CN105977534A - Functional electrolyte for secondary lithium-sulfur battery and preparation method thereof - Google Patents
Functional electrolyte for secondary lithium-sulfur battery and preparation method thereof Download PDFInfo
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- CN105977534A CN105977534A CN201610453973.XA CN201610453973A CN105977534A CN 105977534 A CN105977534 A CN 105977534A CN 201610453973 A CN201610453973 A CN 201610453973A CN 105977534 A CN105977534 A CN 105977534A
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- electrolyte
- sulfur battery
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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
- H01M10/0567—Liquid materials characterised by the additives
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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 relates to a functional electrolyte for a secondary lithium-sulfur battery and a preparation method thereof. The electrolyte includes lithium salt, an organic solvent and an additive. A concentration of the lithium salt in the electrolyte is 0.5-5mol/L. A mass percent concentration of the additive in the electrolyte is 0.1-30%. The preparation method includes the steps of adding the lithium salt into the organic solvent, stirring uniformly so as to prepare the electrolyte, then adding the additive into the electrolyte, and continuing to stir till mixing uniformly, so as to obtain the functional electrolyte for the secondary lithium-sulfur battery. Compared with the prior art, a stable interface protection membrane is formed on the positive electrode surface, capacity retention rate and rate discharge capacity of a lithium-sulfur battery are improved remarkably, and the electrochemical performance of the lithium-sulfur battery is enhanced.
Description
Technical field
The present invention relates to a kind of electrolyte and preparation method thereof, especially relate to a kind of secondary lithium-sulfur battery function
Electrolyte and preparation method thereof.
Background technology
Conventional lithium ion battery is held quantitative limitation by its positive electrode, energy density relatively low (about 150Wh kg-1),
The demand of Large Electric car cannot be met, and chargeable lithium-sulfur cell has appreciable theoretical energy density
(2600Wh kg-1).Based on the research before us, Li/S@pPAN battery is at 1M LiPF6/EC+DMC
(1:1, v/v) electrolyte system shows best cycle performance, but its capability retention and high rate performance are still
Have much room for improvement.This mainly can be attributed in lithium-sulfur cell charge and discharge process, due to the organic solvent in electrolyte
And lithium salts decomposes generation gas and the formation of organic compound participation solid electrolyte membrane, at S@pPAN just cause
Surface, pole fails to form one layer of stable SEI film.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and provide a kind of capacity that improves to protect
Secondary lithium-sulfur battery function electrolyte of holdup and high rate performance and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of secondary lithium-sulfur battery function electrolyte, comprises lithium salts, organic solvent and additive, described lithium salts
Concentration in the electrolytic solution is 0.5-5mol/L, and described additive mass percent concentration in the electrolytic solution is
0.1-30%.
Described additive is selected from three (trimethyl silane) borate (TMSB), tricresyl phosphate (2,2,2-trifluoro second
Base) one or more in ester (TFEP) or ethyoxyl five fluorine ring three phosphonitrile (PFPN).Such additive energy
Interfacial film that one layer fine and close, that resistivity is low is formed, it is to avoid electrolyte and electrode material carry out pair at sulfur positive electrode surface
Reaction, plays the effect of stable interface, considerably improves cyclical stability and the high rate performance of lithium-sulfur rechargeable battery.
Preferably, additive is three (trimethyl silane) borate (TMSB).
Preferably, additive is ethyoxyl five fluorine ring three phosphonitrile (PFPN).
Very little, effect is little for addition, adds too many, and owing to additive viscosity is relatively large, cost is of a relatively high,
All battery performance and application are produced harmful effect, therefore preferably, additive mass percent in the electrolytic solution is dense
Degree is 1-20%.
Described lithium salts is LiPF6、LiBF4、LiBOB、LiBC2O4F2、LiClO4、LiCF3SO3、LiN(FSO2)2
Or LiN (CF3SO2)2One or more.
One or more in carbonate based organic solvent or ether organic solvent of described organic solvent.
Preferably, carbonate based organic solvent be ethylene carbonate, vinylene carbonate, fluorinated ethylene carbonate,
One or more of Allyl carbonate, ethyl methyl carbonate, dimethyl carbonate or diethyl carbonate.
Preferably, ether organic solvent is dioxolane, dioxane, glycol dimethyl ether, diethylene glycol diformazan
One or more in ether, tetraethyleneglycol dimethyl ether, ethylene glycol diethyl ether or diethylene glycol diethyl ether.
The preparation method of a kind of secondary lithium-sulfur battery function electrolyte, adds lithium salts in organic solvent, and stirring is all
It is configured to electrolyte after even, in electrolyte, then adds additive, continue to stir to mix homogeneously, i.e. obtain two
Secondary lithium-sulfur cell function electrolyte.
