O40·xH2O), the concentration of silicotungstic acid in the electrolyte is 5mmol/L, stirring and mixing are carried out, all reagents used in preparation are dried in a glove box for more than 12 hours, and the electrolyte is prepared.
Comparative example 2
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 in a mixed non-aqueous organic solvent, the final concentration of lithium hexafluorophosphate is 1mol/L, no additive is used, the mixture is stirred and mixed, and all reagents used in the preparation are in a glove boxDrying for more than 12h to obtain the electrolyte.
Assembling the lithium-lithium symmetrical battery: the battery assembly needs to be 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 prepared electrolyte without the polyoxometallate additive or the electrolyte with the polyoxometallate additive is injected into the battery, and the battery is packaged through a packaging machine, so that the lithium-lithium symmetrical battery assembly is completed.
Electrochemical testing of the lithium symmetric battery of this example was performed on a LAND test system, with the test temperature maintained at a constant temperature of 25 ℃. As can be seen from the time-voltage curve of the lithium symmetric battery using no polyoxometalate electrolyte additive, as shown in fig. 4, the polarization voltage starts to increase after 20 cycles, and the battery is damaged after 30 cycles; as shown in FIG. 5, H is added4SiW12O40·xH2The time-voltage curve of the lithium-lithium symmetrical battery assembled by the O additive still keeps stable after 80 circles, so that the electrolyte additive 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 (9)
1. An electrolyte additive, characterized in that the additive is a polyoxometallate.
2. The electrolyte additive as claimed in claim 1, wherein the polyoxometallate is selected from one or more of the group consisting of a multimetal molybdate, a multimetal tungstate, a multimetal vanadate, a multimetal niobate, a multimetal tantalate, and a multimetal titanate.
3. An electrolyte comprising an electrolytic lithium salt, a non-aqueous organic solvent and an additive, wherein the additive is the electrolyte additive according to claim 1 or 2, and the concentration of the additive in the electrolyte is 2 to 8 mmol/L.
4. The electrolyte of claim 3, wherein the electrolyte lithium salt is selected from one or more of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium trifluorochloroborate, lithium tetracyanoborate, lithium difluorooxalato borate, lithium dioxaoxalato borate, lithium difluorosulfate borate, lithium difluorosulfonimide, lithium trifluoromethylsulfonimide, and lithium fluoroalkylphosphonate.
5. The electrolyte as claimed in claim 3, wherein the non-aqueous organic solvent is selected from one of cyclic ethylene carbonate, propylene carbonate and butylene carbonate, and one or two of chain dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate and ethyl acetate.
6. The electrolyte of claim 5, wherein the cyclic organic solvent is present in an amount of 25 to 50% by volume based on the total volume of the electrolyte.
7. The electrolyte of claim 3, wherein the concentration of the electrolytic lithium salt in the electrolyte is 0.8-1.5 mol/L.
8. A lithium metal battery comprising a positive electrode, a negative electrode, a separator and an electrolyte, wherein the positive electrode active material is at least one of oxygen, air and a lithium-containing metal oxide, and the negative electrode active material is a lithium metal or a lithium alloy, and the electrolyte is the electrolyte according to any one of claims 3 to 7.
9. The lithium metal battery of claim 8, wherein the lithium-containing metal oxide is selected from one or more of lithium cobaltate, lithium nickelate, lithium manganate, lithium iron phosphate, or lithium nickel cobalt manganate.
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| CN202010843835.9A CN111900478A (en) | 2020-08-20 | 2020-08-20 | Electrolyte additive, electrolyte containing electrolyte additive and lithium metal battery containing electrolyte |
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| CN202010843835.9A CN111900478A (en) | 2020-08-20 | 2020-08-20 | Electrolyte additive, electrolyte containing electrolyte additive and lithium metal battery containing electrolyte |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112713309A (en) * | 2021-01-11 | 2021-04-27 | 天津市捷威动力工业有限公司 | Safety lithium ion battery electrolyte and lithium ion battery thereof |
| CN114122439A (en) * | 2021-11-06 | 2022-03-01 | 上海大学 | Lithium/carbon fluoride battery electrolyte containing Lewis acid additive |
| CN114744190A (en) * | 2022-03-22 | 2022-07-12 | 浙江南都电源动力股份有限公司 | Additive for preventing partial lithium supplement excess of pre-lithiation negative electrode, method thereof and lithium ion battery |
| WO2023123413A1 (en) * | 2021-12-31 | 2023-07-06 | 宁德时代新能源科技股份有限公司 | Electrolyte, secondary battery, and electric device |
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