CN110854437A - Lithium-sulfur battery electrolyte containing multifunctional additive and application thereof - Google Patents
Lithium-sulfur battery electrolyte containing multifunctional additive and application thereof Download PDFInfo
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- 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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Abstract
The invention discloses a lithium-sulfur battery electrolyte containing a multifunctional additive and application thereof, belonging to the technical field of chargeable and dischargeable high-specific-energy secondary batteries. The electrolyte comprises an organic solvent, lithium salt and a multifunctional additive, wherein the multifunctional additive is a compound with R1‑O‑R2One or more of the compounds of the formula; the R is1、R2Identical or different, R1Or R2Selected from C1-C8 alkyl, C2-C8 alkenyl, C3-C8 cycloalkyl, C3-C8 heterocycloalkyl or partially unsaturated C3-C8 cycloalkyl; the ring structure of the C3-C8 naphthenic base, the C3-C8 heterocyclic alkyl or the partially unsaturated C3-C8 cyclic hydrocarbon group contains or does not contain substituent. The invention reduces the loss of active substances of sulfur and lithium, enhances the cycling stability of the battery, inhibits the chemical reaction between polysulfide in electrolyte and metal lithium, and promotes the improvement of the battery performance by introducing the multifunctional ether additiveCoulombic efficiency of the cell.
Description
Technical Field
The invention belongs to the technical field of chargeable and dischargeable high-specific-energy secondary batteries, and particularly relates to a lithium-sulfur battery electrolyte containing a multifunctional additive and application thereof.
Background
With the continuous development of new energy technology, especially with the urgent need of high energy density secondary batteries in the fields of intelligent communication equipment and electric vehicles. The method has practical significance for the research of high-energy density energy storage and conversion devices. Compared with the traditional lithium ion battery which stores energy by depending on the insertion and extraction of lithium ions, the multi-electron reaction material system is the basis for constructing the high-specific-energy secondary battery from the electrochemical perspective. Among them, the lithium-sulfur battery has a very high theoretical specific capacity (1672mAh/g) and theoretical energy density (2570Wh/kg), and the sulfur is cheap and abundant, so it has become the key research object of the next generation of new lithium secondary battery.
Although the lithium-sulfur battery has many advantages, the lithium-sulfur battery is still not commercialized at present, and the main reason is that the intermediate product lithium polysulfide can be dissolved in the conventional ether electrolyte during the charging and discharging processes of the lithium-sulfur battery, and migrates between the positive electrode and the negative electrode under the dual action of an electric field and a concentration field, namely, the shuttle effect. On the one hand, the shuttling effect reduces the availability of active substances; on the other hand, lithium polysulfide can also undergo an irreversible chemical reaction with a lithium metal cathode to corrode the lithium metal, causing serious lithium dendrite problems and rapid failure of the lithium cathode, which seriously affects the coulombic efficiency and cycle life of the lithium-sulfur battery. At present, research on lithium-sulfur batteries is mainly focused on a positive electrode material part, and shuttle reaction of lithium polysulfide can be effectively inhibited by the design of a positive electrode structure and the introduction of chemical adsorption. However, on the one hand, this results in increased costs, and on the other hand, requires complicated electrode material design, which is not favorable for the wide application and popularization of lithium-sulfur batteries. The formation of a stable SEI on the surface of lithium metal by the introduction of functional additives is an effective method for protecting lithium metal negative electrodes, but poor long-term cycling stability is caused due to the small amount of additives and the continuous consumption during cycling.
The method is simple, economic and effective for a long time, and can relieve the corrosion of metal lithium and greatly improve the cycle stability and the coulombic efficiency of the lithium-sulfur battery by changing the solvent composition of the electrolyte. Therefore, the development of lithium-sulfur battery electrolytes that significantly improve the cycle life of the batteries is a current research focus. However, the development of lithium sulfur electrolytes is greatly challenged by the complexity of the multiple electron conversion mechanism and the instability of polysulfides.
Disclosure of Invention
The invention aims to provide a lithium-sulfur battery electrolyte containing a multifunctional additive and application thereof, and the specific technical scheme is as follows:
a lithium-sulfur battery electrolyte containing a multifunctional additive comprises an organic solvent, a lithium salt and the multifunctional additive, wherein the multifunctional additive is a compound having R1-O-R2One or more of the compounds of the formula;
the R is1、R2Identical or different, R1Or R2Selected from C1-C8 alkyl, C2-C8 alkenyl, C3-C8 cycloalkyl, C3-C8 heterocycloalkyl or partially unsaturated C3-C8 cycloalkyl;
the alkyl group from C1 to C8 and the alkenyl group from C2 to C8 are straight chain or branched chain alkyl groups.
