CN115810799A - High-performance lithium metal battery electrolyte and high-performance lithium metal battery - Google Patents
High-performance lithium metal battery electrolyte and high-performance lithium metal battery Download PDFInfo
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- CN115810799A CN115810799A CN202111084748.0A CN202111084748A CN115810799A CN 115810799 A CN115810799 A CN 115810799A CN 202111084748 A CN202111084748 A CN 202111084748A CN 115810799 A CN115810799 A CN 115810799A
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a high-performance lithium metal battery electrolyte and a high-performance lithium metal battery. The high-performance lithium metal battery electrolyte comprises an organic solvent, a lithium salt and an additive, wherein the organic solvent comprises 0-30wt% of carboxylic ester, 0-30wt% of fluorocarboxylic ester, 20-40wt% of carbonic ester, 20-40wt% of fluorocarbonic ester, 0-20wt% of ether and 0-20wt% of fluoroether, and the additive comprises a film-forming additive and a flame-retardant additive. According to the invention, the ester and ether non-aqueous organic solvents are mixed for use, so that the voltage stability window of the electrolyte is improved, the solubility of lithium salt and additives is increased to improve the ionic conductivity of the electrolyte, and the melting point of the electrolyte is further adjusted, thereby being beneficial to improving the high-temperature and low-temperature performances of the electrolyte.
Description
Technical Field
The invention relates to a lithium metal electrolyte, in particular to a high-performance lithium metal battery electrolyte and a high-performance lithium metal battery, and belongs to the technical field of lithium batteries.
Background
With the vigorous popularization of new energy automobiles and the rise of large-scale energy storage products, people continuously pursue an energy storage battery system with high energy density, long cycle life, safety and low cost. The lithium metal has high theoretical specific capacity (3860 mAh/g) and low density (0.534 g/cm) 3 ) The lowest electrochemical potential (-3.04 Vvs. Standard Hydrogen electrode), therefore, the material is considered to be the most ideal negative electrode material for constructing novel energy storage batteries.
However, the lithium dendrite problem is always the biggest obstacle in practical application of lithium metal negative electrodes, lithium metal reacts with an organic solvent in an electrolyte due to extremely strong reducibility, a fragile solid electrolyte film (SEI) is generated on the surface of the lithium metal, and lithium metal cannot be uniformly deposited due to non-uniformity of mass transfer of the SEI film in the lithium deposition/desorption process, so that the lithium dendrite grows. The growing lithium dendrites penetrate the SEI film and even the separator, causing serious safety problems. Meanwhile, the SEI film, which is continuously damaged and regrown, continuously consumes the electrolyte, causing the inside of the battery to dry and become invalid, and severely restricting the cycle life of the battery.
Disclosure of Invention
The invention mainly aims to provide a high-performance lithium metal battery electrolyte and a high-performance lithium metal battery so as to overcome the defects in the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a high-performance lithium metal battery electrolyte, which comprises an organic solvent, a lithium salt and an additive, wherein the organic solvent comprises 0-30wt% of carboxylic ester, 0-30wt% of fluorocarboxylic ester, 20-40wt% of carbonic ester, 20-40wt% of fluorocarbonic ester, 0-20wt% of ether and 0-20wt% of fluoroether, the additive comprises a film forming additive and a flame retardant additive, and the mass fraction of the film forming additive is 0.01-5wt%, and the mass fraction of the flame retardant additive is 0-5wt%.
The embodiment of the invention also provides a high-performance lithium metal battery which comprises a positive electrode, a negative electrode, a diaphragm and the high-performance lithium metal battery electrolyte.
