CN107342438B - Lithium-sulfur battery electrolyte with high coulombic efficiency and preparation method thereof - Google Patents
Lithium-sulfur battery electrolyte with high coulombic efficiency and preparation method 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 relates to a lithium-sulfur battery electrolyte with high coulombic efficiency and a preparation method thereof, and the lithium-sulfur battery electrolyte comprises an ether organic solvent, a lithium salt and an ester additive, wherein the ester additive is a mixture consisting of one or more of carbonic ester and sulfite; the special additive is mixed with the ether organic solvent and the lithium salt, so that the special additive can react with polysulfide generated in the charging and discharging processes of the lithium-sulfur battery in the charging and discharging processes, the back-and-forth shuttling of the polysulfide is further inhibited, the shuttling effect of the lithium-sulfur battery is effectively inhibited, and the cycle life and the coulombic efficiency of the lithium-sulfur battery are improved.
Description
Technical Field
The invention belongs to the field of lithium-sulfur batteries, relates to a lithium-sulfur battery electrolyte, and particularly relates to a high coulombic efficiency lithium-sulfur battery electrolyte and a preparation method thereof.
Background
In the development of modern society, fossil energy consumption accounts for a larger and larger proportion of energy consumption, and sustainable clean energy is urgently developed. How to solve the problem of environmental pollution and the continuous consumption of fossil energy, and an efficient energy storage device is the core support of the sustainable renewable energy industry, the consumer electronics industry and the traffic industry as the most popular research and development direction.
Among many energy storage modes, lithium ion batteries occupy a central position in current energy storage devices due to the advantages of small self-discharge, high specific energy, long cycle life, wide charging power range, light weight and the like. Most of carbon materials for lithium batteries are used as a negative electrode, a lithium sheet is used as a positive electrode, and lithium ions shuttle back and forth between the positive electrode and the negative electrode to contribute to capacity. After sony first introduced a commercial lithium ion battery in 1991, the lithium ion battery began to be widely applied to portable electronic products such as mobile phones, notebook computers, digital cameras, and the like, and along with the global popularization of these products, the market demand for the lithium ion battery has been kept at a relatively high growth rate, and the huge demand of the market for the lithium ion battery also leads the lithium ion battery industry to continue to be strong, and along with the increasing global attention to electric vehicles, the application of the lithium ion battery in the electric vehicle is made possible. After more than 20 years of development, the existing lithium ion battery is close to the theoretical capacity, but still cannot meet the requirements of industries such as the rapidly-developed electronic industry and the emerging electric automobile, and the like, and the search for a battery system with higher energy density is urgent.
Lithium sulfur battery systems have extremely high theoretical energy densities and are one of the most potential secondary batteries in a variety of energy storage systems. The lithium-sulfur battery uses natural rich sulfur element as a cathode material, has high theoretical specific capacity (1675mAh/g) and higher energy density (2500Wh/kg), and is more than five times of the theoretical capacity of the lithium-ion battery. Unlike conventional lithium ion battery mechanisms, lithium sulfur batteries provide high capacity through a multi-phase transition redox reaction between elemental sulfur, soluble polysulfides, and insoluble lithium sulfides. However, polysulfides, which are intermediates, can be dissolved in the organic liquid electrolyte, resulting in a severe shuttling effect, resulting in a loss of active species. At the same time, severe parasitic reactions with the lithium anode occur, reducing cycle life, resulting in particularly low coulombic efficiencies. In addition, due to the insulation property of sulfur element and the volume expansion (≈ 80%) during charge and discharge, further shortening of the cycle life of the lithium-sulfur battery and reduction of the charging efficiency are caused. Researchers have proposed many improvements on how to improve the coulombic efficiency of lithium sulfur batteries. These solutions focus on the negative electrode material of the battery, and the improvement of the negative electrode material often results in a complicated preparation process and increases the cost of the battery. The development of new lithium sulfur battery electrolytes is one of the convenient and feasible directions.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a lithium-sulfur battery electrolyte with high coulombic efficiency.
In order to achieve the purpose, the invention adopts the technical scheme that: a high coulombic efficiency lithium-sulfur battery electrolyte comprises an ether organic solvent, a lithium salt and an ester additive, wherein the ester additive is a mixture consisting of one or more of carbonate and sulfite.
Optimally, the mass fraction of the ester additive is 0.5-5%.
Further, the mass fraction of the ester additive is 1-3%.
Optimally, the general structural formula of the ester additive is
Wherein Z is C or S, R1And R2Independently of one another, alkyl or phenyl, R3And R4Independently of one another, hydrogen or nitro, R5And R6Independently of one another, H or F.
Further, the ester additive is one or more selected from the following structural formulas,
furthermore, the structural formula of the ester additive is shown in the specification
Preferably, the ether organic solvent is a mixture of ethylene glycol dimethyl ether and 1,3 dioxolane, and the volume ratio of the mixture is 1: 1.
optimally, the concentration of the lithium salt is 0.8-1.2 mol/L.
