CN107342438A - A kind of high coulombic efficiency lithium-sulfur cell electrolyte and preparation method thereof - Google Patents
A kind of high coulombic efficiency lithium-sulfur cell electrolyte and preparation method thereof Download PDFInfo
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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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- 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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Abstract
The present invention relates to a kind of high coulombic efficiency lithium-sulfur cell electrolyte and preparation method thereof, and it includes ether organic solvent, lithium salts and esters additive, and the esters additive is one or more mixtures formed in carbonic ester and sulfite；Mixed using specific additive with ether organic solvent, lithium salts, so as to be reacted in charge and discharge process with caused polysulfide in lithium-sulfur cell charge and discharge process, and then suppress shuttling for polysulfide, the effective shuttle effect for suppressing lithium-sulfur cell, improve the cycle life and coulombic efficiency of lithium-sulfur cell.
Description
Technical field
The invention belongs to lithium-sulfur cell field, is related to a kind of lithium-sulfur cell electrolyte, and in particular to a kind of high coulombic efficiency
Lithium-sulfur cell electrolyte and preparation method thereof.
Background technology
The development of modern society, fossil energy consumption occupy increasing ratio in energy resource consumption, and development is sustainable
Clean energy resource is extremely urgent.How the lasting consumption of problem of environmental pollution and fossil energy to be solved, efficient energy storage device,
It is sustainable renewable sources of energy industry, consumer electronics industry, the core of transportation industry as instantly most popular research and development direction
Heart pillar.
In many energy storage modes, lithium ion battery due to self discharge is small, it is higher than energy, have extended cycle life, charge power
Scope is wide and the advantages that light weight, core status is occupied in current energy storage device.Most lithium battery is regarded with carbon material
Negative pole, lithium piece are positive pole, and shuttled contribution capacity using lithium ion between both positive and negative polarity.Sony in 1991 releases business first
After the lithium ion battery of change, lithium ion battery starts to be widely used in the portable electronics such as mobile phone, notebook computer, digital camera
Product, and as popularization of these products in the whole world, the market demand of lithium ion battery are always maintained at a relatively high growth rate,
Market for the great demand of lithium ion battery also guide lithium ion battery industry continue enhancement and as the whole world is to electronic
The growing interest of automobile, also makes it possible application of the lithium ion battery in terms of electric car.It is existing by the development of more than 20 years
Lithium ion battery close to its theoretical capacity, but still the electronics industry of high speed development and emerging electric automobile etc. can not be met
The requirement of industry, it is extremely urgent to find the battery system with higher energy density.
Lithium-sulfur cell system has high theoretical energy density, is most potential one kind two in a variety of energy-storage systems
Primary cell.Lithium-sulfur cell uses naturally abundant element sulphur to have very high theoretical specific volume (1675mAh/g) as negative material
It it is more than five times of the theoretical capacity of lithium ion battery with higher energy density (2500Wh/kg).With traditional lithium ion battery
Mechanism is different, and lithium-sulfur cell is gone back by the multiphase conversion oxidation between element sulphur, soluble polysulfide and insoluble lithium sulfide
Original is reacted to provide high power capacity.However, the polysulfide as intermediate, can be dissolved in liquid organic electrolyte, cause
Serious shuttle effect, causes the loss of active material.Meanwhile and serious parasitic reaction occurs with lithium anode, reduce the circulation longevity
Life, causes especially low coulombic efficiency.Further, since the insulating properties of element sulphur and the volumetric expansion (≈ in charge and discharge process
80%) lithium-sulfur cell cycle life, is further resulted in shorten and charge efficiency reduction.How the coulomb effect of lithium-sulfur cell is improved
Rate, researcher propose more improvement project.These schemes concentrate on the negative material of battery, and negative material is changed
Enter, often can all bring the preparation technology of complexity, and improve the cost of battery.It is one to develop new lithium-sulfur cell electrolyte
Facilitate one of feasible direction.