Compared with the prior art, the invention has the advantages that:
1) According to the invention, the ester and ether non-aqueous organic solvents are mixed for use, so that the voltage stability window of the electrolyte is improved, the solubility of lithium salt and additives is increased to improve the ionic conductivity of the electrolyte, and the melting point of the electrolyte is further adjusted, thereby being beneficial to the improvement of the high and low temperature performance of the electrolyte;
2) The lithium salt system selected by the invention is stable to the corrosion current collector, and can form a layer of stable CEI on the surface of the anode material, so that the catalytic decomposition of the anode material on the electrolyte in a high-voltage state is inhibited, the consumption speed of the electrolyte is reduced, and the cycle stability of the lithium metal battery is improved;
3) The film forming additive, one of the additives, can form a compact, flexible and low-resistance SEI film on the surface of a negative electrode, and simultaneously, the film forming additive can reduce the surface tension of the electrolyte and increase the oxidation resistance of the electrolyte under high voltage; the flame-retardant additive can remarkably improve the lightning of the electrolyte, inhibit thermal runaway and improve the safety performance of the lithium metal battery under abuse conditions.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
The embodiment of the invention provides a high-performance lithium metal battery electrolyte, which comprises an organic solvent, a lithium salt and an additive, wherein the organic solvent comprises 0-30wt% of carboxylic ester, 0-30wt% of fluorocarboxylic ester, 20-40wt% of carbonic ester, 20-40wt% of fluorocarbonic ester, 0-20wt% of ether and 0-20wt% of fluoroether, the additive comprises a film-forming additive and a flame-retardant additive, the contents of the carboxylic ester, the fluorocarboxylic ester, the carbonic ester, the fluorocarbonic ester, the ether and the fluoroether are all not 0, and the total amount of the carboxylic ester, the fluorocarboxylic ester, the carbonic ester, the fluorocarbonic ester, the ether and the fluoroether contained in the organic solvent is 100%.
Furthermore, the additive accounts for 0.01-10wt% of the total mass of the electrolyte.
Furthermore, the additive comprises 0.01-5wt% of film-forming additives and 0-5wt% of flame-retardant additives, and the content of the flame-retardant additives is more than 0.
Further, the additive includes a combination of two or more of vinylene carbonate, propylene carbonate, fluoroethylene ester, lithium nitrate, lithium difluorooxalate lithium borate, lithium difluorophosphate, hexamethoxycyclotriphosphazene, hexa (2,2,2-trifluoroethoxy) cyclotriphosphazene, phenoxy pentafluorocyclotriphosphazene, ethoxy pentafluorocyclotriphosphazene, triisopropylethanesulfonyl (pentafluorophenyl) phosphine, but is not limited thereto.
Further, the lithium salt accounts for 10-30wt% of the total mass of the electrolyte.
Further, the lithium salt includes any one or a combination of two or more of lithium hexafluorophosphate, lithium bis (fluorosulfonyl) imide, lithium bis (trifluoromethanesulfonyl) imide, lithium bis (oxalato) borate, lithium difluoro (oxalato) borate, and lithium tetrafluoroborate, but is not limited thereto.
Further, the concentration of the lithium salt is 0.6-4.2mol/L.
Further, the organic solvent accounts for 50-80% of the total mass of the electrolyte.
Further, the carboxylic acid ester includes any one or a combination of two or more of propyl acetate, propyl propionate, ethyl propionate, and ethyl butyrate, but is not limited thereto.
Further, the fluorocarboxylic acid ester includes any one or a combination of two or more of propyl difluoroacetate, propyl trifluoropropionate, and ethyl heptafluorobutyrate, but is not limited thereto.
Further, the carbonate includes any one or a combination of two or more of ethylene carbonate, ethyl methyl carbonate, dimethyl carbonate and diethyl carbonate, but is not limited thereto.
Further, the fluoro carbonate includes any one or a combination of two or more of fluoroethylene carbonate, fluoroethylene carbonate and diethyl fluoro carbonate, but is not limited thereto.
Further, the ethers include any one or a combination of two or more of ethylene glycol dimethyl ether, 1,3-dioxolane, 4-methyl-1,3-dioxolane, 2-methyl-1,3-dioxolane, diglyme, tetrahydrofuran, 2-methyltetrahydrofuran, and dimethoxymethane, but are not limited thereto.
Further, the fluoroether includes any one or a combination of two or more of fluoroethylene glycol dimethyl ether, fluoro 1,3-dioxolane, fluoro 4-methyl-1,3-dioxolane, fluoro 2-methyl-1,3-dioxolane, fluoro diglyme, fluoro tetrahydrofuran, fluoro 2-methyl tetrahydrofuran, and fluoro dimethoxymethane, but is not limited thereto.
The embodiment of the invention also provides a high-performance lithium metal battery which comprises a positive electrode, a negative electrode, a diaphragm and the high-performance lithium metal battery electrolyte.
Further, the active material of the positive electrode includes O 2 、CO 2 、LiCoO 2 、LiFePO 4 、LiNi 1-x-y Co x Mn y O 2 、 LiNi 1-x-y Co x Al y O 2 Any one or more of lithium-rich manganese-based positive electrode material and carbon-sulfur composite positive electrode materialA combination of two or more, but not limited thereto.
Further, the negative electrode includes any one of or a combination of two or more of a lithium metal negative electrode, a surface-modified lithium metal negative electrode, a lithium-copper composite negative electrode, a lithium-magnesium composite negative electrode, a lithium-aluminum composite negative electrode, or a lithium-carbon composite negative electrode, but is not limited thereto.