The ring structure of the C3-C8 naphthenic base, the C3-C8 heterocyclic alkyl or the partially unsaturated C3-C8 cyclic hydrocarbon group contains or does not contain substituent.
The heteroatom in the C3-C8 heterocycloalkyl is a nitrogen atom, a sulfur atom or an oxygen atom; the partially unsaturated C3-C8 cyclic hydrocarbon group comprises C3-C8 cycloalkenyl, phenyl and substituted phenyl.
And the substituent on the ring structure of the C3-C8 naphthenic base, C3-C8 heterocyclic alkyl or partially unsaturated C3-C8 cyclic hydrocarbon is C1-C6 alkyl, C1-C6 alkylene, amino, phenyl or halogen.
The organic solvent is one or more of 1, 3-dioxolane, 1, 4-dioxane, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, tetrahydrofuran, ethylmethylsulfone, sulfolane, isopropyl methylsulfone, dimethyl sulfoxide, dimethyl trisulfide, dimethyl disulfide and dimethyl sulfide.
The lithium salt is one or more of lithium hexafluorophosphate, lithium dioxalate borate, lithium bistrifluoromethanesulfonylimide (LiTFSI), lithium bistrifluoromethanesulfonylimide, lithium perchlorate, lithium difluorooxalate borate, lithium nitrate and lithium trifluoromethanesulfonate.
The concentration of the lithium salt in the lithium-sulfur battery electrolyte is 0.1-4 mol/L, and the volume of the multifunctional additive is 5-80% of the volume of the lithium-sulfur battery electrolyte.
The lithium-sulfur battery electrolyte also contains an auxiliary additive, wherein the auxiliary additive is one or more of lithium nitrate, lithium polysulfide, potassium nitrate, cesium nitrate and lithium bromide.
The auxiliary additive accounts for 0.1-5% of the mass of the lithium-sulfur battery electrolyte.
The lithium-sulfur battery electrolyte is used for preparing a lithium-sulfur battery. The lithium-sulfur battery comprises a positive electrode, a negative electrode, a diaphragm and the lithium-sulfur battery electrolyte; the active material of the positive electrode is one or more of elemental sulfur, a sulfur-containing polymer, lithium sulfide and lithium polysulfide; the negative electrode is any one of metal lithium foil, lithium sheet and lithium alloy.
The invention has the beneficial effects that:
(1) according to the lithium-sulfur battery electrolyte containing the multifunctional additive, on one hand, chemical reaction between polysulfide in the electrolyte and metal lithium is inhibited; on the other hand, the deposition morphology of the metal lithium is changed, the deposition uniformity of the metal lithium is enhanced, the problems of rapid consumption of the metal lithium cathode, generation of dead lithium, growth of dendrite and the like are effectively avoided, the deposition behavior of the metal lithium is regulated, the lithium cathode is prevented from being corroded by high-concentration polysulfide, and the concentration of polysulfide in the electrolyte is reduced. The multifunctional ether additive is introduced, so that the loss of active substances, namely sulfur and lithium, is reduced, the coulombic efficiency of the battery is improved, and the cycle stability of the battery is enhanced.
(2) The lithium-sulfur battery electrolyte containing the multifunctional additive provided by the invention is simple in component and low in cost, can be applied to a sulfur positive electrode with high sulfur capacity, and is a lithium-sulfur battery electrolyte with research value and industrialization potential.
Drawings
FIG. 1 shows the cycle performance and coulombic efficiency of a lithium-sulfur battery according to example 2 of the present invention;
FIG. 2 shows the cycle performance and coulombic efficiency of a lithium-sulfur battery of comparative example 2 according to the present invention.
Detailed Description
The invention provides a lithium-sulfur battery electrolyte containing a multifunctional additive and application thereof, and the invention is further described by combining the embodiment and the attached drawings.