The content of the invention
A kind of high coulombic efficiency lithium-sulfur cell electrolyte is provided the invention aims to overcome the deficiencies in the prior art.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：A kind of high coulombic efficiency lithium-sulfur cell electrolyte, it
Including ether organic solvent, lithium salts and esters additive, the esters additive is one in carbonic ester and sulfite
The mixture of kind or a variety of compositions.
Optimally, the mass fraction of the esters additive is 0.5~5%.
Further, the mass fraction of the esters additive is 1~3%.
Optimally, the general structure of the esters additive is In formula, 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 esters additive is the one or more in following structural formula,
Further, the structural formula of the esters additive is
Optimally, the ether organic solvent is glycol dimethyl ether and 1, the mixture of 3 dioxolanes, and its volume ratio is
1：1.
Optimally, the concentration of the lithium salts is 0.8~1.2mol/L.
Further, the lithium salts is two (trimethyl fluoride sulfonyl) imine lithiums.
A further object of the present invention is to provide a kind of preparation method of above-mentioned high coulombic efficiency lithium-sulfur cell electrolyte, it
Comprise the following steps：
(a) lithium salts is added into the ether organic solvent, stirring makes its dissolving；
(b) carbonates additive is added in the mixture obtained to step (a), stirring dissolves it.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：The high coulomb effect of the present invention
Rate lithium-sulfur cell electrolyte, using specific additive and ether organic solvent, lithium salts, so as in charge and discharge process with
Caused polysulfide reacts in lithium-sulfur cell charge and discharge process, and then suppresses shuttling for polysulfide, effectively
Suppress the shuttle effect of lithium-sulfur cell, improve the cycle life and coulombic efficiency of lithium-sulfur cell.
Brief description of the drawings
Fig. 1 is that high coulombic efficiency lithium-sulfur cell electrolyte is assembled into average coulombic efficiency after lithium-sulfur cell in embodiment 1-5
Comparison diagram；
Fig. 2 is that high coulombic efficiency lithium-sulfur cell electrolyte is assembled into the circulating effect figure after lithium-sulfur cell in embodiment 4；
Fig. 3 is that high coulombic efficiency lithium-sulfur cell electrolyte is assembled into charging and discharging curve after lithium-sulfur cell in embodiment 4；
Fig. 4 is coulombic efficiency comparison diagram in the embodiment of the present invention 2, embodiment 4 and comparative example 1；
Fig. 5 is coulombic efficiency comparison diagram in the embodiment of the present invention 4, comparative example 1 and comparative example 2.
Embodiment
The high coulombic efficiency lithium-sulfur cell electrolyte of the present invention, it includes ether organic solvent, lithium salts and esters additive, institute
State mixture of the esters additive for one or more compositions in carbonic ester and sulfite；Using specific additive
Mixed with ether organic solvent, lithium salts, so as in charge and discharge process with being produced in lithium-sulfur cell charge and discharge process
Polysulfide react, and then suppress polysulfide and shuttle, the effective shuttle effect for suppressing lithium-sulfur cell, carry
The cycle life and coulombic efficiency of high lithium-sulfur cell.
The mass fraction of above-mentioned esters additive is preferably 0.5~5%, and more excellent is 1~3%.The esters additive
General structure is preferablyIn formula, Z
For C or S, R1And R2Independently of one another alkyl or phenyl, R3And R4Independently of one another hydrogen or nitro, R5And R6Independently of each other
For H or F；The more excellent one or more in following structural formula, It is optimal to beThe ether organic solvent is preferably glycol dimethyl ether and 1,3 dioxolanes
Mixture, its volume ratio are 1：1.The concentration of the lithium salts is preferably 0.8~1.2mol/L, preferably two (trimethyl fluoride sulfonyls)
Imine lithium.The preparation method of above-mentioned high coulombic efficiency lithium-sulfur cell electrolyte, it comprises the following steps：(a) have to the ethers
Lithium salts is added in solvent, stirring makes its dissolving；(b) carbonates additive is added in the mixture obtained to step (a), is stirred
Mixing dissolves it.
The present invention is further described below in conjunction with embodiment.
