CN114583280A - Lithium metal battery electrolyte and preparation method thereof - Google Patents
Lithium metal battery electrolyte and preparation method thereof Download PDFInfo
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- CN114583280A CN114583280A CN202011372856.3A CN202011372856A CN114583280A CN 114583280 A CN114583280 A CN 114583280A CN 202011372856 A CN202011372856 A CN 202011372856A CN 114583280 A CN114583280 A CN 114583280A
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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
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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
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Abstract
The invention relates to a local high-concentration electrolyte for a lithium metal battery, and preparation and application thereof. By introducing the alkyl compound into the high-concentration electrolyte, the action force of the alkyl compound and lithium ions is weak, so that the complex structure of a high-concentration system is not damaged in a microscopic mode, the formation of an anion passivation film is facilitated, a lithium cathode is protected, and the stable circulation of the battery is realized. And as a diluent, the ionic conductivity of the whole electrolyte is improved by adding a free solvent macroscopically, the viscosity and the cost of the electrolyte are reduced, and the rate performance of the battery is improved.
Description
Technical Field
The invention relates to an electrolyte for a lithium metal battery and a preparation method thereof, in particular to a lithium metal battery electrolyte containing alkane compounds as a solvent.
Background
Currently, the world market for electric vehicles and portable electronic devices, including passenger cars, buses, and passenger cars, is rapidly growing. Lithium ion batteries having high charge and discharge voltages and long cycle lives are widely used as power sources for portable electronic devices and electric automobiles, but due to the limitation of theoretical energy density thereof, development of novel electrode materials having higher energy density is required. Wherein the lithium metal material has a high theoretical energy density (3860mAh g)-1) And the advantage of a low electrochemical potential (-3.040V vs. she), have received a great deal of attention from researchers in recent years.
However, two problems still remain to be solved in the secondary battery using lithium metal as a negative electrode. One is the dendrite problem. Due to the non-uniformity of lithium metal ion deposition, moss/dendrites are formed in the charge-discharge cycle process, and the moss/dendrites easily pierce through the diaphragm to cause short circuit in the battery and even cause fire. Another problem is instability of the electrode/electrolyte interface. Lithium metal reacts spontaneously with the electrolyte to form a solid electrolyte interface film (SEI), which is continuously damaged and repaired as the volume of the negative electrode expands during charge and discharge cycles, resulting in continuous consumption of lithium metal and electrolyte, and a decrease in the coulombic efficiency and cycle life of the lithium metal battery.
Lithium metal is currently the most widely studied negative electrode material, but its practical application is limited by dendrite and interfacial instability. At present, relevant solutions are proposed, and a solid electrolyte can be adopted to inhibit the growth of dendrites by designing a 3D framework structure, but some problems still exist to be solved urgently. The 3D skeleton structure can slow down dendrite growth by reducing current density, but cannot isolate lithium metal from directly contacting an electrolyte to inhibit the occurrence of side reactions; while inorganic solid-state electrolysis has high mechanical strength, the interface resistance is large, and the contact with lithium metal is poor; although the polymer electrolyte has good flexibility and elasticity, the room-temperature ionic conductivity is relatively low (<10-4S cm-1). By designing effective electrolyte, a stable SEI film is formed in situ to improve the uniformity and stability of an interface, which is an important strategy for effectively inhibiting the growth of lithium dendrites and improving the cycling stability and safety performance of a lithium cathode.
In recent years, studies have shown that high concentrations of electrolyte can significantly improve the cycling stability of lithium metal anodes (nat. commun.2015, 6362). In the high-concentration electrolyte, on one hand, an SEI (solid electrolyte interface) film induced by anions stabilizes an interface, and on the other hand, high-concentration lithium ions can also reduce concentration polarization, so that the cycling stability of the lithium metal battery is remarkably improved. However, the high concentration electrolyte is limited by high viscosity, low ionic conductivity, and high lithium salt cost, and is difficult to realize in large-scale application. Therefore, researchers have developed local high-concentration electrolytes on the basis, and the high-concentration electrolytes are diluted by adding hydrofluoroethers to improve the ionic conductivity and promote the uniform deposition of lithium ions so as to inhibit the growth of dendrites on the surface of lithium metal (adv. mater.2018,30,1706102). However, hydrofluoroether is expensive to produce, difficult to be applied in practical production, and the ether bond is unstable and reacts with lithium metal, resulting in consumption of solvent and failure of the battery. Therefore, the search for new low cost diluents is an important means to solve the problem of lithium metal anodes.