Further, the lithium salt is lithium bis (trifluoromethylsulfonyl) imide.
The invention also aims to provide a preparation method of the electrolyte of the lithium-sulfur battery with high coulombic efficiency, which comprises the following steps:
(a) adding lithium salt into the ether organic solvent, and stirring to dissolve the lithium salt;
(b) adding a carbonate additive into the mixture obtained in the step (a), and stirring to dissolve the carbonate additive.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: according to the lithium-sulfur battery electrolyte with high coulombic efficiency, the specific additive, the ether organic solvent and the lithium salt are adopted, so that the electrolyte can react with polysulfide generated in the charging and discharging processes of the lithium-sulfur battery in the charging and discharging processes, the shuttle back and forth of the polysulfide is further inhibited, the shuttle effect of the lithium-sulfur battery is effectively inhibited, and the cycle life and the coulombic efficiency of the lithium-sulfur battery are improved.
Drawings
FIG. 1 is a graph comparing the average coulombic efficiencies of the electrolytes of high coulombic efficiency lithium sulfur batteries assembled into lithium sulfur batteries of examples 1-5;
FIG. 2 is a graph showing the cycle effect of the electrolyte of the high coulombic efficiency lithium sulfur battery in example 4 after the lithium sulfur battery is assembled;
FIG. 3 is a charging and discharging curve of the high Coulomb efficiency lithium sulfur battery electrolyte assembled into a lithium sulfur battery in example 4;
FIG. 4 is a graph comparing coulombic efficiencies in example 2, example 4 and comparative example 1 of the present invention;
FIG. 5 is a graph comparing coulombic efficiencies in example 4 of the present invention, comparative example 1, and comparative example 2.
Detailed Description
The high-coulombic efficiency lithium-sulfur battery electrolyte comprises an ether organic solvent, a lithium salt and an ester additive, wherein the ester additive is a mixture consisting of one or more of carbonate and sulfite; the special additive is mixed with the ether organic solvent and the lithium salt, so that the special additive can react with polysulfide generated in the charging and discharging processes of the lithium-sulfur battery in the charging and discharging processes, the back-and-forth shuttling of the polysulfide is further inhibited, the shuttling effect of the lithium-sulfur battery is effectively inhibited, and the cycle life and the coulombic efficiency of the lithium-sulfur battery are improved.
The mass fraction of the ester additive is preferably 0.5 to 5%, more preferably 1 to 3%. The general structural formula of the ester additive is preferably
Wherein Z is C or S, R1And R2Independently of one another, alkyl or phenyl, R3And R4Independently of one another, hydrogen or nitro, R5And R6Independently of one another, H or F; more preferably one or more selected from the following structural formulae,
is optimally as
The ether organic solvent is preferably a mixture of ethylene glycol dimethyl ether and 1,3 dioxolane, and the volume ratio of the mixture is 1: 1. the concentration of the lithium salt is preferably 0.8-1.2 mol/L, and is preferably lithium bis (trifluoromethylsulfonyl) imide. The preparation method of the lithium-sulfur battery electrolyte with high coulombic efficiency comprises the following steps: (a) adding lithium salt into the ether organic solvent, and stirring to dissolve the lithium salt; (b) adding a carbonate additive into the mixture obtained in the step (a), and stirring to dissolve the carbonate additive.
The present invention will be further illustrated with reference to the following examples.
Example 1
The embodiment provides a lithium-sulfur battery electrolyte with high coulombic efficiency, and the preparation method comprises the following specific steps:
(a) putting lithium bis (trifluoromethylsulfonyl) imide into a glove box for full drying; after sufficient drying, adding a mixture of 1: mixing 1 glycol dimethyl ether and 1,3 dioxolane ether in organic solvent, and stirring for dissolving completely;
(b) to the mixture obtained in step (a), bis (4-nitrophenyl) carbonate (CAS No: 5070-13-3), an additive, in a mass ratio of 0.5 wt% in the resulting mixed solution, was added, and the mixture was stirred thoroughly, and allowed to stand for 24 hours after the additive was completely dissolved.
Example 2
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 1, except that: the mass ratio of the additive in the formed mixed solution was 1 wt%.
Example 3
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 1, except that: the mass ratio of the additive in the formed mixed solution was 2 wt%.
Example 4
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 1, except that: the mass ratio of the additive in the formed mixed solution was 3 wt%, and specific electrochemical test data are shown in fig. 2 and 3.
Example 5
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 1, except that: the mass ratio of the additive in the formed mixed solution was 5 wt%.
Example 6
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 4, except that: the additive was replaced with ethyl methyl carbonate.
Example 7
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 4, except that: the additive was replaced by dimethyl carbonate.
Example 8
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 4, except that: the additive is replaced by fluoroethylene carbonate.
Example 9
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 4, except that: the additive is replaced by propylene carbonate.