The secondary lithium-sulfur battery that the function electrolyte prepared assembles, its sulfenyl material used is elemental sulfur S8、
Many lithium sulfides, sulfenyl composite, organosulfur compound or carbon-sulfur polymer;
Described many lithium sulfides chemical formula is: Li2Sn, wherein, 1≤n≤8;
Described carbon-sulfur polymer chemical formula is: (C2Sx)n, wherein, x is 2~20, n >=2;
Described sulfenyl composite is: after elemental sulfur mixes with polyacrylonitrile in mass ratio 2~16:1, protects at nitrogen
Protect down and be heated to 250~400 DEG C and be incubated and obtain for 1~16 hour.This kind of function electrolyte and sulfur positive electrode
Compatible good, battery performance is had and arrives very much raising.
Compared with prior art, the present invention can significantly increase the chemical property of secondary lithium-sulfur battery, reaches to carry
High power capacity conservation rate and the purpose of high rate performance.Three (trimethyl silane) Borated Ester Additives such as added can be
Sulfur positive electrode surface forms interfacial film that one layer fine and close, that resistivity is low, thus considerably improves lithium-sulfur rechargeable battery
Cyclical stability and high rate performance.
Accompanying drawing explanation
Fig. 1 is the electrolytic conductivity curve chart with three (trimethyl silane) borate changes of contents;
Fig. 2 is that the lithium-sulfur cell assembled by the electrolyte of different three (trimethyl silane) borate content follows first
The lower AC impedance figure surveyed of open circuit after ring;
Fig. 3 is that the lithium-sulfur cell assembled by the electrolyte of different three (trimethyl silane) borate content is the most forthright
Can comparison diagram;
Fig. 4 is that the lithium-sulfur cell assembled by the electrolyte of different three (trimethyl silane) borate content is in room temperature
Under the conditions of cycle performance and coulombic efficiency figure;
Fig. 5 is that the lithium-sulfur cell assembled by the electrolyte of different three (trimethyl silane) borate content is at high temperature
Cycle performance under condition (60 DEG C) and coulombic efficiency figure.
Detailed description of the invention
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.Following example will assist in ability
The technical staff in territory is further appreciated by the present invention, but limits the present invention the most in any form.It should be pointed out that, it is right
For those of ordinary skill in the art, without departing from the inventive concept of the premise, it is also possible to make some adjustment
And improvement.These broadly fall into protection scope of the present invention.
Embodiment 1
1:1 uniform mixed carbonic acid vinyl acetate and ethyl methyl carbonate by volume in glove box, molten to this mixing
Agent adds LiPF6, stir, make the electrolyte that concentration is 0.5mol/L.Add in this electrolyte again
Three (trimethyl silane) Borated Ester Additives, obtains function electrolyte, and described additive accounts for the quality of electrolyte gross weight
Degree is respectively 0.1%, and 1%, 2.5%, 5%, 10%.
Embodiment 2
1:3 uniform mixed carbonic acid vinyl acetate and glycol dimethyl ether by volume in glove box, to this mixed solvent
Middle addition LiN (FSO2)2, stir, make the electrolyte that concentration is 5mol/L.Add in this electrolyte again
Entering tricresyl phosphate (2,2,2-trifluoroethyl) ester additive, obtain function electrolyte, described additive accounts for electrolyte gross weight
Mass percentage content be respectively 0.1%, 5%, 10%, 20%, 30%.
Embodiment 3
In glove box, 1:4 uniformly mixes dioxolane and glycol dimethyl ether by volume, in this mixed solvent
Add LiN (CF3SO2)2With LiN (FSO2)2Each 1mol/L, stirs.Ethoxy is added again in this electrolyte
Base five fluorine ring three phosphonitrile (PFPN) additive, obtains function electrolyte, and described additive accounts for the matter of electrolyte gross weight
Amount degree is respectively 1%, and 5%, 10%, 20%.
Embodiment 4
In glove box, 1:3:3 uniformly mixes fluorinated ethylene carbonate, dioxolane and diethylene glycol two by volume
Methyl ether, adds LiN (FSO in this mixed solvent2)2, stir, make the electrolyte that concentration is 2mol/L.
Tricresyl phosphate (2,2,2-trifluoroethyl) ester of the weight such as addition and three (trimethyl silane) boron in this electrolyte again
Acid esters additive, obtains function electrolyte, and described additive accounts for the mass percentage content of electrolyte gross weight and is respectively
1%, 5%, 10%, 20%.
