CN103531843A - Electrolytic solution for high-temperature high-magnification type lithium ion battery - Google Patents

Electrolytic solution for high-temperature high-magnification type lithium ion battery Download PDF

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CN103531843A
CN103531843A CN201310507641.1A CN201310507641A CN103531843A CN 103531843 A CN103531843 A CN 103531843A CN 201310507641 A CN201310507641 A CN 201310507641A CN 103531843 A CN103531843 A CN 103531843A
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lithium
carbonate
organic solvent
electrolyte
ion battery
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李世友
李晓鹏
崔孝玲
赵伟
张宏明
李永立
刘金良
净洁
李玲霞
薛宇宙
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Lanzhou University of Technology
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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
    • H01M10/056—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
    • 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
    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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 electrolytic solution for a high-temperature high-magnification type lithium ion battery. The electrolytic solution comprises an aprotic organic solvent, basic electrolyte lithium salt and a functional additive, wherein the aprotic organic solvent is one substance or a mixture of more of common carbonic ester, sulfite and sulfone compound and the like; the basic electrolyte lithium salt is 0.5-1.2mol/L of double-oxalate lithium borate or lithium difluoroborate or a mixture of the double-oxalate lithium borate and the lithium difluoroborate; the functional additive is sulfate difluoro lithium borate or sulfite difluoro lithium borate or a mixture of the sulfate difluoro lithium borate and the sulfite difluoro lithium borate. The electrolytic solution disclosed by the invention has the advantages that by optimization of components of the electrolytic solution, the electrical conductivity and the thermal decomposition temperature of the electrolytic solution are improved, the impedance of a solid electrolyte interfacial film formed by the electrolytic solution on the surface of the electrolyte material is greatly reduced, and further the high-temperature performance and the rate performance of the battery are improved.

Description

A kind of high temperature electrolyte for high multiplying power lithium ion battery
Technical field
The present invention relates to a kind of high temperature electrolyte for high multiplying power lithium ion battery, specifically, relate to a kind of electrolyte for lithium ion battery of discharging and recharging under high magnification, working of being adapted under hot environment, belong to battery material field.
Background technology
Lithium ion battery has plurality of advantages, is one of the fastest battery system of development in recent years.Electrolyte, as the important component part of lithium ion battery, affects chemical property and the security performance of lithium ion battery to a great extent.
Obtain at present the lithium ion battery of practical application, its non-proton electrolyte generally adopts LiPF 6as basic electrolyte lithium salt, aprotic organic solvent mostly is the mixed solvent that cyclic carbonate (as ethylene carbonate (EC), propene carbonate (PC)) and linear carbonate (as dimethyl carbonate (DMC), diethyl carbonate (DEC) or methyl ethyl carbonate (EMC)) are formed.This electrolyte system has higher conductivity and wider electrochemical window, and the lithium ion battery of assembling has shown good cycle performance and high rate performance.But except being easy to hydrolysis, for example, under higher temperature conditions (60 ℃), LiPF 6also easily decomposes generates LiF and PF 5.PF 5be a kind of stronger lewis acid and fluorinated ligands, very easily cause electrolyte polymerization and and organic solvent reaction.And, under trace water exists, PF 5facile hydrolysis generates HF positive electrode to strong corrosion.These unfavorable factors have greatly limited use LiPF 6the high-temperature behavior of base electrolyte battery (Liao Hongying, Cheng Baoying, Hao Zhiqiang. lithium-ion battery electrolytes [J]. new material industry, 2003,118 (9): 34-37).
The higher novel electrolytes salt of exploitation thermal stability is one of study hotspot at present to improve the high-temperature behavior of lithium ion battery.In new lithium salts, receiving publicity more is di-oxalate lithium borate (LiBOB) and difluorine oxalic acid boracic acid lithium (LiODFB).Except the routine requirement meeting as electrolyte lithium salt, these two kinds of lithium salts also have two outstanding features: first, the thermal stability of LiBOB and LiODFB is all very excellent, and heat decomposition temperature can reach respectively 302 ℃ and 240 ℃, and this can greatly improve the resistance to elevated temperatures of electrolyte.Second, self all has higher reduction potential LiBOB and LiODFB, even and in pure propene carbonate (PC), still can form stable solid electrolyte interface film (SEI) (Pu Weihua on carbon back negative material surface, He Xiangming, Wang Li, Wan Chunrong, Jiang Changyin. lithium ion battery LiBOB electrolytic salt research [J]. chemical progress, 2006, 18 (12): 1703-1709), this can greatly expand the range of choice of aprotic solvent in electrolyte, break away from EC(fusing point up to 37 ℃) dependence, and then be expected to promote by the optimization of dicyandiamide solution cryogenic property and the high rate performance of battery.Although but carried out more than ten years for the research of LiBOB and LiODFB, they not yet obtain large-scale practical application.It is higher that its main cause is that they form the resistance value of SEI film in carbonate solvent.
