CN107069093A - A kind of high concentration esters electrolyte for lithium-sulfur cell - Google Patents
A kind of high concentration esters electrolyte for lithium-sulfur cell Download PDFInfo
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- CN107069093A CN107069093A CN201710141187.0A CN201710141187A CN107069093A CN 107069093 A CN107069093 A CN 107069093A CN 201710141187 A CN201710141187 A CN 201710141187A CN 107069093 A CN107069093 A CN 107069093A
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- lithium
- electrolyte
- sulfur cell
- esters
- high concentration
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0568—Liquid materials characterised by the solutes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
- H01M2300/0028—Organic electrolyte characterised by the solvent
- H01M2300/0037—Mixture of solvents
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention, which is disclosed, contains lithium salts and organic solvent in a kind of high concentration esters electrolyte for lithium-sulfur cell, the electrolyte, organic solvent is carbonic ester or carboxylate or the two mixing, and concentration of the lithium salts in esters solvent is higher than 3M.The battery electrolyte that the present invention is provided, all solvents are involved in Li+Solvation, thus avoid the reaction of many lithium sulfides and esters solvent, and then obtain and can directly apply to the esters electrolyte of lithium-sulfur cell.Lithium-sulfur cell is directly used as electrolyte using esters, it is to avoid using influence of the shuttle effect to battery performance caused by ethers electrolyte.Meanwhile, it is higher using the lithium-sulphur cell positive electrode sulfur content of esters for small molecule sulphur and sulfurized polyacrylonitrile class battery, contribute to the lithium-sulfur cell that energy density is higher.
Description
Technical field
The present invention relates to a kind of esters battery electrolyte of high concentration, lithium-sulfur cell is mainly used in.
Background technology
Lithium-sulfur cell theoretical specific capacity be 1675mAh/g, theoretical specific energy be 2600Wh/Kg, far above existing lithium from
Sub- battery.And the rich reserves of sulphur, cheap, low toxicity is nuisanceless.Therefore, lithium-sulfur cell turns into high specific energy lithium electricity of future generation
The candidate in pond, causes mondial concern.The many lithium sulfides of lithium-sulfur cell intermediate product can directly react with esters,
Lithium-sulfur cell is typically used as electrolyte solvent, rather than the carbonic ester and carboxylic acid that lithium-ion battery electrolytes are used using ethers
Ester etc..Solubility of many lithium sulfides in ethers electrolyte is higher, and many lithium sulfide meetings in electrolysis are dissolved in charge and discharge process
Migrate to negative pole and occur corrosion reaction with lithium anode, while consuming the active material of both positive and negative polarity, cause circulating battery
The poor, coulombic efficiency of energy is low.Meanwhile, sulphur and Li2Volumetric expansion in S insulating properties, charge and discharge process etc. has also had a strong impact on lithium
The active material utilization and cyclical stability of sulphur battery, seriously hinder its practicalization.
The problem of for lithium-sulfur cell, global researcher is from sulphur positive pole microstructure design, feature barrier film
The many aspects such as preparation, electrolyte modification and the protection of lithium anode have carried out many research work, achieve significant
Effect.Nevertheless, most of work is all based on the expansion of ethers electrolyte, production in the middle of discharge and recharge reaction can not be still completely inhibited
The dissolving and migration of many lithium sulfides of thing in the electrolytic solution, circulating battery stability are not good enough.Meanwhile, for esters, ether
The boiling point of class is very low, thus battery heat endurance is poor, has a strong impact on the security of battery.In addition, researcher also propose by
Small molecule sulphur after cracking is injected into formation small molecule sulphur positive pole in the duct of microporous carbon, and sulfurized polyacrylonitrile is representative
Polymer sulphur positive electrode.Sulphur in this two classes sulphur positive pole combined with electrode material it is closer, can be using conventional carbonic acid
Esters electrolyte, circulating battery stability is also relatively good.But, sulfur content is very low in this two classes sulphur positive pole, is usually no more than
50%, therefore be difficult the lithium-sulfur cell for obtaining higher energy density.Therefore, the influence to battery performance such as reduction shuttle effect,
The heat endurance of sulfur content and raising battery effectively in lifting sulphur positive pole is to realize the only way which must be passed of lithium-sulfur cell industrialization.