Embodiment 5
Electrical conductivity is tested
It is respectively 0% with additive level under conductivity measurement test room temperature, 0.5%, 1%, 2.5%, 5%,
The electrical conductivity of 10% electrolyte (electrolyte of embodiment 1), it is judged that the additive impact on electrolytic conductivity.
Electrolyte is poured into respectively in inlab 710 electrical conductivity test pond (Metter Toledo, Switzerland), use FE30
Its electrical conductivity tested by conductivity meter, and result is shown in Fig. 1.As shown in Figure 1, a small amount of additive electricity to blank electrolysis liquid
Conductance impact is less.
Embodiment 6
It is assembled into battery and carries out electrochemical property test
The preparation of positive electrode: by sulfenyl material, conductive carbon Super P, binding agent PTFE 80:10:10 in proportion
Uniformly mixing, adds ethanol in proper amount dispersion, heats up and boil off excess of solvent, roll film forming with roll squeezer, make diameter
The disk of 12mm, is pressed in nickel foam.This sulfenyl material is that sulfenyl composite is: elemental sulfur and polyacrylonitrile
After 10:1 in mass ratio (can be arbitrary value in 4~16:1) mixing, being heated to 300 DEG C under nitrogen protection (can
It is arbitrary value in 250~400 DEG C) and (can be arbitrary value in 1~16 hour) obtains to be incubated 12 hours.
The assembling of battery and test: with ENTEK PE film as barrier film, lithium sheet is negative pole, and additive level is respectively
It is 0.5%, the electrolyte (electrolyte in embodiment 1) of 1%, 2.5%, 5%, 10% and blank electrolysis liquid,
And sulfur-based positive electrode forms 2016 type button cells, between 1.0~3.0V, carry out charge-discharge test, use
CHI604D electrochemical workstation test battery AC impedance under open-circuit voltage.
Each button cell impedance after the circulation of charge and discharge first is as shown in Figure 2.Along with the increase of additive level, electrode
The impedance of/electrolyte interface significantly increases, and particularly when additive level is 10%, electrochemical impedance significantly increases.
The high rate performance of lithium-sulfur cell containing the most commensurability additive compares as it is shown on figure 3, along with the increase of additive level,
Its high rate performance is substantially deteriorated, and when the amount of additive is 1%, the high rate performance of corresponding lithium-sulfur cell behaves oneself best.
The repeatedly charge-discharge test of the lithium-sulfur cell assembled by the electrolyte of 1% 3 (trimethyl silane) borate content
Result such as Fig. 4 (room temperature), shown in Fig. 5 (high temperature 60 DEG C), when additive level is 1%, lithium-sulfur cell exists
Cyclical stability under room temperature and high temperature is all significantly improved.
Claims (10)
1. a secondary lithium-sulfur battery function electrolyte, it is characterised in that this electrolyte comprises lithium salts, organic
Solvent and additive, described lithium salts concentration in the electrolytic solution is 0.5-5mol/L, and described additive is in electrolysis
Mass percent concentration in liquid is 0.1-30%.
A kind of secondary lithium-sulfur battery function electrolyte the most according to claim 1, it is characterised in that institute
The additive stated is selected from three (trimethyl silane) borate (TMSB), tricresyl phosphate (2,2,2-trifluoroethyl) ester
(TFEP) one or more or in ethyoxyl five fluorine ring three phosphonitrile (PFPN).
A kind of secondary lithium-sulfur battery function electrolyte the most according to claim 1, it is characterised in that institute
The additive stated preferably three (trimethyl silane) borate (TMSB).
A kind of secondary lithium-sulfur battery function electrolyte the most according to claim 1, it is characterised in that institute
The additive preferred ethyoxyl five fluorine ring three phosphonitrile (PFPN) stated.
5., according to a kind of secondary lithium-sulfur battery function electrolyte according to any one of claim 1-4, it is special
Levying and be, described additive mass percent concentration in the electrolytic solution is preferably 1-20%.
A kind of secondary lithium-sulfur battery function electrolyte the most according to claim 1, it is characterised in that institute
The lithium salts stated is LiPF6、LiBF4、LiBOB、LiBC2O4F2、LiClO4、LiCF3SO3、LiN(FSO2)2
Or LiN (CF3SO2)2One or more.
A kind of secondary lithium-sulfur battery function electrolyte the most according to claim 1, it is characterised in that institute
One or more in carbonate based organic solvent or ether organic solvent of the organic solvent stated.
