CN106816634A - A kind of pseudo- high concentration lithium-sulfur cell electrolyte and lithium-sulfur cell - Google Patents
A kind of pseudo- high concentration lithium-sulfur cell electrolyte and lithium-sulfur cell Download PDFInfo
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- CN106816634A CN106816634A CN201710141499.1A CN201710141499A CN106816634A CN 106816634 A CN106816634 A CN 106816634A CN 201710141499 A CN201710141499 A CN 201710141499A CN 106816634 A CN106816634 A CN 106816634A
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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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- 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
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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 invention discloses a kind of pseudo- high concentration lithium-sulfur cell electrolyte and lithium-sulfur cell, the electrolyte contains lithium salts, ether solvent and non-solvent solution, concentration of the lithium salts in ether solvent is higher than 3.0mol/L, and concentration of the lithium salts in pseudo- high concentration electrolyte is not less than 0.5mol/L.The battery electrolyte that the present invention is provided, can improve the high viscosity and low conductivity problem of the lithium-sulfur cell electrolyte of high concentration lithium salts, and with incombustibility, be remarkably improved the chemical property and security of lithium-sulfur cell.
Description
Technical field
The present invention relates to a kind of pseudo- high concentration lithium-sulfur cell electrolyte and corresponding lithium-sulfur cell, more particularly to one kind contains
There is the lithium-sulfur cell electrolyte of the high concentration lithium salts of fluoro-ether.
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 typically uses ethers as electrolyte solvent, rather than carbonic ester and carboxylic acid that lithium-ion battery electrolytes are used
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 corrosion reaction occurs 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 insulating properties, the charge and discharge process of S etc. has also had a strong impact on lithium
The active material utilization and cyclical stability of sulphur battery, seriously hinder its practicalization.
For the problem of lithium-sulfur cell, global researcher is from sulphur positive pole microstructure design, feature barrier film
Prepare, electrolyte is modified and many aspects such as protection of lithium anode have carried out many research work, achieve significant
Effect.Wherein around the modified of lithium-sulfur cell electrolyte, many work are carried out, such as use can dissolve lithium salts and but can not
The ionic liquid of many lithium sulfides is dissolved as electrolyte co-solvents, suppresses the dissolving and migration in the electrolytic solution of many lithium sulfides.Adopt
Use LiNO3、KNO3、P2S5Deng as electrolysis additive, assistant metal cathode of lithium side forms more stable SEI films, suppresses molten
Corrosion reaction between solution many lithium sulfides in the electrolytic solution and lithium metal.In addition, more lithium salts are dissolved in into ether solvent
In, form high concentration lithium salt electrolyte.The lithium ion that the molten middle most of solvent molecule of high concentration lithium salts has been involved in lithium salts is molten
Agent, few free solvent molecules, thus many lithium sulfides can not be redissolved.Also, the viscosity of high concentration lithium salt electrolyte
It is very high, hence it is evident that to reduce the migration in the electrolytic solution of many lithium sulfides.Therefore, high concentration lithium salts electrolysis liquid energy substantially reduce due to
Shadow of the corrosion of shuttle effect and lithium anode that the dissolving in the electrolytic solution of many lithium sulfides and migration are caused to battery performance
Ring, help to obtain high performance lithium-sulfur cell.
Electrical conductivity in lithium-ion battery electrolytes is decided by the mobility and electrolysis fluid viscosity of lithium ion in electrolyte.But
Be, in high concentration lithium salt electrolyte most of solvent molecule participate in lithium ion solvation and few free solvent molecules,
The subject matter that high concentration lithium-sulfur cell electrolyte is present is that the viscosity of electrolyte is high low with electrical conductivity.Viscosity is high be unfavorable for lithium from
Being fully contacted between the migration of son and electrolyte and electrode, corresponding lithium-sulfur cell impedance value is higher.The relatively low indication of electrical conductivity
The migration rate that lithium ion in electrolyte is slower, is unfavorable for the high rate performance and cryogenic property of battery.Therefore, new side is found
Method, solve the problems, such as the electrolysis of high concentration lithium-sulfur cell fluid viscosity be high and electrical conductivity it is low be to promote high concentration lithium-sulfur cell electrolyte reality
With the important channel for changing and accelerating lithium-sulfur cell commercialization process.
The content of the invention
It is an object of the invention to provide a kind of pseudo- high concentration lithium-sulfur cell electrolyte, high concentration lithium-sulfur cell is can solve the problem that
The high viscosity of electrolyte and the problem of low conductivity.