Disclosure of Invention
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
in one aspect of the present invention, there is provided an electrolyte for a lithium metal battery, the electrolyte including a solvent a; the solvent A is an alkane compound, and the alkane compound is saturated chain hydrocarbon (C) consisting of two elements of hydrocarbonnH2n+2Wherein n is>4) Or cyclic hydrocarbons (C)nH2nWherein n is>4) One of (1); preferably, the number of C atoms is 5 to 8 such as pentane, hexane, cyclohexane and the like.
According to the lithium metal battery, the negative electrode is made of lithium metal; the positive electrode can use corresponding metal ion electrode materials (such as lithium iron phosphate, lithium cobaltate, nickel cobalt manganese ternary materials, or sulfur positive electrodes).
Preferably, the electrolyte further comprises a solvent B; the solvent B is at least one of organic solvents of ester, ether, sulfone, ketone and nitrile.
Preferably, the solvent B is one or more of 1, 3-dioxolane, 1, 4-dioxane, ethylene oxide, ethylene glycol dimethyl ether, methyl ethyl ether, ethylene carbonate, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, propylene carbonate, acetonitrile, succinonitrile, sulfolane, dimethyl sulfoxide and cyclobutanone; preferably at least one of 1, 3-dioxolane, ethylene glycol dimethyl ether, ethylene carbonate, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate and propylene carbonate.
Preferably, the electrolyte is a locally high concentration electrolyte. The local high-concentration electrolyte is formed by two different solvents A and B with different mutual solubilities with the supporting electrolyte, and the solvent B has stronger interaction with the supporting electrolyte, so that homogeneous phase dissolution can be realized; solvent a is an anti-solvent supporting the electrolyte.
Preferably, the solvent A accounts for 10-90% of the electrolyte by mass, and preferably 10-50% of the electrolyte by mass.
Preferably, the mass fraction of the supporting electrolyte in the electrolyte accounts for 15-87%, preferably 50-70%, of the electrolyte.
Preferably, the supporting electrolyte is at least one of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium dioxalate borate, lithium difluorooxalate borate, lithium bistrifluoromethylsulphonylimide, lithium trifluoromethanesulfonate, lithium difluorosulphonate, lithium perchlorate, sodium hexafluorophosphate, potassium hexafluorophosphate.
In another aspect of the present invention, there is provided a method for preparing an electrolyte, comprising the steps of:
(1) uniformly mixing the solvent A and the solvent B according to a certain proportion to obtain a mixed organic solvent;
(2) and dissolving the supporting electrolyte in the organic solvent, and uniformly stirring to obtain the electrolyte.
Beneficial results
The invention relates to alkane compounds for regulating lithium metal deposition,
(1) according to the invention, the alkane compound is added to dilute the high-concentration electrolyte, and since the alkane hardly interacts with ions, the complex structure of the high-concentration electrolyte cannot be changed microscopically, so that the formation of an anion passivation film is facilitated, the lithium cathode is protected, and the stable circulation of the battery is realized.
(2) The high-concentration electrolyte has high cost, high viscosity and low ionic conductivity, and is difficult to realize large-scale application. Compared with high-concentration electrolyte, in macroscopical view, the increase of the free solvent can accelerate the lithium ion transmission, reduce the uneven deposition caused by concentration polarization and realize the stable circulation of the battery. The local high-concentration electrolyte has high conductivity, low viscosity and good wettability, and can effectively improve the rate capability of the lithium metal battery.
(3) The alkane compound used in the electrolyte is used as a diluent, and compared with other widely used hydrofluoroethers, the alkane compound has the advantages of wide cost source and low price, greatly reduces the cost of the electrolyte, can be applied in a large scale, has extremely high commercial value, and is more friendly to lithium metal.