Embodiment 1
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, and its preparation method is specially：
(a) two (trimethyl fluoride sulfonyl) imine lithiums are put into glove box and fully dried；After fully drying, body is added
Product is than being 1：1 glycol dimethyl ether and 1, in 3 dioxolanes ethers mixed organic solvents, sufficiently stirred, until complete
Fully dissolved；
(b) double (4- nitrobenzene) carbonic esters (No. CAS of additive are added in the mixture obtained to step (a)：5070-13-
3, additive mass ratio in the mixed solution of formation is 0.5wt%), it is sufficiently stirred, after to be added dose is completely dissolved, stands 24
Hour.
Embodiment 2
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 1
Unanimously, unlike：Additive mass ratio in the mixed solution of formation is 1wt%.
Embodiment 3
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 1
Unanimously, unlike：Additive mass ratio in the mixed solution of formation is 2wt%.
Embodiment 4
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 1
Unanimously, unlike：Additive mass ratio in the mixed solution of formation is 3wt%., specific electrochemical test data is as schemed
Shown in 2 and Fig. 3.
Embodiment 5
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 1
Unanimously, unlike：Additive mass ratio in the mixed solution of formation is 5wt%.
Embodiment 6
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 4
Unanimously, unlike：Additive has changed methyl ethyl carbonate into.
Embodiment 7
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 4
Unanimously, unlike：Additive has changed dimethyl carbonate into.
Embodiment 8
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 4
Unanimously, unlike：Additive has changed fluorinated ethylene carbonate into.
Embodiment 9
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 4
Unanimously, unlike：Additive has changed propene carbonate into.
Embodiment 10
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 4
Unanimously, unlike：Additive has changed ethylene carbonate into.
Embodiment 11
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 4
Unanimously, unlike：Additive has changed tert-butyl-phenyl carbonic ester into.
Embodiment 12
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 4
Unanimously, unlike：Additive has changed sour two tert-pentyl esters of coke into.
Embodiment 13
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 4
Unanimously, unlike：Additive has changed sulfurous acid diethyl ester into.
Embodiment 14
The present embodiment provides a kind of high coulombic efficiency lithium-sulfur cell electrolyte, its preparation process with it is basic in embodiment 4
Unanimously, unlike：Additive has changed glycol sulfite into.
Comparative example 1
The present embodiment provides a kind of lithium-sulfur cell electrolyte, and its preparation process is different with basically identical in embodiment 1
It is：Additive mass ratio in the mixed solution of formation is 0wt%.
Comparative example 2
The present embodiment provides a kind of lithium-sulfur cell electrolyte, and its preparation process is different with basically identical in embodiment 4
It is：Additive has changed traditional lithium-sulfur cell additive lithium nitrate into, and lithium nitrate mass ratio in the mixed solution of formation is
3wt%.
By the lithium-sulfur cell electrolyte in the various embodiments described above according to existing method, by the use of traditional sulphur carbon mix as
Electrode material is assembled into lithium-sulfur cell progress electro-chemical test and (refers to Xu, N.et al.Greatly suppressed
shuttle effect for improved lithium sulfur battery performance through short
chain intermediates.Nano Lett.17,538-543(2017))。
The test data of different additive lithium-sulfur cell in the embodiment 4 of table 1, embodiment 6-14
| Embodiment | Lithium-sulfur cell electrolysis additive | Coulombic efficiency |
| 4 | Double (4- nitrobenzene) carbonic esters | 100% |
| 6 | Methyl ethyl carbonate | 91.5% |
| 7 | Dimethyl carbonate | 93.7% |
| 8 | Fluorinated ethylene carbonate | 92.3% |
| 9 | Propene carbonate | 94.7% |
| 10 | Ethylene carbonate | 95.3% |
| 11 | Tert-butyl-phenyl carbonic ester | 96.1% |
| 12 | Coke two tert-pentyl esters of acid | 97.2% |
| 13 | Sulfurous acid diethyl ester | 94.1% |
| 14 | Glycol sulfite | 93.5% |
From figure 1 it appears that when mass ratio is 3wt% to additive in the mixed solution of formation, it is thus obtained
The average coulombic efficiency highest of battery.And Fig. 4 is coulombic efficiency comparison diagram in embodiment 2, embodiment 4 and comparative example 1；Fig. 5 is real
Apply coulombic efficiency comparison diagram in example 4, comparative example 1 and comparative example 2；Obviously it is added without additive or using conventional additive system
The battery coulombic efficiency obtained is less than use additive of the present invention.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention, all according to the present invention
The equivalent change or modification that Spirit Essence is made, it should all be included within the scope of the present invention.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent change or modification that Spirit Essence is made, it should all be included within the scope of the present invention.