It is as follows that the present invention provides specific technical scheme：
A kind of pseudo- high concentration lithium-sulfur cell electrolyte, it is characterised in that：
The electrolyte contains lithium salts, ether solvent and non solvent liquid；
Concentration of the lithium salts in ether solvent is not less than 3mol/L；
Described non solvent liquid is less than 0.1mol/L to the solubility of lithium salts.
Preferably, molar concentration of the lithium salts in ether solvent is higher than 3.0mol/L, and the lithium salts is pseudo- high
Overall density in concentration electrolytic solution is higher than 0.5mol/L.
Preferably, the non solvent liquid preferably is selected from least one in the fluoro-ether shown in following structure formula (I)
Wherein：Rf1、Rf2Independently selected from the alkyl or the fluoro-alkyl of C1~C10 of C1~C10, and at least one is selected from
The fluoro-alkyl of C1~C10..
It is furthermore preferred that the Rf1、Rf2The fluoro-alkyl of C1~C6 or the alkyl of C1~C6 preferably independently are selected from, and at least
One fluoro-alkyl selected from C1~C6.
Preferably, in the electrolyte, the mass fraction of fluoro-ether is 5~90%, the quality point of ether solvent solvent
Number is 20~98%.
It is furthermore preferred that in the electrolyte, the mass fraction of fluoro-ether is 30~60%, and the mass fraction of ether solvent is
40~70%.
Preferably, the lithium salts is selected from LiPF6、LiBF4、LiBOB、LiDFOB、LiPO2F2、LiSO3CF3, double fluoroforms
At least one in base sulfimide lithium (LiTFSI) and double fluorine sulfimide lithium (LiFSI).
Preferably, the ether solvent is selected from tetrahydrofuran, 2- methyltetrahydrofurans, 1,3- dioxolanes, second two
At least one in diethylene glycol dimethyl ether, dimethoxymethane, 1,2- dimethoxies and diethylene glycol dimethyl ether；
A kind of lithium-sulfur cell, using electrolyte as described above.
The present invention is to add appropriate non solvent liquid in high concentration lithium-sulfur cell electrolyte, especially fluoro-ether.It is first
Fluorine in first fluoro-ether has very strong an electronegativity and low pole, thus ether solvent declined to a great extent by dissolubility after fluoro,
Lithium salts and many lithium sulfides can not much be dissolved.Thus, the addition of fluoro-ether will not change lithium ion in high concentration lithium salt electrolyte
With solvent molecule Solvation State, the new electrolyte property of formation is similar with high concentration lithium salt electrolyte performance, although overall
On see that new electrolyte lithium salt decreases, this new electrolyte is named as the electrolysis of pseudo- high concentration lithium salts lithium-sulfur cell
Liquid.
Relative to high concentration lithium salt electrolyte, appropriate fluoro-ether is with the addition of in pseudo- high concentration lithium salt electrolyte.Fluoro-ether
Viscosity is very low, all has relatively good wetability to electrode, barrier film.Therefore, pseudo- high concentration lithium salt electrolyte viscosity is decreased obviously,
Causing electrolytic conductivity increases.In addition, fluoro-ether is in itself non-flammable, thus the addition of fluoro-ether can also be to a certain degree
The upper combustibility for reducing electrolyte, or even obtain non-flammable electrolyte.
Specific embodiment
The present invention is further described with reference to specific embodiment, but does not limit the invention to these tools
Body implementation method.One skilled in the art would recognize that present invention encompasses being potentially included in Claims scope
All alternatives, improvement project and equivalents.
The abbreviation of fluoro-ether described in following examples is as follows：
HFMOP is (CF3)2CHOCH3, HFEOP is (CF3)2CHOCH2CH3, HFTFPOP is (CF3)2CHOCH2CF2CF2H,
TFEOTFP is HCF2CF2OCH2CF2CF2H, TFEOPFP are HCF2CF2OCH2CF2CF3, HFPEE is CF3CF2CHFOCH2CH3。
Embodiment 1
A kind of lithium-ion battery electrolytes, including 1,3 dioxolanes (DOL), two kinds of ethers of glycol dimethyl ether (DME) are molten
Agent, with LiTFSI as lithium salts.Its preparation method is：By DOL, DME 1: 1 mixing by volume, LiTFSI is subsequently adding, is allowed to dense
Degree reaches 5.0mol/L.Backward electrolyte in add HFMOP, make HFMOP mass fractions in the electrolytic solution for 40%, obtain
Lithium-sulfur cell electrolyte.