(4) Compared with the multi-element compound such as fluoroether, fluorobenzene and the like as the diluent, the diluent (solvent A) in the invention is an alkane compound, and the C-H has strong bonding energy, so that the diluent has excellent stability and is not easy to react with lithium metal, and the consequence that the battery fails due to the dry-up of electrolyte can not occur.
(5) The electrolyte has good stability of the cathode, is used as a diluent, improves the ion conductivity of the whole electrolyte by adding a free solvent macroscopically, reduces the viscosity and the cost of the electrolyte, improves the rate capability of the battery, improves the ion conductivity, can be matched with a high-rate lithium metal battery, and realizes large-scale application.
Drawings
FIG. 1: microstructure schematic diagrams of the high-concentration electrolyte (a) and the local high-concentration electrolyte (b);
FIG. 2: cycling performance of the lithium metal symmetric batteries of comparative examples 1, 5 and examples 1, 3;
FIG. 3: cycling performance of the lithium metal symmetric batteries of comparative example 2 and example 2;
FIG. 4: the lithium copper batteries of comparative example 4 and example 7 had cycling performance and coulombic efficiency;
FIG. 5: lithium metal electrodes of comparative example 1(a) and example 1(b) at 1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (a) surface topography after 10 cycles of deposition.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1
1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is taken as a supporting electrolyte, and ethylene glycol is taken as a solventAnd preparing a local high-concentration electrolyte from a mixed solution of dimethyl ether (DME) and cyclohexane (the cyclohexane accounts for 10% of the total mass of the electrolyte). A lithium sheet with the diameter of 1.6mm and a celgard 2325 diaphragm are used for assembling the lithium | lithium symmetrical battery. 1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (a) is subjected to charge-discharge cycles.
Example 2
1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and a solvent is a mixed solution of ethylene glycol dimethyl ether (DME) and cyclohexane (the cyclohexane accounts for 30 percent of the total mass of the electrolyte) to prepare a local high-concentration electrolyte. A lithium sheet with the diameter of 1.6mm and a celgard 2325 diaphragm are used for assembling the lithium | lithium symmetrical battery. 1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (a) is subjected to charge-discharge cycles.
Example 3
1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and a solvent is a mixed solution of ethylene glycol dimethyl ether (DME) and cyclohexane (the cyclohexane accounts for 50 percent of the total mass of the electrolyte) to prepare a local high-concentration electrolyte. A lithium sheet with the diameter of 1.6mm and a celgard 2325 diaphragm are used for assembling the lithium | lithium symmetrical battery. 1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (a) is subjected to charge-discharge cycles.
Example 4
1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and a solvent is a mixed solution of ethylene glycol dimethyl ether (DME) and pentane (pentane accounts for 10 percent of the total mass of the electrolyte) to prepare a local high-concentration electrolyte. A lithium sheet with the diameter of 1.6mm and a celgard 2325 diaphragm are used for assembling the lithium | lithium symmetrical battery. 1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (a) is subjected to charge-discharge cycles.
Example 5
1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and a solvent is a mixed solution of ethylene glycol dimethyl ether (DME) and pentane (the pentane accounts for 30 percent of the total mass of the electrolyte) to prepare a local high-concentration electrolyte. A lithium | lithium symmetrical battery is assembled by using a lithium sheet with the diameter of 1.6mm and a celgard 2325 as a diaphragm。1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (a) is subjected to charge-discharge cycles.
Example 6
1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and a solvent is a mixed solution of ethylene glycol dimethyl ether (DME) and pentane (pentane accounts for 50% of the total mass of the electrolyte) to prepare a local high-concentration electrolyte. A lithium sheet with the diameter of 1.6mm and a celgard 2325 diaphragm are used for assembling the lithium | lithium symmetrical battery. 1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (a) is subjected to charge-discharge cycles.
Example 7
1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and a solvent is a mixed solution of ethylene glycol dimethyl ether (DME) and cyclohexane (the cyclohexane accounts for 50 percent of the total mass of the electrolyte) to prepare a local high-concentration electrolyte. A lithium sheet with the diameter of 1.6mm is used as a negative electrode, celgard 2325 is used as a diaphragm, and a copper foil with the diameter of 1.9mm is used as a positive electrode, so that the lithium | copper battery is assembled. 1mA/cm2At a current density of 1mAh/cm2Capacity deposition, 1V voltage dissolution for charge and discharge cycles.
