CN106816634B - pseudo high-concentration lithium-sulfur battery electrolyte and lithium-sulfur battery - Google Patents

pseudo high-concentration lithium-sulfur battery electrolyte and lithium-sulfur battery Download PDF

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CN106816634B
CN106816634B CN201710141499.1A CN201710141499A CN106816634B CN 106816634 B CN106816634 B CN 106816634B CN 201710141499 A CN201710141499 A CN 201710141499A CN 106816634 B CN106816634 B CN 106816634B
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lithium
electrolyte
sulfur battery
concentration
pseudo high
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CN106816634A (en
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黄飞飞
田颖
雷若姗
张军杰
徐时清
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China University of Metrology
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China University of Metrology
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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
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Secondary Cells (AREA)

Abstract

The invention discloses a pseudo high-concentration lithium-sulfur battery electrolyte and a lithium-sulfur battery, wherein the electrolyte contains lithium salt, an ether solvent and a non-solvent solution, the concentration of the lithium salt in the ether solvent is higher than 3.0mol/L, and the concentration of the lithium salt in the pseudo high-concentration electrolyte is not lower than 0.5 mol/L. The battery electrolyte provided by the invention can improve the problems of high viscosity and low conductivity of the lithium-sulfur battery electrolyte with high-concentration lithium salt, has incombustibility, and can obviously improve the electrochemical performance and safety of the lithium-sulfur battery.