Meanwhile, there is some document reports high concentration lithium salt electrolyte answering in lithium ion battery and lithium-sulfur cell
With, mainly use between solvent molecule and lithium ion strong solvation reduce electrode, collector etc. and electrolyte it
Between side reaction.Therefore, high concentration electrolyte is improving electrolyte oxidative resistance, reducing resistance and the corruption for suppressing current collector aluminum foil
Significant advantage is shown in terms of erosion.Meanwhile, the high concentration lithium salt electrolyte of non-EC bases also contributes to graphite cathode surface SEI films
Formation, will not occur the stripping of graphite.But the carbonates electrolyte still not on high concentration is applied to lithium-sulfur cell
Report.
The content of the invention
It is an object of the invention to provide a kind of high concentration esters battery electrolyte, it is adaptable to lithium-sulfur cell, can solve
The problem of shuttle effect and bad battery heat endurance that ethers electrolyte is brought.
The present invention provides following technical scheme：
A kind of high concentration esters electrolyte for lithium-sulfur cell,
The electrolyte contains lithium salts and organic solvent；
The molar concentration of the lithium salts in the electrolytic solution is higher than 3.0mol/L；And the organic solvent is selected from carbonic ester and carboxylic
Acid esters or the mixing of the two.As preferred, the molar concentration of the lithium salts in the electrolytic solution is higher than 4.5mol/L.
The lithium salts is generally selected from LiPF6, LiBF4、LiBOB、LiDFOB、LiPO2F2、LiSO3CF3, bis trifluoromethyl sulphur
At least one of imide li (LiTFSI), double fluorine sulfimide lithiums (LiFSI).
In the electrolyte, selected carbonic ester is：Dimethyl carbonate, diethyl carbonate, dipropyl carbonate, carbonic acid first
At least one of base ethyl ester, ethylene carbonate, propene carbonate, gamma-butyrolacton, butylene carbonate.
In the electrolyte, carboxylate is：Methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methyl propionate, third
At least one of acetoacetic ester, methyl butyrate, ethyl butyrate.
A kind of lithium-sulfur cell, the battery uses above-mentioned electrolyte, and contains S in the positive pole of lithium-sulfur cell8It is used as activity
Material.
The beneficial effects of the present invention are：
The present invention proposes to be used as lithium-sulfur cell electrolyte using the esters electrolyte of high concentration.First, high concentration electrolyte
In all solvent molecules be involved in Li+ solvated layer, thus without free solvent molecule and production in the middle of lithium-sulfur cell
The many lithium sulfides of thing react.Meanwhile, high concentration electrolyte is in saturation state, and more many lithium sulfides are not had and are dissolved in electricity
Solve in liquid, thus there is higher coulombic efficiency using the lithium-sulfur cell of this electrolyte, do not shuttle effect.3rd, the electrolysis
Liquid, as solvent, with higher boiling point, thus improves the heat endurance and security of battery using carbonates.4th,
The high concentration esters electrolyte is applied to elemental sulfur as the lithium-sulfur cell of positive pole, relative to small molecule sulphur positive pole and vulcanization poly- third
For alkene nitrile positive pole, positive active material content is high, is conducive to obtaining the higher lithium-sulfur cell of energy density.
Embodiment
The present invention is further described with reference to specific embodiment, but does not limit the invention to these tools
Body embodiment.One skilled in the art would recognize that present invention encompasses potentially included in Claims scope
All alternatives, improvement project and equivalents.
The Solvent abbreviations used in following examples are as follows：
Dimethyl carbonate is DMC, and ethylene carbonate is EC, and methyl ethyl carbonate is EMC, and ethyl acetate is EA, methyl acetate
For MA.
Embodiment 1
A kind of lithium-ion battery electrolytes, including two kinds of carbonate solvents of EC, EMC, using LiTFSI as lithium salts.Its preparation side
Method is：By EC, EMC 3: 7 mixing by volume, LiTFSI is then added, concentration is allowed to and reaches 5.0mol/L, obtain lithium-ion electric
Pond electrolyte.