The lithium-sulfur battery comprises a positive electrode, a negative electrode, a diaphragm and electrolyte. The positive electrode comprises a positive electrode current collector and a positive electrode material compounded on the surface of the positive electrode current collector; the positive electrode current collector is a current collector having excellent conductivity in the art, such as aluminum foil.
The positive electrode material is obtained by curing slurry of a positive electrode active material, a conductive agent, a binder and a solvent, wherein the conductive agent, the binder and the solvent are all common materials in the field.
The embodiment of the invention selects the carbon nano tube conventionally used by the lithium-sulfur battery as the carrier of the active substance sulfur of the positive electrode, and prepares the positive electrode material with acetylene black as a conductive agent, polyvinylidene fluoride as a binder and NMP as a solvent, and the specific operation is as follows:
(1) mixing 30g of multi-walled carbon nanotubes (MWCNT) with 70g of commercial sulfur powder, and performing ball milling at the rotating speed of 600rpm for 6h to obtain uniformly mixed powder MWCNT/S; uniformly mixing the ball-milled mixture MWCNT/S, acetylene black and polyvinylidene fluoride in an N-methyl pyrrolidone (NMP) solution according to the ratio of 8:1:1 to obtain prepared slurry;
(2) and uniformly coating the slurry on an aluminum foil, drying at 60 ℃ for 12h, cutting into pole pieces with the diameter of 13mm, and putting the pole pieces into a glove box to remove water for later use.
In the embodiment of the invention, a polypropylene microporous membrane of Celgard 2400 is selected as the diaphragm.
Examples
Electrolyte preparation: in a glove box filled with argon (O)2，H2Content of O is equal to<0.1ppm), a mixed solution of two or more of ethylene glycol dimethyl ether (DME), 1, 3-Dioxolane (DOL), diethylene glycol dimethyl ether (G2), triethylene glycol dimethyl ether (G3), tetraethylene glycol dimethyl ether (G4), Tetrahydrofuran (THF), dimethyl sulfoxide (DMSO), and dimethyl trisulfide (DMTS) is used as the organic solvent. Adding 0.1-5% of auxiliary additive based on total electrolyte mass, and adding 5-80% of multifunctional additive based on total electrolyte volumeAnd adding an additive into the electrolyte, and fully and uniformly stirring the additive and the electrolyte to ensure that the concentration of the lithium salt in the electrolyte is 1.0mol/L (M) to obtain the lithium-sulfur battery electrolyte.
In argon atmosphere, a metal lithium sheet is taken as a negative electrode, a polypropylene microporous membrane with the model of Celgard 2400 is selected as a diaphragm, the using amount of electrolyte is 15 mu L/mg S, and the CR2025 lithium-sulfur battery is sequentially assembled.
Lithium sulfur batteries were assembled with electrolytes of different component contents to give examples 1-10; lithium sulfur batteries were assembled with electrolyte without the addition of auxiliary additives to give examples 11-15; lithium sulfur batteries were assembled with electrolytes of different organic solvent compositions, to which the same functional additives and auxiliary additives as in examples 1-3 were added, to obtain examples 16-18.
Comparative example 1
The electrolyte prepared without adding the multifunctional additive and the auxiliary additive, namely the electrolyte containing the organic solvent and the lithium salt is taken as a comparative example 1, and the specific operation is as follows: in a glove box filled with argon (O)2，H2Content of O is equal to<0.1ppm), mixing the components in a volume ratio of 1: taking a mixed solution of 1 ethylene glycol dimethyl ether (DME) and 1, 3-Dioxolane (DOL) as an organic solvent, adding a lithium salt to ensure that the concentration of the lithium salt in the electrolyte is 1.0M, and fully and uniformly stirring to obtain the electrolyte of the lithium-sulfur battery.
In argon atmosphere, a lithium metal sheet is taken as a negative electrode, a polypropylene microporous membrane with the model of Celgard 2400 is selected as a diaphragm, and the lithium-sulfur battery is sequentially assembled by using 15 mu L/mg S of electrolyte.
Comparative example 2
The electrolyte prepared without adding the multifunctional additive, namely the electrolyte containing the organic solvent, the lithium salt and the auxiliary additive is taken as a comparative example 2, and the operation is as follows: in a glove box filled with argon (O)2，H2Content of O is equal to<0.1ppm), mixing the components in a volume ratio of 1: a mixed solution of 1-glycol dimethyl ether (DME) and 1, 3-Dioxolane (DOL) as an organic solvent; anhydrous lithium nitrate (LiNO) with a total electrolyte mass of 2% is added3) As an auxiliary additive; and adding lithium salt, and fully and uniformly stirring to ensure that the concentration of the lithium salt in the electrolyte is 1.0M, thereby obtaining the electrolyte of the lithium-sulfur battery.