Description

pseudo high-concentration lithium-sulfur battery electrolyte and lithium-sulfur battery
Technical Field
The present invention relates to a pseudo high concentration lithium-sulfur battery electrolyte and a corresponding lithium-sulfur battery, and more particularly, to a lithium-sulfur battery electrolyte containing a high concentration lithium salt of fluoroether.
Background
The lithium-sulfur battery has the advantages that the theoretical specific capacity is 1675mAh/g, the theoretical specific energy is 2600Wh/Kg and is far higher than that of the existing lithium ion battery, the storage capacity of sulfur is rich, the price is low, the toxicity is low, and the pollution is avoided, therefore, the lithium-sulfur battery becomes a candidate of the next generation of lithium batteries with high specific energy and attracts the attention all over the world, lithium polysulfide which is an intermediate product of the lithium-sulfur battery can directly react with esters, the lithium-sulfur battery generally adopts ethers as an electrolyte solvent instead of carbonic ester, carboxylic ester and the like which are adopted by an electrolyte of the lithium ion battery, the solubility of the lithium polysulfide in the ether electrolyte is higher, the lithium polysulfide dissolved in the electrolysis in the charging and discharging process can migrate to a negative electrode and carry out a corrosion reaction with a metal lithium negative electrode, active substances of the positive electrode and the negative electrode are consumed, the cycle performance of the battery is poor, the coulombic efficiency is low, meanwhile, the insulativity of sulfur and Li 2 S, the volume expansion in the charging and discharging process also seriously influence the utilization rate and.
In the lithium-sulfur battery electrolyte modification, many works are carried out, such as the adoption of an ionic liquid which can dissolve lithium salt but cannot dissolve lithium polysulfide as an electrolyte cosolvent to inhibit the dissolution and migration of lithium polysulfide in the electrolyte, the adoption of LiNO 3, KNO 3, P 2 S 5 and the like as electrolyte additives to assist the lithium metal cathode side to form a relatively stable SEI film and inhibit the corrosion reaction between lithium polysulfide dissolved in the electrolyte and the lithium metal.
The conductivity in a lithium ion battery electrolyte is determined by the mobility of the lithium ions in the electrolyte and the viscosity of the electrolyte. However, most of solvent molecules in the high-concentration lithium salt electrolyte participate in the solvation of lithium ions and few free solvent molecules, and the high-concentration lithium-sulfur battery electrolyte has major problems of high viscosity and low conductivity. The high viscosity is not beneficial to the migration of lithium ions and the sufficient contact between the electrolyte and the electrode, and the corresponding lithium-sulfur battery has a higher impedance value. The lower conductivity indicates that the migration rate of lithium ions in the electrolyte is slower, and the rate performance and the low-temperature performance of the battery are not facilitated. Therefore, finding a new method to solve the problems of high viscosity and low conductivity of the electrolyte of the high-concentration lithium-sulfur battery is an important way to promote the practicability of the electrolyte of the high-concentration lithium-sulfur battery and accelerate the commercialization process of the lithium-sulfur battery.
disclosure of Invention
The invention aims to provide a pseudo high-concentration lithium-sulfur battery electrolyte, which can solve the problems of high viscosity and low conductivity of the high-concentration lithium-sulfur battery electrolyte.
The invention provides a specific technical scheme as follows:
A pseudo high concentration lithium sulfur battery electrolyte, characterized in that:
The electrolyte contains lithium salt, ether solvent and non-solvent liquid;
the concentration of the lithium salt in the ether solvent is not lower than 3 mol/L;
The solubility of the non-solvent liquid to lithium salt is lower than 0.1 mol/L.
preferably, the molar concentration of the lithium salt in the ether solvent is higher than 3.0mol/L, and the overall concentration of the lithium salt in the pseudo high-concentration electrolyte is higher than 0.5 mol/L.
Preferably, the non-solvent liquid is at least one selected from the group consisting of fluoroethers represented by the following structural formula (I)
Wherein Rf 1 and Rf 2 are independently selected from C1-C10 alkyl or C1-C10 fluoroalkyl, and at least one is selected from C1-C10 fluoroalkyl.
More preferably, the Rf 1 and Rf 2 are independently selected from C1-C6 fluoroalkyl or C1-C6 alkyl, and at least one is selected from C1-C6 fluoroalkyl.
Preferably, in the electrolyte, the mass fraction of the fluoroether is 5 to 90%, and the mass fraction of the ether solvent is 20 to 98%.
More preferably, in the electrolyte, the mass fraction of the fluoroether is 30 to 60%, and the mass fraction of the ether solvent is 40 to 70%.
Preferably, the lithium salt is at least one selected from LiPF 6, LiBF 4, LiBOB, liddob, LiPO 2 F 2, LiSO 3 CF 3, lithium bis (trifluoromethyl) sulfonyl imide (LiTFSI) and lithium bis (fluoro) sulfonyl imide (LiFSI).
Preferably, the ether solvent is at least one selected from the group consisting of tetrahydrofuran, 2-methyltetrahydrofuran, 1, 3-dioxolane, ethylene glycol dimethyl ether, dimethoxymethane, 1, 2-dimethoxyethane and diglyme;
a lithium-sulfur battery employing the electrolyte as described above.
The invention relates to a method for adding proper amount of non-solvent liquid, especially fluoroether, into high-concentration electrolyte of a lithium-sulfur battery. First, fluorine in fluoroether has strong electronegativity and weak polarity, so that the ether solvent is greatly reduced in solubility after being fluorinated, and many cannot dissolve lithium salt and lithium polysulfide. Thus, the addition of the fluoroether does not change the solvation state of the lithium ions and solvent molecules in the high concentration lithium salt electrolyte, and the resulting new electrolyte has similar properties to the high concentration lithium salt electrolyte, although the overall new electrolyte has a reduced lithium salt concentration, and is named as a pseudo high concentration lithium salt lithium sulfur battery electrolyte.
An appropriate amount of fluoroether is added to the pseudo high concentration lithium salt electrolyte relative to the high concentration lithium salt electrolyte. The fluoroether has low viscosity and has better wettability to an electrode and a diaphragm. Therefore, the viscosity of the pseudo high-concentration lithium salt electrolyte is significantly reduced, causing an increase in the electrolyte conductivity. In addition, the fluoroether itself is non-flammable, so that the addition of the fluoroether can reduce the flammability of the electrolyte to some extent, and even obtain a non-flammable electrolyte.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the invention to these embodiments. It will be appreciated by those skilled in the art that the present invention encompasses all alternatives, modifications and equivalents as may be included within the scope of the claims.