Summary of the invention
the object of the invention isfurther reduce the impedance of SEI film, and improve the compatibility of electrolyte and positive electrode, reduce the corrosion of electrolyte to positive electrode.
The present invention is a kind of high temperature electrolyte for high multiplying power lithium ion battery, and this electrolyte is usingd di-oxalate lithium borate, difluorine oxalic acid boracic acid lithium or their mixture as basic lithium salts; Using several solvents in ethylene carbonate, propene carbonate, gamma-butyrolacton, sulfolane, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, dimethyl sulfite, sulfurous acid diethyl ester combination as mixing aprotic organic solvent; Using sulfuric acid difluoro lithium borate or sulfurous acid difluoro lithium borate or their mixture as functional additive; The molality of basis lithium salts is 0.5 ~ 1.2 mol/kg.
The invention has the advantages that and using LiBOB or LiODFB as basic lithium salts, the organic solvent that contains element sulphur of usining one of forms as mixed solvent, with LiBSO 4f 2or LiBSO 3f 2as functional additive, under the guidance of mutual supplement with each other's advantages principle, set up novel electrolyte system, can obtain in high temperature high-multiplying-power battery field scale application.Constructed electrolyte system can tolerate the high temperature of 60 ℃, and the high rate performance of assembled battery, cycle performance are excellent.
Embodiment
The present invention is a kind of high temperature electrolyte for high multiplying power lithium ion battery, and this electrolyte is usingd di-oxalate lithium borate, difluorine oxalic acid boracic acid lithium or their mixture as basic lithium salts; Using several solvents in ethylene carbonate, propene carbonate, gamma-butyrolacton, sulfolane, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, dimethyl sulfite, sulfurous acid diethyl ester combination as mixing aprotic organic solvent; Using sulfuric acid difluoro lithium borate or sulfurous acid difluoro lithium borate or their mixture as functional additive; The molality of basis lithium salts is 0.5 ~ 1.2 mol/kg.
The molality of described basic lithium salts is 0.5 ~ 1.2 mol/kg.
In described mixing aprotic organic solvent, need to contain the ring-type organic solvent of at least one, i.e. ethylene carbonate, propene carbonate, gamma-butyrolacton, sulfolane simultaneously; With the chain organic solvent of at least one, i.e. dimethyl carbonate, or diethyl carbonate, or methyl ethyl carbonate, or dimethyl sulfite, or sulfurous acid diethyl ester; And the total organic solvent that contains element sulphur, i.e. sulfolane, or dimethyl sulfite, or sulfurous acid diethyl ester, be not less than 1/3 with the volume ratio of always mixing aprotic organic solvent.
The quality of functional additive accounts for 1% ~ 10% of solution and additive quality summation.
embodiment 1
In the present embodiment, the layoutprocedure of electrolyte is as follows: in ar gas environment, DEC and SL are mixed according to the ratio of volume ratio 1:1, in the organic solvent mixing, add LiBOB again, be made into the lithium salt solution that molality is 0.5 mol/kg, and then to add wherein mass ratio be 10% LiBSO 4f 2, to be added dose dissolve completely and mix after, can preparation cost invent needed electrolyte.
embodiment 2
In the present embodiment, in the present embodiment, the layoutprocedure of electrolyte is as follows: in ar gas environment, GBL and DMS are mixed according to the ratio of volume ratio 1:1, in the organic solvent mixing, add LiBOB again, be made into the lithium salt solution that molality is 1.2 mol/kg, and then to add wherein mass ratio be 3% LiBSO 4f 2, to be added dose dissolve completely and mix after, can preparation cost invent needed electrolyte.