In argon atmosphere, a lithium metal sheet is taken as a negative electrode, a polypropylene microporous membrane with the model of Celgard 2400 is selected as a diaphragm, and the lithium-sulfur battery is sequentially assembled by using 15 mu L/mg S of electrolyte.
The types of components and their contents in the electrolytes of lithium-sulfur batteries of examples 1 to 18, comparative example 1 and comparative example 2 are shown in table 1:
TABLE 1
After the batteries prepared in examples 1 to 18, comparative example 1 and comparative example 2 are placed in a thermostatic chamber at 25 ℃ and are kept still for 12 hours, a charge-discharge cycle test is carried out on a blue test charge-discharge tester under the constant current 0.5C (1C: 1672mAh/g) charge-discharge and the potential interval is 1.7-2.6V, and the cycle is 200 circles.
The cycling performance and coulombic efficiency of the cells of examples 1-18, comparative example 1, comparative example 2 are shown in table 2:
TABLE 2
Comparing and analyzing examples 11-15 and comparative example 1, the specific discharge capacity of the first circle of the battery in examples 11-15 is not obviously different from that in comparative example 1, the cycle capacity retention rate of 200 circles reaches 72.6% -75.2%, the coulombic efficiency reaches 91.5% -93.4%, and is far higher than that in comparative example 1, the cycle capacity retention rate of 200 circles is 40.5%, and the coulombic efficiency is 64.2%. The single use of the multifunctional additive can greatly improve the capacity retention rate and the coulombic efficiency of the battery.
Comparing and analyzing examples 1-10 and comparative example 2, under the discharge rate of 0.5C, the first-turn specific discharge capacity of examples 1-10 is not obviously different from that of comparative example 2, the cycle capacity retention rate of 200 turns reaches 78.6% -90.3%, and the coulombic efficiency is 94.6% -99.5%, which are far higher than the cycle capacity retention rate of 200 turns in comparative example 2, 57.5%, and the coulombic efficiency is 89.6%. The multifunctional additive is also suitable for greatly improving the cycle performance and the coulombic efficiency of the battery containing non-solvent substances such as lithium nitrate, lithium bromide and the like in the electrolyte.
Comparing and analyzing examples 1-10 and comparative example 1, the first-turn specific discharge capacity of examples 1-10 is not obviously different from that of comparative example 1 under the discharge rate of 0.5C, the cycle capacity retention rate of 200 turns reaches 78.6% -90.3%, and the coulombic efficiency is 94.6% -99.5%, which are far higher than the cycle capacity retention rate of 40.5% of 200 turns and the coulombic efficiency of 64.2% in comparative example 1. Therefore, the auxiliary additive and the multifunctional additive are added simultaneously, so that the circulation capacity retention rate and the coulombic efficiency can be obviously improved.
Comparing examples 11-15 and examples 1-10, it can be seen that the cycle capacity retention rate at 200 cycles and the coulombic efficiency of examples 1-10 are both greater than those of examples 11-15. The auxiliary additive and the multifunctional additive can generate a synergistic effect, and can further improve the cycle performance and the coulombic efficiency of the battery.
Comparing examples 1-3 and examples 16-18, it can be found that there is no obvious difference in first-cycle discharge capacity, 200-cycle capacity retention rate, and average coulombic efficiency. The multifunctional additive of the invention is applicable to different systems of organic solvents.
Claims (10)
1. The lithium-sulfur battery electrolyte containing the multifunctional additive is characterized by comprising an organic solvent, a lithium salt and the multifunctional additive, wherein the multifunctional additive is a compound with R1-O-R2One or more of the compounds of the formula;
the R is1、R2Identical or different, R1Or R2Selected from C1-C8 alkyl, C2-C8 alkenyl, C3-C8 cycloalkyl, C3-C8 heterocycloalkyl or partially unsaturated C3-C8 cycloalkyl;
the ring structure of the C3-C8 naphthenic base, the C3-C8 heterocyclic alkyl or the partially unsaturated C3-C8 cyclic hydrocarbon group contains or does not contain substituent.