Abbreviations for the fluoroethers described in the following examples are as follows:
HFMOP is (CF 3) 2 CHOCH 3 is (CF 3) 2 CHOCH 2 CH 3 is (CF 3) 2 CHOCH 2 CF 2 CF 2 H, TFEOTFP is HCF 2 CF 2 OCH 2 CF 2 CF 2 H, TFEOPFP is HCF 2 CF 2 OCH 2 CF 2 CF 3 is CF 3 CF 2 CHFOCH 2 CH 3.
Example 1
The electrolyte of the lithium ion battery comprises two ether solvents of 1,3 Dioxolane (DOL) and ethylene glycol dimethyl ether (DME), and LiTFSI is used as a lithium salt. The preparation method comprises the following steps: DOL and DME are mixed according to the volume ratio of 1:1, and then LiTFSI is added to enable the concentration to reach 5.0 mol/L. And then adding HFMOP into the electrolyte to ensure that the mass fraction of the HFMOP in the electrolyte is 40 percent, thereby obtaining the electrolyte of the lithium-sulfur battery.
Example 2
the electrolyte of the lithium ion battery comprises two ether solvents of 1,3 Dioxolane (DOL) and ethylene glycol dimethyl ether (DME), and LiTFSI is used as a lithium salt. The preparation method comprises the following steps: DOL and DME are mixed according to the volume ratio of 1:1, and then LiTFSI is added to enable the concentration to reach 5.0 mol/L. And then adding HFEOP into the electrolyte to ensure that the mass fraction of the HFEOP in the electrolyte is 50 percent, thereby obtaining the electrolyte of the lithium-sulfur battery.
Example 3
The electrolyte of the lithium ion battery comprises two ether solvents of 1,3 Dioxolane (DOL) and ethylene glycol dimethyl ether (DME), and LiTFSI is used as a lithium salt. The preparation method comprises the following steps: DOL and DME are mixed according to the volume ratio of 1:1, and then LiTFSI is added to enable the concentration to reach 5.0 mol/L. And then adding HFTFPAP into the electrolyte to ensure that the mass fraction of the HFTFPAP in the electrolyte is 60 percent to obtain the electrolyte of the lithium-sulfur battery.
Example 4
the electrolyte of the lithium ion battery comprises two ether solvents of 1,3 Dioxolane (DOL) and ethylene glycol dimethyl ether (DME), and LiTFSI is used as a lithium salt. The preparation method comprises the following steps: DOL and DME are mixed according to the volume ratio of 1:1, and then LiTFSI is added to enable the concentration to reach 5.0 mol/L. And then adding TFEOTFP into the electrolyte to ensure that the mass fraction of TFEOTFP in the electrolyte is 60 percent, thereby obtaining the electrolyte of the lithium-sulfur battery.
Example 5
The electrolyte of the lithium ion battery comprises two ether solvents of 1,3 Dioxolane (DOL) and ethylene glycol dimethyl ether (DME), and LiTFSI is used as a lithium salt. The preparation method comprises the following steps: DOL and DME are mixed according to the volume ratio of 1:1, and then LiTFSI is added to enable the concentration to reach 7.0 mol/L. And then adding TFEOPFP into the electrolyte to ensure that the mass fraction of TFEOPFP in the electrolyte is 60 percent, thereby obtaining the electrolyte of the lithium-sulfur battery.
Example 6
The electrolyte of the lithium ion battery comprises two ether solvents of 1,3 Dioxolane (DOL) and ethylene glycol dimethyl ether (DME), and LiTFSI is used as a lithium salt. The preparation method comprises the following steps: DOL and DME are mixed according to the volume ratio of 1:1, and then LiTFSI is added to enable the concentration to reach 7.0 mol/L. And then adding HFPEEE into the electrolyte to ensure that the mass fraction of the HFPEEE in the electrolyte is 60 percent, thereby obtaining the lithium-sulfur battery electrolyte.
Comparative example 1
The electrolyte of the lithium ion battery comprises two ether solvents of 1,3 Dioxolane (DOL) and ethylene glycol dimethyl ether (DME), and LiTFSI is used as a lithium salt. The preparation method comprises the following steps: DOL and DME are mixed according to the volume ratio of 1:1, and then LiTFSI is added to enable the concentration to reach 1.0 mol/L.
Comparative example 2
The electrolyte of the lithium ion battery comprises two ether solvents of 1,3 Dioxolane (DOL) and ethylene glycol dimethyl ether (DME), and LiTFSI is used as a lithium salt. The preparation method comprises the following steps: DOL and DME are mixed according to the volume ratio of 1:1, and then LiTFSI is added to enable the concentration to reach 5.0 mol/L.
Comparative example 3
The electrolyte of the lithium ion battery comprises two ether solvents of 1,3 Dioxolane (DOL) and ethylene glycol dimethyl ether (DME), and LiTFSI is used as a lithium salt. The preparation method comprises the following steps: DOL and DME are mixed according to the volume ratio of 1:1, and then LiTFSI is added to enable the concentration to reach 7.0 mol/L.
The electrolytes prepared in examples 1 to 6 and comparative examples 1 to 3 were tested.
The main test method comprises the following steps:
(1) soaking 2cm by 10cm of glass fiber cloth in the electrolyte for 1min, and testing the flammability and self-extinguishing time of the cloth strips soaked with the electrolyte.
(2) The conductivity and viscosity of the electrolyte at 20 ℃ and the contact angle between the electrolyte and the diaphragm;
(3) Uniformly mixing sulfur and Ketjen black in a mass ratio of 2:1, and performing vacuum treatment at 155 ℃ for 12 hours to obtain the sulfur-carbon composite material. Mixing a sulfur-carbon composite material: acetylene black: and (3) dispersing the hydroxymethyl cellulose and the styrene butadiene rubber in a proper amount of water at a ratio of 8:1:1, and performing ball milling for 6 hours to obtain the electrode slurry. Coating the obtained slurry on an aluminum foil, drying under an infrared lamp, drying at 60 ℃ in vacuum for 12 hours, and cutting into electrode slices with the diameter of 14mm for later use. And then, assembling the lithium-sulfur battery by adopting the electrolyte, the metal lithium as a negative electrode and the Cegrad 2400 as a diaphragm, and testing the cycle performance of the lithium-sulfur battery after 50 weeks of cycle at a rate of 0.2C. The test results were as follows:
TABLE 1
as can be seen from table 1, the pseudo high-concentration lithium salt electrolyte provided by the present invention overcomes the original disadvantages of the high-concentration lithium salt electrolyte, and has the advantages of low viscosity, high conductivity, small contact angle with the separator, and the like. Moreover, the pseudo high concentration lithium salt electrolyte retains the advantages of the high concentration lithium salt electrolyte, such as lower average coulombic efficiency and higher capacity retention rate due to the suppression of the shuttle effect. Meanwhile, a certain amount of non-flammable fluoroether is added into the pseudo high-concentration electrolyte, so that the electrolyte is not flammable integrally, and the safety of the electrolyte is further improved.