Example 8
1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and a solvent is a mixed solution of ethylene glycol dimethyl ether (DME) and pentane (pentane accounts for 50% of the total mass of the electrolyte) to prepare a local high-concentration electrolyte. A lithium sheet with the diameter of 1.6mm is used as a negative electrode, celgard 2325 is used as a diaphragm, and a copper foil with the diameter of 1.9mm is used as a positive electrode, so that the lithium | copper battery is assembled. 1mA/cm2At a current density of 1mAh/cm2Capacity deposition, 1V voltage dissolution for charge and discharge cycles.
Comparative example 1
1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and a solvent is ethylene glycol dimethyl ether (DME) to prepare a low-concentration electrolyte. A lithium sheet with the diameter of 1.6mm and a celgard 2325 diaphragm are used for assembling the lithium | lithium symmetrical battery. 1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (a) is subjected to charge-discharge cycles.
Comparative example 2
4M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and ethylene glycol dimethyl ether (DME) is used as a solvent to prepare a high-concentration electrolyte. A lithium sheet with the diameter of 1.6mm and a celgard 2325 diaphragm are used for assembling the lithium | lithium symmetrical battery. 1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (a) is subjected to charge-discharge cycles.
Comparative example 3
The local high-concentration electrolyte is prepared by using 1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) as a supporting electrolyte and a mixed solution of ethylene glycol dimethyl ether (DME) and hydrofluoroether (the hydrofluoroether accounts for 50 percent of the total mass of the electrolyte). A lithium sheet with the diameter of 1.6mm and a celgard 2325 diaphragm are used for assembling the lithium | lithium symmetrical battery. 1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (2) is subjected to charge-discharge cycles.
Comparative example 4
4M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and a solvent is ethylene glycol dimethyl ether (DME) to prepare a high-concentration electrolyte. A lithium sheet with the diameter of 1.6mm is used as a negative electrode, celgard 2325 is used as a diaphragm, and a copper foil with the diameter of 1.9mm is used as a positive electrode, so that the lithium | copper battery is assembled. 1mA/cm2At a current density of 1mAh/cm2Capacity deposition, 1V voltage dissolution for charge and discharge cycles.
Comparative example 5
1M lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) is used as a supporting electrolyte, and a solvent is a mixed solution of ethylene glycol dimethyl ether (DME) and cyclohexane (the cyclohexane accounts for 60 percent of the total mass of the electrolyte) to prepare a local high-concentration electrolyte. A lithium sheet with the diameter of 1.6mm and a celgard 2325 diaphragm are used for assembling the lithium | lithium symmetrical battery. 1mA/cm2At a current density of 1mAh/cm2The deposition dissolution capacity of (a) is subjected to charge-discharge cycles.
Fig. 1(a) and (b) are schematic views of microstructures of a high concentration electrolyte and a local high concentration electrolyte, respectively. The internal structure of the high-concentration electrolyte is a solvent-anion-lithium ion structure, which can reduce the reaction of a free solvent and lithium metal on one hand, and on the other hand, anions are preferentially reduced on the lithium surface to form an anion-induced SEI film, thereby inhibiting dendritic crystal growth. However, the decrease in the free solvent leads to an increase in the viscosity of the electrolyte and a decrease in the ionic conductivity. By introducing alkane, the original solvation structure is not changed due to weak action force between the alkane and ions, and the increase of the free solvent can accelerate ion transmission and improve the ion conductivity.
The addition of alkanes to the electrolyte can significantly improve the cycling stability of the lithium deposition dissolution. As can be seen from FIG. 2, at a current density of 1mA/cm2The deposition capacity is 1mAh/cm2Under these conditions, the polarization voltage of a lithium symmetrical cell equipped with a low concentration of electrolyte (1M LiTFSI/DME) (comparative example 1) increased to 300mV after 300h cycling. The electrolyte contains alkane, so that the stability of the battery is improved, because the alkane (solvent A) has high stability and is not easy to react with the lithium cathode, the high ionic conductivity of the electrolyte is kept, the SEI induced by anions keeps good cycling stability, the reaction of the lithium cathode and the solvent B is further inhibited, and the battery has low polarization voltage and long cycle life. But as the mass fraction of alkane increases, the polarization voltage decreases first and then increases. The polarization voltage (about 15mV after 500 h) of the electrolyte containing 50% by mass of alkane (example 3) was lower than that of the electrolyte containing 10% by mass of alkane (example 1) (about 30mV after 500 h) and that of the electrolyte containing 60% by mass of alkane (comparative example 5) (about 60mV after 500 h).