Embodiment 2
A kind of lithium-ion battery electrolytes, including 1,3 dioxolanes (DOL), two kinds of ethers of glycol dimethyl ether (DME) are molten
Agent, with LiTFSI as lithium salts.Its preparation method is：By DOL, DME 1: 1 mixing by volume, LiTFSI is subsequently adding, is allowed to dense
Degree reaches 5.0mol/L.Backward electrolyte in add HFEOP, make HFEOP mass fractions in the electrolytic solution for 50%, obtain
Lithium-sulfur cell electrolyte.
Embodiment 3
A kind of lithium-ion battery electrolytes, including 1,3 dioxolanes (DOL), two kinds of ethers of glycol dimethyl ether (DME) are molten
Agent, with LiTFSI as lithium salts.Its preparation method is：By DOL, DME 1: 1 mixing by volume, LiTFSI is subsequently adding, is allowed to dense
Degree reaches 5.0mol/L.Backward electrolyte in add HFTFPOP, make HFTFPOP mass fractions in the electrolytic solution for 60%,
Obtain lithium-sulfur cell electrolyte.
Embodiment 4
A kind of lithium-ion battery electrolytes, including 1,3 dioxolanes (DOL), two kinds of ethers of glycol dimethyl ether (DME) are molten
Agent, with LiTFSI as lithium salts.Its preparation method is：By DOL, DME 1: 1 mixing by volume, LiTFSI is subsequently adding, is allowed to dense
Degree reaches 5.0mol/L.Backward electrolyte in add TFEOTFP, make TFEOTFP mass fractions in the electrolytic solution for 60%,
Obtain lithium-sulfur cell electrolyte.
Embodiment 5
A kind of lithium-ion battery electrolytes, including 1,3 dioxolanes (DOL), two kinds of ethers of glycol dimethyl ether (DME) are molten
Agent, with LiTFSI as lithium salts.Its preparation method is：By DOL, DME 1: 1 mixing by volume, LiTFSI is subsequently adding, is allowed to dense
Degree reaches 7.0mol/L.Backward electrolyte in add TFEOPFP, make TFEOPFP mass fractions in the electrolytic solution for 60%,
Obtain lithium-sulfur cell electrolyte.
Embodiment 6
A kind of lithium-ion battery electrolytes, including 1,3 dioxolanes (DOL), two kinds of ethers of glycol dimethyl ether (DME) are molten
Agent, with LiTFSI as lithium salts.Its preparation method is：By DOL, DME 1: 1 mixing by volume, LiTFSI is subsequently adding, is allowed to dense
Degree reaches 7.0mol/L.Backward electrolyte in add HFPEE, make HFPEE mass fractions in the electrolytic solution for 60%, obtain
Lithium-sulfur cell electrolyte.
Comparative example 1
A kind of lithium-ion battery electrolytes, including 1,3 dioxolanes (DOL), two kinds of ethers of glycol dimethyl ether (DME) are molten
Agent, with LiTFSI as lithium salts.Its preparation method is：By DOL, DME 1: 1 mixing by volume, LiTFSI is subsequently adding, is allowed to dense
Degree reaches 1.0mol/L.
Comparative example 2
A kind of lithium-ion battery electrolytes, including 1,3 dioxolanes (DOL), two kinds of ethers of glycol dimethyl ether (DME) are molten
Agent, with LiTFSI as lithium salts.Its preparation method is：By DOL, DME 1: 1 mixing by volume, LiTFSI is subsequently adding, is allowed to dense
Degree reaches 5.0mol/L.
Comparative example 3
A kind of lithium-ion battery electrolytes, including 1,3 dioxolanes (DOL), two kinds of ethers of glycol dimethyl ether (DME) are molten
Agent, with LiTFSI as lithium salts.Its preparation method is：By DOL, DME 1: 1 mixing by volume, LiTFSI is subsequently adding, is allowed to dense
Degree reaches 7.0mol/L.
The electrolyte that embodiment 1 to 6 and comparative example 1 to 3 are prepared, is tested.
Main method of testing：
(1) 1min in the electrolytic solution, the cloth after test infiltration electrolyte are infiltrated using the glass fabric of 2cm*10cm
Flammable and self-extinguishing time.