A kind of secondary lithium-sulfur battery function electrolyte the most according to claim 7, it is characterised in that institute
The carbonate based organic solvent stated is ethylene carbonate, vinylene carbonate, fluorinated ethylene carbonate, propylene carbonate
One or more of ester, ethyl methyl carbonate, dimethyl carbonate or diethyl carbonate.
A kind of secondary lithium-sulfur battery function electrolyte the most according to claim 7, it is characterised in that institute
The ether organic solvent stated is dioxolane, dioxane, glycol dimethyl ether, diethylene glycol dimethyl ether, tetrem
One or more in glycol dimethyl ether, ethylene glycol diethyl ether or diethylene glycol diethyl ether.
The preparation method of a kind of secondary lithium-sulfur battery function electrolyte the most as claimed in claim 1, its feature
It is, the party's normal direction organic solvent adds lithium salts, is configured to electrolyte after stirring, then in electrolyte
Add additive, continue to stir to mix homogeneously, i.e. obtain secondary lithium-sulfur battery function electrolyte.
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Cited By (12)
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CN106450455A (en) * | 2016-10-20 | 2017-02-22 | 重庆工业职业技术学院 | High-efficiency lithium-sulfur battery additive and application method thereof |
CN107181004A (en) * | 2017-07-05 | 2017-09-19 | 山东大学 | A kind of lithium-sulfur cell electrolyte and the lithium-sulfur cell using the electrolyte |
CN108336405A (en) * | 2017-12-18 | 2018-07-27 | 合肥国轩高科动力能源有限公司 | A kind of lithium-sulfur cell function electrolyte and preparation method thereof |
CN109411816A (en) * | 2018-10-25 | 2019-03-01 | 河南省法恩莱特新能源科技有限公司 | A kind of high magnification electrolyte of lithium ion battery |
CN109599592A (en) * | 2018-11-07 | 2019-04-09 | 上海交通大学 | A kind of secondary lithium-sulfur battery intrinsic safety electrolyte and preparation method thereof |
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CN106450455B (en) * | 2016-10-20 | 2018-12-21 | 重庆工业职业技术学院 | A kind of efficient lithium-sulfur cell additive |
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CN107181004B (en) * | 2017-07-05 | 2019-12-06 | 山东大学 | Lithium-sulfur battery electrolyte and lithium-sulfur battery using same |
CN107181004A (en) * | 2017-07-05 | 2017-09-19 | 山东大学 | A kind of lithium-sulfur cell electrolyte and the lithium-sulfur cell using the electrolyte |
CN108336405A (en) * | 2017-12-18 | 2018-07-27 | 合肥国轩高科动力能源有限公司 | A kind of lithium-sulfur cell function electrolyte and preparation method thereof |
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CN110611084A (en) * | 2018-06-15 | 2019-12-24 | 武汉大学 | Lithium-sulfur secondary battery with long cycle life and 100% coulombic efficiency |
CN109411816A (en) * | 2018-10-25 | 2019-03-01 | 河南省法恩莱特新能源科技有限公司 | A kind of high magnification electrolyte of lithium ion battery |
CN109599592A (en) * | 2018-11-07 | 2019-04-09 | 上海交通大学 | A kind of secondary lithium-sulfur battery intrinsic safety electrolyte and preparation method thereof |
CN111384441A (en) * | 2018-12-27 | 2020-07-07 | 浙江省化工研究院有限公司 | Battery electrolyte additive, electrolyte containing additive and lithium ion battery |
CN110350251A (en) * | 2019-07-26 | 2019-10-18 | 南京海泰纳米材料有限公司 | A kind of high-temperature and high-presure resistent sulphur electrolyte for lithium cells and preparation method thereof |
CN110350251B (en) * | 2019-07-26 | 2020-09-11 | 南京海泰纳米材料有限公司 | Electrolyte for high-temperature and high-pressure resistant sulfur lithium battery and preparation method thereof |
JPWO2021090666A1 (en) * | 2019-11-05 | 2021-05-14 | ||
JP7169604B2 (en) | 2019-11-05 | 2022-11-11 | 学校法人 関西大学 | Electrolyte, Lithium Sulfur Secondary Battery and Module |
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 |
CN111755745A (en) * | 2020-06-18 | 2020-10-09 | 合肥国轩高科动力能源有限公司 | Lithium-sulfur battery electrolyte and liquid injection method thereof |
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CN114512733A (en) * | 2022-01-21 | 2022-05-17 | 厦门大学 | Method for improving electrochemical performance of lithium-sulfur battery |
CN114512733B (en) * | 2022-01-21 | 2024-02-27 | 厦门大学 | Method for improving electrochemical performance of lithium-sulfur battery |
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Application publication date: 20160928 |