Embodiment 2
A kind of lithium-ion battery electrolytes, including two kinds of carbonate solvents of EC, EMC, with LiPF6For lithium salts.Its preparation side
Method is：By EC, EMC 3: 7 mixing by volume, LiPF is then added6, it is allowed to concentration and reaches 5.0mol/L, obtains lithium-ion electric
Pond electrolyte.
Embodiment 3
A kind of lithium-ion battery electrolytes, including two kinds of solvents of EC, EA, using LiTFSI as lithium salts.Its preparation method is：Will
EC, EA 3: 7 mixing by volume, then add LiTFSI, are allowed to concentration and reach 6.0mol/L, obtain lithium ion battery electrolysis
Liquid.
Embodiment 4
A kind of lithium-ion battery electrolytes, including two kinds of solvents of EC, MA, using LiFSI as lithium salts.Its preparation method is：Will
EC, MA 3: 7 mixing by volume, then add LiFSI, are allowed to concentration and reach 6.0mol/L, obtain lithium-ion battery electrolytes.
Embodiment 5
A kind of lithium-ion battery electrolytes, including two kinds of carbonate solvents of EC, EMC, using LiBOB as lithium salts.Its preparation side
Method is：By EC, EMC 3: 7 mixing by volume, LiBOB is then added, concentration is allowed to and reaches 4.0mol/L, obtain lithium-ion electric
Pond electrolyte.
Comparative example 1
A kind of lithium-ion battery electrolytes, including ethylene carbonate, two kinds of carbonate solvents of methyl ethyl carbonate, with LiTFSI
For lithium salts.Its preparation method is：By 3: 7 mixing by volume of ethylene carbonate, methyl ethyl carbonate, LiTFSI is then added, is made
Concentration reach 1.0mol/L.
Comparative example 2
A kind of lithium-ion battery electrolytes, including ethylene carbonate, two kinds of carbonate solvents of methyl ethyl carbonate, with LiFSI
For lithium salts.Its preparation method is：By 3: 7 mixing by volume of ethylene carbonate, methyl ethyl carbonate, LiFSI is then added, is allowed to
Concentration reaches 1.0mol/L.
Comparative example 3
A kind of lithium-ion battery electrolytes, including glycol dimethyl ether, 1,3 two kinds of dioxolanes solvents, using LiTFSI as
Lithium salts.Its preparation method is：By glycol dimethyl ether, 1, then 3 dioxolanes, 1: 1 mixing by volume adds LiTFSI, makes
Concentration reach 1.0mol/L, obtain lithium-ion battery electrolytes.
The electrolyte that embodiment 1 to 5 and comparative example 1 to 3 are prepared, is tested.Main method of testing：By quality
Than for 2:After 1 sulphur and Ketjen black is well mixed, application of vacuum 12h obtains sulphur carbon composite at 155 DEG C.Sulphur carbon is combined
Material：Acetylene black：Hydroxymethyl cellulose+butadiene-styrene rubber=8:1:1 is distributed in appropriate water, and electrode slurry is obtained after ball milling 6h
Material.Obtained slurry is coated on aluminium foil, after being dried under infrared lamp, 12h is dried at 60 DEG C of vacuum, a diameter of 14mm is cut into
Electrode slice it is standby.Afterwards, it is barrier film assembling lithium-sulfur cell for negative pole, Cegrald2400 to use above-mentioned electrolyte, lithium metal,
The cycle performance tested under 0.2C multiplying powers after the circulation 50 weeks of lithium-sulfur cell.Test result is as follows：
Table 1
As shown in Table 1, only had using the lithium-sulfur cell first discharge specific capacity of the esters electrolyte of low concentration more than 400
MAh.g-1, is consumed by esters solvent corresponding to many lithium sulfides of generation, can not subsequently circulate.Esters proposed by the present invention are highly concentrated
Degree electrolyte shows significant advantage applied to lithium-sulfur cell, is that battery first discharge specific capacity is higher first.Secondly, battery
With more preferable cyclical stability, the capability retention of battery reaches 90% or so after circulation 50 weeks, hence it is evident that higher than using ether
80% or so of class electrolyte.3rd, due to the influence of shuttle effect, using the average coulomb effect of the lithium-sulfur cell of ethers electrolyte
Rate only has 80.6%, and use high concentration esters electrolyte lithium-sulfur cell avoid the dissolving of many lithium sulfides in the electrolytic solution and
Migration, thus battery coulombic efficiency is promoted to more than 99%.