Further, the upper limit of the charging voltage of the high-performance lithium metal battery is 2.6-4.3V.
The technical solution, the implementation process and the principle thereof will be further explained with reference to the specific embodiments as follows.
Specifically, the high-performance lithium metal battery electrolyte comprises the following components: a non-aqueous organic solvent, an electrolyte lithium salt, a functional additive; wherein the non-aqueous organic solvent is a mixed solvent of carboxylic ester, fluorocarboxylic ester, carbonic ester, fluorocarbonic ester, ethers and fluoroether, and accounts for 50-80% of the total mass of the electrolyte; the electrolyte lithium salt is LiDFOB with the concentration of 0.6-1.0mol/L and LiBH with the concentration of 0.2-0.6mol/L 4 The functional additive comprises VC and LiNO 3 And HFEPN, wherein LiNO 3 Accounting for 0.5-2% of the total mass of the electrolyte, and HFEPN accounting for 3-4.5% of the total mass of the electrolyte.
Example 1
1) Preparing a high-performance lithium metal battery electrolyte:
in a glove box filled with argon, propyl acetate, difluoropropyl acetate, ethylene carbonate, fluoroethylene carbonate and ethylene glycol dimethyl ether are mixed according to the mass ratio of 1: 2: 1, and then lithium hexafluorophosphate with the concentration of 0.6mol/L and LiBH with the concentration of 0.4mol/L are slowly added into the mixed solution 4 Finally, VC accounting for 2 percent of the total mass of the electrolyte and LiNO accounting for 2 percent of the total mass of the electrolyte are added 3 And 1% HFEPN, and uniformly stirring to obtain the high-voltage lithium ion battery electrolyte of the embodiment 1;
2) Preparing a positive plate:
2.1 LiNi in NMP solvent at low dew point conditions 0.8 Co 0.1 Mn 0.1 O 2 Mixing with conductive agent (carbon black) and adhesive (PVDF) at weight ratio of 98: 1Stirring under vacuum condition to prepare anode slurry; then evenly coating the slurry on an aluminum foil with the thickness of 10 mu m;
2.2 Preparing a pole piece; drying the aluminum foil obtained in the step 2.1) at the temperature of 100 ℃, and rolling and splitting to obtain a positive plate;
3) Preparing a negative plate: punching the lithium belt into a standard shape by using a die cutting machine under the condition of low dew point, polishing and grinding the surface of the lithium belt, and rolling and flattening to obtain a negative plate;
4) Preparing a battery: and (2) sequentially laminating the positive plate and the negative plate obtained by the preparation and a polyethylene diaphragm with the thickness of 12 mu m to prepare a square battery core, packaging the battery core into a soft package battery shell (made of an aluminum plastic film), then injecting the prepared electrolyte in vacuum, and packaging, standing, forming, degassing, aging and grading to obtain the soft package lithium metal battery.
Electrochemical testing:
1) And (3) cyclic discharge test: charging the soft package lithium metal battery to 4.3V at a constant current and a constant voltage of 0.2C and a cutoff current of 0.02C at the temperature of 25 ℃, then standing for 10 minutes, discharging to 3.0V at a constant current of 0.5C, and recording the number of cycles when the capacity is attenuated to 80% of the nominal capacity;
2) 4.30V full State 85 ℃/4h storage test: charging the soft package lithium metal battery to 4.30V at room temperature according to 0.2C, setting the cut-off current to 0.02C, standing for 10min, then discharging 0.5C to 3.0V, recording the initial capacity D1, then charging to 4.30V with 0.2C constant current and constant voltage, setting the cut-off current to 0.02C, and testing the thickness T1, voltage and internal resistance of the battery;
the fully charged battery is placed in a thermostat at 85 ℃ for storage for 4 hours, the thermal thickness of the battery is measured and recorded as T2, the cold thickness T3, the voltage and the internal resistance of the battery are tested after the battery is placed for 2 hours at normal temperature, then the battery is placed to 3.0V according to 0.5C to record the retention capacity D2, the battery is placed for 10 minutes and then charged to 4.30V by using 0.2C constant current and constant voltage, the current is cut off by 0.02C, the battery is placed for 10 minutes and then placed to 3.0V by using 0.5C to record the recovery capacity D3.
Battery thermal expansion rate (%) = (T2-T1)/T1 × 100%;
battery capacity retention (%) = D2/D1 × 100%;
battery capacity recovery (%) = D3/D1 × 100%.