Claims (10)
- A kind of 1. high coulombic efficiency lithium-sulfur cell electrolyte, it is characterised in that：It adds including ether organic solvent, lithium salts and esters Add agent, the esters additive is one or more mixtures formed in carbonic ester and sulfite.
- 2. high coulombic efficiency lithium-sulfur cell electrolyte according to claim 1, it is characterised in that：The matter of the esters additive It is 0.5~5% to measure fraction.
- 3. high coulombic efficiency lithium-sulfur cell electrolyte according to claim 2, it is characterised in that：The matter of the esters additive It is 1~3% to measure fraction.
- 4. high coulombic efficiency lithium-sulfur cell electrolyte according to claim 1, it is characterised in that：The esters additive General structure isIn formula, Z be 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。
- 5. high coulombic efficiency lithium-sulfur cell electrolyte according to claim 4, it is characterised in that：The esters additive is One or more in following structural formula,
- 6. high coulombic efficiency lithium-sulfur cell electrolyte according to claim 5, it is characterised in that：The esters additive Structural formula is
- 7. high coulombic efficiency lithium-sulfur cell electrolyte according to claim 1, it is characterised in that：The ether organic solvent For glycol dimethyl ether and 1, the mixture of 3 dioxolanes, its volume ratio is 1：1.
- 8. high coulombic efficiency lithium-sulfur cell electrolyte according to claim 1, it is characterised in that：The concentration of the lithium salts is 0.8~1.2mol/L.
- 9. high coulombic efficiency lithium-sulfur cell electrolyte according to claim 8, it is characterised in that：The lithium salts is two (three Methyl fluoride sulphonyl) imine lithium.
- 10. the preparation method of any high coulombic efficiency lithium-sulfur cell electrolyte in claim 1 to 9, it is characterised in that it Comprise the following steps：(a) lithium salts is added into the ether organic solvent, stirring makes its dissolving；(b) carbonates additive is added in the mixture obtained to step (a), stirring dissolves it.
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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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| CN110444816A (en) * | 2019-07-23 | 2019-11-12 | 浙江大学 | A kind of electrolyte and preparation method thereof for lithium-sulfur cell |
| CN110581248A (en) * | 2019-08-23 | 2019-12-17 | 中南大学 | Lithium-sulfur battery and composite diaphragm thereof |
| CN110649316A (en) * | 2019-08-27 | 2020-01-03 | 南方科技大学 | Electrolyte additive, lithium ion battery electrolyte and lithium sulfur battery |
| CN114207902A (en) * | 2020-04-14 | 2022-03-18 | 株式会社Lg新能源 | Electrolyte for lithium-sulfur battery 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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| CN108808092A (en) * | 2018-09-04 | 2018-11-13 | 四川华昆能源有限责任公司 | A kind of active electrolyte and preparation method and purposes |
| CN110444816A (en) * | 2019-07-23 | 2019-11-12 | 浙江大学 | A kind of electrolyte and preparation method thereof for lithium-sulfur cell |
| CN110581248A (en) * | 2019-08-23 | 2019-12-17 | 中南大学 | Lithium-sulfur battery and composite diaphragm thereof |
| CN110649316A (en) * | 2019-08-27 | 2020-01-03 | 南方科技大学 | Electrolyte additive, lithium ion battery electrolyte and lithium sulfur battery |
| CN114207902A (en) * | 2020-04-14 | 2022-03-18 | 株式会社Lg新能源 | Electrolyte for lithium-sulfur battery 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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|---|---|
| WO2018232863A1 (en) | 2018-12-27 |
| CN107342438B (en) | 2020-05-22 |
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