Claims (7)
1. a kind of high concentration esters electrolyte for lithium-sulfur cell, it is characterised in that：Described electrolyte contains lithium salts and had
Machine solvent, and the molar concentration of described lithium salts in the electrolytic solution is higher than 3.0mol/L, described organic solvent for carbonic ester or
Carboxylate or the mixing of the two.
2. according to the high concentration esters electrolyte for lithium-sulfur cell described in claim 1, it is characterised in that：Described lithium salts
Molar concentration in the electrolytic solution is higher than 4.5mol/L.
3. according to the high concentration esters electrolyte for lithium-sulfur cell described in claim 1, it is characterised in that：Described lithium salts
Selected from LiPF6、LiBF4、LiBOB、LiDFOB、LiPO2F2、LiSO3CF3, bis trifluoromethyl sulfimide lithium (LiTFSI), double fluorine
At least one of sulfimide lithium (LiFSI).
4. according to the high concentration esters electrolyte for lithium-sulfur cell described in claim 1, it is characterised in that：Selected carbon
Acid esters is：Dimethyl carbonate, diethyl carbonate, dipropyl carbonate, methyl ethyl ester, ethylene carbonate, propene carbonate,
At least one of gamma-butyrolacton, butylene carbonate.
5. according to the high concentration esters electrolyte for lithium-sulfur cell described in claim 1, it is characterised in that：Selected carboxylic
Acid esters is：Methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methyl propionate, ethyl propionate, methyl butyrate, butyric acid second
At least one of ester.
6. a kind of lithium-sulfur cell, it is characterised in that：Using electrolyte as claimed in claim 1.
7. according to the lithium-sulfur cell described in claim 6, it is characterised in that：Contain S in the positive pole of the lithium-sulfur cell8It is used as activity
Material.
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| CN201710141187.0A CN107069093B (en) | 2017-03-10 | 2017-03-10 | High-concentration ester electrolyte for lithium-sulfur battery |
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| CN201710141187.0A CN107069093B (en) | 2017-03-10 | 2017-03-10 | High-concentration ester electrolyte for lithium-sulfur battery |
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| CN108232302A (en) * | 2017-12-30 | 2018-06-29 | 国联汽车动力电池研究院有限责任公司 | A kind of high concentration lithium salt electrolyte suitable for silicon-based anode lithium ion battery |
| CN108832149A (en) * | 2018-06-15 | 2018-11-16 | 中国计量大学 | Lithium-sulfur cell electrolyte of one kind and lithium-sulfur cell |
| GB2577114A (en) * | 2018-09-14 | 2020-03-18 | Oxis Energy Ltd | Battery |
| CN110911756A (en) * | 2019-11-28 | 2020-03-24 | 华中科技大学 | Diluted lithium salt mixed lithium-sulfur battery electrolyte |
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| EP3641020A4 (en) * | 2017-09-01 | 2020-08-12 | LG Chem, Ltd. | Method for manufacturing electrochemical device |
| CN111640939A (en) * | 2020-05-22 | 2020-09-08 | 华中科技大学 | Sulfur cathode material based on solid-phase reaction mechanism and preparation method thereof |
| CN113972399A (en) * | 2021-10-25 | 2022-01-25 | 郑州中科新兴产业技术研究院 | Local high-concentration lithium-sulfur battery electrolyte |
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| CN108232302A (en) * | 2017-12-30 | 2018-06-29 | 国联汽车动力电池研究院有限责任公司 | A kind of high concentration lithium salt electrolyte suitable for silicon-based anode lithium ion battery |
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| CN111640939A (en) * | 2020-05-22 | 2020-09-08 | 华中科技大学 | Sulfur cathode material based on solid-phase reaction mechanism and preparation method thereof |
| CN113972399A (en) * | 2021-10-25 | 2022-01-25 | 郑州中科新兴产业技术研究院 | Local high-concentration lithium-sulfur battery electrolyte |
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