The electrolytes of examples 2 to 9 were arranged as shown in table 1, and the other constituent materials and further the structures of the lithium-ion batteries for soft pack of examples 2 to 9 were the same as those of example 1.
Table 1 shows the composition of the electrolytes of examples 1 to 9 and the results of the corresponding lithium metal batteries:
as can be seen from Table 1, VC and LiNO are shown in example 1 and example 2,3 3 As a film forming additive, the film forming additive and the combined organic solvent provided by the invention form an electrolyte together, which is helpful for improving the cycle stability, and the HFEPN is helpful for improving the high-temperature storage performance.
As can be seen from examples 1 to 3 and examples 4 to 6, the DMC solvent, compared to the EMC solvent, together with the combined organic solvent provided by the present invention, forms an electrolyte solution, which can improve the cycle stability and high-temperature storage property of the lithium metal battery.
From examples 1 to 3 and examples 7 to 9, it is clear that LiPF 6 The lithium salt system formed by LiDFOB and the combined organic solvent provided by the invention form an electrolyte together, and the electrochemical performance and the high-temperature storage performance are superior to those of LiPF 6 And LiBH 4 A lithium salt system.
The electrolyte is a key component in the lithium metal battery and has a key influence on the electrochemical performance and the safety performance of the battery. The lithium metal cathode has very strong chemical activity, and can almost spontaneously react with all organic solvents to form an SEI film on the surface of the lithium metal; an ideal SEI film should have good lithium ion conductivity, excellent electron blocking capability, excellent mechanical strength and uniform uniformity, and the traditional electrolyte for lithium ion batteries has an SEI film formed on the surface of lithium metal, mainly contains organic substances, has poor strength, is easy to crack in the charge-discharge cycle process, causes problems of dendrite, liquid consumption and the like, causes short cycle life and low coulombic efficiency, and is not beneficial to the practical application of the lithium metal batteries.
The invention can improve the content of compact inorganic components in the SEI film, enhance the mechanical strength and the electronic blocking capability of the SEI film, ensure the uniform separation and deposition of the lithium metal cathode and obviously prolong the cycle life by adjusting the types of solvent components, lithium salts and additives of the electrolyte.
According to the invention, the ester and ether non-aqueous organic solvents are mixed for use, so that the voltage stability window of the electrolyte is improved, the solubility of lithium salt and additives is increased to improve the ionic conductivity of the electrolyte, and the melting point of the electrolyte is further adjusted, thereby being beneficial to the improvement of the high and low temperature performance of the electrolyte.
The lithium salt system selected by the invention is stable to the corrosion current collector, and can form a layer of stable CEI on the surface of the anode material, so that the catalytic decomposition of the anode material on the electrolyte in a high-voltage state is inhibited, the consumption speed of the electrolyte is reduced, and the cycle stability of the lithium metal battery is improved.
The film forming additive, one of the additives, can form a compact, flexible and low-resistance SEI film on the surface of the negative electrode, and simultaneously can reduce the surface tension of the electrolyte and increase the oxidation resistance of the electrolyte under high voltage; the flame-retardant additive can remarkably improve lightning of the electrolyte, inhibit thermal runaway and improve the safety performance of the lithium metal battery under abuse conditions.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. The electrolyte of the high-performance lithium metal battery is characterized by comprising an organic solvent, a lithium salt and additives, wherein the organic solvent comprises 0-30wt% of carboxylic ester, 0-30wt% of fluorocarboxylic ester, 20-40wt% of carbonic ester, 20-40wt% of fluorocarbonic ester, 0-20wt% of ethers and 0-20wt% of fluoroether, and the additives comprise a film-forming additive and a flame-retardant additive.
2. The high performance lithium metal battery electrolyte of claim 1, wherein: the additive accounts for 0.1-10% of the total mass of the electrolyte.
3. The high performance lithium metal battery electrolyte of claim 1 or 2, wherein: the additive comprises 0.01-5wt% of film-forming additive and 0-5wt% of flame-retardant additive.
4. The high performance lithium metal battery electrolyte of claim 3, wherein: the additive comprises the combination of more than two of vinylene carbonate, propylene carbonate, fluoroethylene ester, lithium nitrate, lithium difluoro oxalate, lithium borate, lithium difluoro phosphate, hexamethoxycyclotriphosphazene, hexa (2,2,2-trifluoroethoxy) cyclotriphosphazene, phenoxy pentafluorocyclotriphosphazene, ethoxy pentafluorocyclotriphosphazene and triisopropyl ethanesulfonyl (pentafluorophenyl) phosphine.