As can be seen from fig. 3, the polarization voltage of the electrolyte (example 2) with cyclohexane as a diluent (anti-solvent) was lower than that of the high concentration electrolyte (4M LiTFSI/DME) (comparative example 2). The polarizing voltage is controlled by the diffusion of ions in the solution and SEI film, the high-concentration electrolyte has high viscosity, low ionic conductivity and high polarizing voltage, and the ionic conductivity can be obviously improved and the polarization of the battery can be reduced after the diluent is added.
Experiments have further explored the influence of the reversibility of alkanes on the dissolution of lithium metal battery deposits. As can be seen from fig. 4, when alkane is added as a diluent (example 7) compared with a high-concentration electrolyte (comparative example 4), the coulombic efficiency during the circulation process can reach 99%, which proves that the reversibility of the battery is good, and the coulombic efficiency is stable after 80 times of circulation, which proves that the circulation stability of the battery can be obviously improved by using alkane as the diluent.
And (4) exploring the lithium deposition morphology by utilizing SEM. As can be seen from FIG. 5, the current density at which the current density was 1mA/cm2Specific capacity of 1mAh/cm2After 10 times of charge-discharge circulation under the condition, the surface of the lithium metal electrode taking 1M LiTFSI/DME as electrolyte (comparative example 1) is uneven, loose and porous, the specific surface area of the lithium electrode is large, and the electrolyte is continuously consumed, so that the polarization voltage of the lithium symmetrical battery is increased. The alkane is added as a diluent (example 1), the solvation structure is locally maintained, the SEI formed by the preferential decomposition of anions can effectively inhibit the growth of dendrites, and the surface is more uniform and flat.
Claims (10)
1. An electrolyte for a lithium metal battery, characterized in that: the electrolyte comprises a solvent A; the solvent A is an alkane compound, and the alkane compound is CnH2n+2Or CnH2nAt least one of (1).
2. The electrolyte for a lithium metal battery according to claim 1, wherein: the n is greater than 4.
3. The electrolyte for a lithium metal battery according to claim 1, wherein: preferably, n is more than or equal to 5 and less than or equal to 8.
4. The electrolyte of claim 1, wherein: the electrolyte is a local high-concentration electrolyte.
5. The electrolyte of claim 1, wherein: the solvent A accounts for 10-90% of the electrolyte by mass, and preferably 10-50%.
6. The electrolyte of claim 1, wherein: the mass fraction of the supporting electrolyte in the electrolyte accounts for 15-87%, preferably 50-70%.
7. The electrolyte of claim 5, wherein the supporting electrolyte is at least one of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium dioxalate borate, lithium difluorooxalate borate, lithium bistrifluoromethylsulphonylimide, lithium trifluoromethanesulfonate, lithium difluorosulphonate, lithium perchlorate, sodium hexafluorophosphate, potassium hexafluorophosphate.
8. The electrolyte of claim 1, wherein: the electrolyte also comprises a solvent B; the solvent B is at least one of organic solvents of ester, ether, sulfone, ketone and nitrile.
9. The electrolyte according to claim 8, wherein the solvent B is one or more of 1, 3-dioxolane, 1, 4-dioxane, ethylene oxide, ethylene glycol dimethyl ether, methyl ethyl ether, ethylene carbonate, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, propylene carbonate, acetonitrile, succinonitrile, sulfolane, dimethyl sulfoxide, and cyclobutanone.
10. A method for preparing the electrolyte of claim 8 or 9, comprising the steps of:
(1) uniformly mixing the solvent A and the solvent B according to a certain proportion to obtain a mixed organic solvent;
(2) and dissolving the supporting electrolyte in the organic solvent, and uniformly stirring to obtain the electrolyte.
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