Example 10
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 4, except that: the additive is replaced by ethylene carbonate.
Example 11
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 4, except that: the additive was replaced with tert-butylphenyl carbonate.
Example 12
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 4, except that: the additive was replaced with di-tert-amyl dicarbonate.
Example 13
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 4, except that: the additive is replaced by diethyl sulfite.
Example 14
This example provides a high coulombic efficiency lithium sulfur battery electrolyte, which is prepared substantially as in example 4, except that: the additive is replaced by ethylene sulfite.
Comparative example 1
This example provides a lithium sulfur battery electrolyte prepared substantially as described in example 1, except that: the mass ratio of the additive in the formed mixed solution was 0 wt%.
Comparative example 2
This example provides a lithium sulfur battery electrolyte prepared substantially as described in example 4, except that: the additive is replaced by the traditional lithium-sulfur battery additive lithium nitrate, and the mass ratio of the lithium nitrate in the formed mixed solution is 3 wt%.
The lithium-sulfur battery electrolyte in each of the above examples was assembled into a lithium-sulfur battery according to the conventional method using a conventional sulfur-carbon mixture as an electrode material to perform electrochemical tests (refer to Xu, n.et al.
TABLE 1 test data for lithium sulfur batteries with different additives in example 4 and examples 6-14
| Examples | Additive for lithium-sulfur battery | Coulombic efficiency | |
| 4 | Bis (4-nitrophenyl) |
100％ | |
| 6 | Carbonic acid methyl ethyl ester | 91.5％ | |
| 7 | Carbonic acid dimethyl ester | 93.7％ | |
| 8 | Fluoroethylene carbonate | 92.3％ | |
| 9 | Propylene carbonate | 94.7％ | |
| 10 | Ethylene carbonate | 95.3％ | |
| 11 | Tert-butylphenyl carbonate | 96.1％ | |
| 12 | Di-tert-amyl dicarbonate | 97.2％ | |
| 13 | Sulfurous acid diethyl ester | 94.1％ | |
| 14 | Ethylene sulfite | 93.5％ |
As can be seen from fig. 1, when the additive is present in the formed mixed solution at a mass ratio of 3 wt%, the average coulombic efficiency of the battery thus manufactured is the highest. And FIG. 4 is a graph comparing coulombic efficiencies in example 2, example 4 and comparative example 1; FIG. 5 is a graph comparing coulombic efficiencies in example 4, comparative example 1, and comparative example 2; it is clear that the coulombic efficiency of the cells made without the addition of additives or with conventional additives is inferior to that of the cells made with the additives of the present invention.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. 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 (1)
1. The preparation method of the high-coulombic-efficiency lithium-sulfur battery electrolyte is characterized in that the high-coulombic-efficiency lithium-sulfur battery electrolyte comprises an ether organic solvent, a lithium salt and an ester additive, wherein the mass fraction of the ester additive is 3%, and the ester additive is
The ether organic solvent is a mixture of ethylene glycol dimethyl ether and 1,3 dioxolane, and the volume ratio of the ether organic solvent to the ethylene glycol dimethyl ether is 1: 1, the concentration of the lithium salt is 0.8-1.2 mol/L, and the lithium salt is bis (trifluoromethylsulfonyl) imide lithium, and the method comprises the following steps:
(a) adding lithium salt into the ether organic solvent, and stirring to dissolve the lithium salt;
(b) adding an ester additive into the mixture obtained in the step (a), and stirring to dissolve the ester additive.
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| CN201710472347.XA CN107342438B (en) | 2017-06-21 | 2017-06-21 | Lithium-sulfur battery electrolyte with high coulombic efficiency and preparation method thereof |
| PCT/CN2017/096364 WO2018232863A1 (en) | 2017-06-21 | 2017-08-08 | Lithium-sulfur battery electrolyte and preparation method therefor |
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| CN108808092B (en) * | 2018-09-04 | 2020-10-09 | 四川华昆能源有限责任公司 | Active electrolyte, preparation method and application |
| CN110444816A (en) * | 2019-07-23 | 2019-11-12 | 浙江大学 | A kind of electrolyte and preparation method thereof for lithium-sulfur cell |
| CN110581248B (en) * | 2019-08-23 | 2021-02-26 | 中南大学 | Lithium-sulfur battery and composite diaphragm thereof |
| CN110649316B (en) * | 2019-08-27 | 2021-04-30 | 南方科技大学 | Electrolyte additive, lithium ion battery electrolyte and lithium sulfur battery |
| EP3993130A4 (en) * | 2020-04-14 | 2022-12-14 | LG Energy Solution, Ltd. | Lithium-sulfur battery electrolyte and lithium-sulfur battery comprising same |
| CN114597489A (en) * | 2022-03-22 | 2022-06-07 | 香河昆仑新能源材料股份有限公司 | Electrolyte containing fluorobenzene carbonate and battery composed of electrolyte |
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