2. The lithium sulfur battery electrolyte as defined in claim 1 wherein the heteroatom in the C3-C8 heterocycloalkyl group is a nitrogen atom, a sulfur atom, or an oxygen atom; the partially unsaturated C3-C8 cyclic hydrocarbon group comprises C3-C8 cycloalkenyl, phenyl and substituted phenyl.
3. The lithium sulfur battery electrolyte as claimed in claim 1 wherein the substituents on the C3-C8 cycloalkyl, C3-C8 heterocycloalkyl or partially unsaturated C3-C8 cycloalkyl ring structure are C1-C6 alkyl, C1-C6 alkenyl, amino, phenyl, halogen.
4. The lithium sulfur battery electrolyte as claimed in claim 1 wherein the organic solvent is one or more of 1, 3-dioxolane, 1, 4-dioxane, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, tetrahydrofuran, ethylmethyl sulfone, sulfolane, isopropyl methyl sulfone, dimethyl sulfoxide, dimethyl trisulfide, dimethyl disulfide, and dimethyl sulfide.
5. The lithium sulfur battery electrolyte of claim 1 wherein the lithium salt is one or more of lithium hexafluorophosphate, lithium dioxalate borate, lithium bistrifluoromethanesulfonylimide, lithium bifluorosulfonylimide, lithium perchlorate, lithium difluorooxalato borate, lithium nitrate and lithium trifluoromethanesulfonate.
6. The electrolyte for a lithium-sulfur battery according to claim 1, wherein the concentration of the lithium salt in the electrolyte for a lithium-sulfur battery is 0.1 to 4mol/L, and the volume of the multifunctional additive is 5 to 80% of the volume of the electrolyte for a lithium-sulfur battery.
7. The lithium sulfur battery electrolyte of claim 1 further comprising an auxiliary additive that is one or more of lithium nitrate, lithium polysulfide, potassium nitrate, cesium nitrate, lithium bromide.
8. The lithium sulfur battery electrolyte as defined in claim 7 wherein the auxiliary additive is 0.1 to 5% by mass of the lithium sulfur battery electrolyte.
9. Use of the lithium sulphur battery electrolyte according to any of claims 1 to 8 for the preparation of a lithium sulphur battery.
10. The use of claim 9, wherein the lithium sulfur battery comprises a positive electrode, a negative electrode, a separator, and the lithium sulfur battery electrolyte; the active material of the positive electrode is one or more of elemental sulfur, a sulfur-containing polymer, lithium sulfide and lithium polysulfide; the negative electrode is any one of metal lithium foil, lithium sheet and lithium alloy.
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| CN112768766A (en) * | 2020-12-04 | 2021-05-07 | 中国科学院金属研究所 | Lithium-sulfur battery electrolyte and application thereof |
| CN113675471A (en) * | 2021-08-12 | 2021-11-19 | 湖州昆仑亿恩科电池材料有限公司 | Battery electrolyte and battery comprising same |
| CN114097122A (en) * | 2020-03-06 | 2022-02-25 | 株式会社Lg新能源 | Lithium-sulfur battery electrolyte and lithium-sulfur battery comprising same |
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| CN114097122A (en) * | 2020-03-06 | 2022-02-25 | 株式会社Lg新能源 | Lithium-sulfur battery electrolyte and lithium-sulfur battery comprising same |
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| JP7353459B2 (en) | 2020-03-06 | 2023-09-29 | エルジー エナジー ソリューション リミテッド | Electrolyte for lithium-sulfur batteries and lithium-sulfur batteries containing the same |
| CN111628221A (en) * | 2020-06-18 | 2020-09-04 | 合肥国轩高科动力能源有限公司 | Lithium-sulfur secondary battery electrolyte |
| CN112768766A (en) * | 2020-12-04 | 2021-05-07 | 中国科学院金属研究所 | Lithium-sulfur battery electrolyte and application thereof |
| WO2022149877A1 (en) * | 2021-01-07 | 2022-07-14 | 주식회사 엘지에너지솔루션 | Electrolyte for lithium-sulfur battery, and lithium-sulfur battery comprising same |
| CN113675471A (en) * | 2021-08-12 | 2021-11-19 | 湖州昆仑亿恩科电池材料有限公司 | Battery electrolyte and battery comprising same |
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