5. The high performance lithium metal battery electrolyte of claim 1, wherein: the lithium salt accounts for 10-30wt% of the total mass of the electrolyte.
6. The high performance lithium metal battery electrolyte of claim 1 or 5, wherein: the lithium salt comprises any one or the combination of more than two of lithium hexafluorophosphate, lithium bis (fluorosulfonyl) imide, lithium bis (trifluoromethanesulfonyl) imide, lithium bis (oxalato) borate, lithium difluoro (oxalato) borate and lithium tetrafluoroborate.
7. The high performance lithium metal battery electrolyte of claim 6, wherein: the concentration of the lithium salt is 0.6-4.2mol/L.
8. The high performance lithium metal battery electrolyte of claim 1, wherein: the organic solvent accounts for 50-80% of the total mass of the electrolyte;
preferably, the carboxylic ester comprises any one or a combination of more than two of propyl acetate, propyl propionate, ethyl propionate and ethyl butyrate;
preferably, the fluorocarboxylic acid ester comprises any one or a combination of more than two of propyl difluoroacetate, propyl trifluoropropionate and ethyl heptafluorobutyrate;
preferably, the carbonate comprises any one or a combination of more than two of ethylene carbonate, ethyl methyl carbonate, dimethyl carbonate and diethyl carbonate;
preferably, the fluoro carbonic ester comprises any one or the combination of more than two of fluoroethylene carbonate, fluoro ethyl methyl carbonate and fluoro diethyl carbonate;
preferably, the ethers include any one or a combination of two or more of ethylene glycol dimethyl ether, 1,3-dioxolane, 4-methyl-1,3-dioxolane, 2-methyl-1,3-dioxolane, diglyme, tetrahydrofuran, 2-methyltetrahydrofuran, and dimethoxymethane;
preferably, the fluoroether comprises any one or the combination of more than two of fluoroether dimethyl ether, fluoro 1,3-dioxolane, fluoro 4-methyl-1,3-dioxolane, fluoro 2-methyl-1,3-dioxolane, fluoro diglycol dimethyl ether, fluoro tetrahydrofuran, fluoro 2-methyl tetrahydrofuran and fluoro dimethoxymethane.
9. A high-performance lithium metal battery comprising a positive electrode, a negative electrode, a separator and the high-performance lithium metal battery electrolyte according to any one of claims 1 to 8.
10. The high performance lithium metal battery of claim 9, wherein: the active material of the positive electrode comprises O 2 、CO 2 、LiCoO 2 、LiFePO 4 、LiNi 1-x-y Co x Mn y O 2 、LiNi 1-x-y Co x Al y O 2 Any one or the combination of more than two of lithium-rich manganese-based positive electrode materials and carbon-sulfur composite positive electrode materials;
preferably, the negative electrode comprises any one or a combination of more than two of a lithium metal negative electrode, a surface modified lithium metal negative electrode, a lithium-copper composite negative electrode, a lithium-magnesium composite negative electrode, a lithium-aluminum composite negative electrode or a lithium-carbon composite negative electrode;
preferably, the upper limit of the charging voltage of the high-performance lithium metal battery is 2.6 to 4.3V.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116231091A (en) * | 2023-05-08 | 2023-06-06 | 宁德时代新能源科技股份有限公司 | Electrolyte for lithium secondary battery, and electricity using device |
| CN117154233A (en) * | 2023-11-01 | 2023-12-01 | 英德市科恒新能源科技有限公司 | Lithium ion battery multiplying power type electrolyte, preparation method and lithium ion battery |
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- 2021-09-15 CN CN202111084748.0A patent/CN115810799A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116231091A (en) * | 2023-05-08 | 2023-06-06 | 宁德时代新能源科技股份有限公司 | Electrolyte for lithium secondary battery, and electricity using device |
| CN116231091B (en) * | 2023-05-08 | 2023-08-29 | 宁德时代新能源科技股份有限公司 | Electrolyte for lithium secondary battery, and electricity using device |
| CN117154233A (en) * | 2023-11-01 | 2023-12-01 | 英德市科恒新能源科技有限公司 | Lithium ion battery multiplying power type electrolyte, preparation method and lithium ion battery |
| CN117154233B (en) * | 2023-11-01 | 2024-02-02 | 英德市科恒新能源科技有限公司 | Lithium ion battery multiplying power type electrolyte, preparation method and lithium ion battery |
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