Claims (7)

1. A pseudo high concentration lithium sulfur battery electrolyte, characterized in that:
the electrolyte contains lithium salt, ether solvent and non-solvent liquid;
The concentration of the lithium salt in the ether solvent is higher than 3 mol/L;
The solubility of the non-solvent liquid to lithium salt is lower than 0.1 mol/L;
the ether solvent is a mixed solution of 1, 3-dioxolane and glycol dimethyl ether in a volume ratio of 1: 1;
The lithium-sulfur battery is a lithium-sulfur battery with S8 as an active material;
the non-solvent liquid is at least one of fluoroethers shown in the following structural formula (I)
wherein: rf1 and Rf2 are independently selected from C1-C10 alkyl or C1-C10 fluoroalkyl, and at least one is selected from C1-C10 fluoroalkyl.
2. A pseudo high concentration lithium sulfur battery electrolyte according to claim 1 wherein: the molar concentration of the lithium salt in the ether solvent is higher than 3.0mol/L, and the overall concentration of the lithium salt in the pseudo high-concentration electrolyte is higher than 0.5 mol/L.
3. A pseudo high concentration lithium sulfur battery electrolyte according to claim 1 wherein: the Rf1 and the Rf2 are independently selected from C1-C6 fluoroalkyl or C1-C6 alkyl, and at least one is selected from C1-C6 fluoroalkyl.
4. A pseudo high concentration lithium sulfur battery electrolyte according to claim 1 wherein: in the electrolyte, the mass fraction of the fluoroether is 5-90%, and the mass fraction of the ether solvent is 20-98%.
5. The pseudo high concentration lithium sulfur battery electrolyte of claim 4 wherein: in the electrolyte, the mass fraction of the fluoroether is 30-60%, and the mass fraction of the ether solvent is 40-70%.
6. A pseudo high concentration lithium sulfur battery electrolyte according to claim 1 wherein: the lithium salt is at least one selected from LiPF6, LiBF4, LiBOB, LiDFOB, LiPO2F2, LiSO3CF3, lithium bis (trifluoromethyl) sulfonyl imide (LiTFSI) and lithium bis (fluoro) sulfonyl imide (LiFSI).
7. A lithium sulfur battery characterized by: use of an electrolyte as claimed in any of claims 1 to 6.
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CN107799828B (en) * 2017-10-26 2020-09-11 中国科学院过程工程研究所 Bifunctional electrolyte suitable for intercalation and conversion type lithium battery, preparation method and lithium battery comprising same
CN112886065B (en) * 2019-11-29 2022-07-19 深圳新宙邦科技股份有限公司 Electrolyte and metal-sulfur 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
CN113972399B (en) * 2021-10-25 2023-02-07 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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CN108270035A (en) * 2016-12-30 2018-07-10 浙江省化工研究院有限公司 A kind of battery electrolyte containing high concentration lithium salts

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CN108270035A (en) * 2016-12-30 2018-07-10 浙江省化工研究院有限公司 A kind of battery electrolyte containing high concentration lithium salts

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