The electrical conductivity of electrolyte, viscosity and its contact angle with barrier film at (2) 20 DEG C；
(3) it is 2 by mass ratio:After 1 sulphur and Ketjen black is well mixed, application of vacuum 12h obtains sulphur carbon and answers at 155 DEG C
Condensation material.By sulphur carbon composite：Acetylene black：Hydroxymethyl cellulose+butadiene-styrene rubber=8:1:1 is distributed in appropriate water, ball
Electrode slurry is obtained after mill 6h.The slurry that will be obtained is coated on aluminium foil, after being dried under infrared lamp, 12h is dried at 60 DEG C of vacuum,
The electrode slice for cutting into a diameter of 14mm is standby.Afterwards, use above-mentioned electrolyte, lithium metal for negative pole, Cegrald2400 be every
Film assembles lithium-sulfur cell, 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, the pseudo- high concentration lithium salt electrolyte that the present invention is provided overcomes compared with high concentration lithium salt electrolyte
Its original shortcoming, has the advantages that viscosity is low, electrical conductivity is high and barrier film contact angle is smaller.And, the pseudo- high concentration lithium salts
Electrolyte remain the advantage of high concentration lithium salt electrolyte, the relatively low average storehouse for such as being obtained because shuttle effect is suppressed
Human relations efficiency and capability retention higher.Meanwhile, a certain amount of non-flammable fluoro-ether is with the addition of in pseudo- high concentration electrolyte, electricity
Solution liquid is integrally non-combustible, further improves the security of electrolyte.
Claims (9)
1. a kind of pseudo- high concentration lithium-sulfur cell electrolyte, it is characterised in that：
Described electrolyte contains lithium salts, ether solvent and non solvent liquid；
Concentration of the described lithium salts in ether solvent is higher than 3mol/L；
Described non solvent liquid is less than 0.1mol/L to the solubility of lithium salts.
2. according to a kind of pseudo- high concentration lithium-sulfur cell electrolyte described in claim 1, it is characterised in that：Described lithium salts is in ether
Molar concentration in class solvent is higher than 3.0mol/L, and the overall density of described lithium salts in pseudo- high concentration electrolyte is higher than
0.5mol/L。
3. according to a kind of pseudo- high concentration lithium-sulfur cell electrolyte described in claim 1, it is characterised in that：Described non-solvent liquid
Body is selected from least one in the fluoro-ether shown in following structure formula (I)
Wherein：Rf1、Rf2Independently selected from the alkyl or the fluoro-alkyl of C1~C10 of C1~C10, and at least one is selected from C1
The fluoro-alkyl of~C10.
4. according to a kind of pseudo- high concentration lithium-sulfur cell electrolyte described in claim 3, it is characterised in that：Described Rf1、Rf2Solely
Fluoro-alkyl or the alkyl of C1~C6 on the spot selected from C1~C6, and at least one is selected from the fluoro-alkyl of C1~C6.
5. according to a kind of pseudo- high concentration lithium-sulfur cell electrolyte described in claim 3, it is characterised in that：Described electrolyte
In, the mass fraction of fluoro-ether is 5~90%, and the mass fraction of ether solvent solvent is 20~98%.
6. according to a kind of pseudo- high concentration lithium-sulfur cell electrolyte described in claim 5, it is characterised in that：Described electrolyte
In, the mass fraction of fluoro-ether is 30~60%, and the mass fraction of ether solvent is 40~70%.
7. according to a kind of pseudo- high concentration lithium-sulfur cell electrolyte described in claim 1, it is characterised in that：Described lithium salts is selected from
LiPF6、LiBF4、LiBOB、LiDFOB、LiPO2F2、LiSO3CF3, bis trifluoromethyl sulfimide lithium (LiTFSI) and double fluorine sulphur
At least one in imide li (LiFSI).
8. according to a kind of pseudo- high concentration lithium-sulfur cell electrolyte described in claim 1, it is characterised in that：Described ether solvent
Selected from tetrahydrofuran, 2- methyltetrahydrofurans, 1,3- dioxolanes, glycol dimethyl ether, dimethoxymethane, 1,2- dimethoxies
At least one in ethane and diethylene glycol dimethyl ether.
9. a kind of lithium-sulfur cell, it is characterised in that：Using the electrolyte as described in claim any one of 1-8.
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| CN107799828A (en) * | 2017-10-26 | 2018-03-13 | 中国科学院过程工程研究所 | Suitable for insertion, the Difunctional electrolyte of transformant lithium battery, preparation method and include its lithium battery |
| CN111584936A (en) * | 2020-06-29 | 2020-08-25 | 四川东为氢源科技有限公司 | Electrolyte and preparation method thereof |
| CN112886065A (en) * | 2019-11-29 | 2021-06-01 | 深圳新宙邦科技股份有限公司 | Electrolyte and metal-sulfur battery |
| 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 |
| CN115117453A (en) * | 2022-07-20 | 2022-09-27 | 武汉大学 | Electrolyte for lithium metal secondary battery |
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