embodiment 3
In the present embodiment, in the present embodiment, the layoutprocedure of electrolyte is as follows: in ar gas environment, GBL, SL, EMC are mixed according to the ratio of volume ratio 1:1:2, in the organic solvent mixing, add LiBOB again, be made into the lithium salt solution that molality is 0.7 mol/kg, and then to add wherein mass ratio be 8% LiBSO 3f 2, to be added dose dissolve completely and mix after, can preparation cost invent needed electrolyte.
embodiment 4
In the present embodiment, in the present embodiment, the layoutprocedure of electrolyte is as follows: in ar gas environment, EC, DMS are mixed according to the ratio of volume ratio 3:7, in the organic solvent mixing, add LiODFB again, be made into the lithium salt solution that molality is 0.8 mol/kg, and then to add wherein mass ratio be 3% LiBSO 3f 2, to be added dose dissolve completely and mix after, can preparation cost invent needed electrolyte.
embodiment 5
In the present embodiment, in the present embodiment, the layoutprocedure of electrolyte is as follows: in ar gas environment, PC, EMS, DMC are mixed according to the ratio of volume ratio 2:2:1, in the organic solvent mixing, add LiODFB again, be made into the lithium salt solution that molality is 0.7 mol/kg, and then to add wherein mass ratio be 5% LiBSO 3f 2, to be added dose dissolve completely and mix after, can preparation cost invent needed electrolyte.
embodiment 6
In the present embodiment, the layoutprocedure of electrolyte is as follows: in ar gas environment, SL and DMS are mixed according to the ratio of volume ratio 1:1, in the organic solvent mixing, add LiBOB again, be made into the lithium salt solution that molality is 0.6 mol/kg, and then to add wherein mass ratio be 1% LiBSO 3f 2, to be added dose dissolve completely and mix after, can preparation cost invent needed electrolyte.
comparative example 1
In the present embodiment, the layoutprocedure of electrolyte is as follows: in ar gas environment, EC and DMC are mixed according to the ratio of volume ratio 1:1, then add LiPF in the organic solvent mixing 6, be made into the lithium salt solution that molality is 1 mol/kg.
the assembling of test cell and performance test
(1) preparation of electrode plates
First by LiFePO 4or LiMn 2o 4or LiCoO 2, acetylene black and polyvinylidene fluoride (PVDF) be fully uniformly mixed with the mass ratio of 84:8:8, then the mixture obtaining evenly mixed according to the mass ratio of 1.5:1 with 1-METHYLPYRROLIDONE (NMP), makes anode sizing agent.Adopt coating machine that gained anode sizing agent is coated in aluminum foil current collector equably, with 120 ℃ at vacuumize, after cutting, rolling, obtain anode pole piece.
Carbonaceous mesophase spherules (MCMB) is fully uniformly mixed with the mass ratio of 92:8 with PVDF, then the mixture obtaining is evenly mixed according to the mass ratio of 1.5:1 with 1-METHYLPYRROLIDONE (NMP), make cathode size.Adopt coating machine that gained cathode size is coated on Copper Foil collector equably, with 110 ℃ at vacuumize, after cutting, rolling, obtain cathode pole piece.
(2) assembling of test cell
Above-mentioned anode pole piece, metal lithium sheet and polypropylene diaphragm are assembled into button lithium ion battery, the electrolyte that (in ar gas environment) injection embodiment 1-6 and comparative example 1 are prepared in glove box, then sealing, compressing tablet, make 2032 type lithium ion test cells and (be respectively LiFePO 4/ MCMB, LiMn 2o 4/ MCMB or LiCoO 2/ MCMB battery).
(3) high-temperature behavior of test cell test
Under high temperature (60 ℃) condition, the charge-discharge magnification with 0.5 C carries out 100 circulations to the test cell of being assembled respectively.The test result of the discharge capacitance after 100 circulations is in Table 1.Discharge capacitance after 100 circulations=(discharge capacity of discharge capacity/first of the 100th circulation) * 100%.
Discharge capacitance after table 1.100 time circulation
Figure 947164DEST_PATH_IMAGE001
(4) the high temperature high rate performance of test cell test
Under 60 ℃ of conditions, respectively with the charge-discharge magnification of 0.2 C, 1 C, 3 C to the LiFePO being assembled 4/ MCMB test cell discharges and recharges.After 10 circulations, according to its average discharge capacity, calculate the capability retention under different multiplying.The capability retention of capability retention under 1 C=(under 1 C under average discharge capacity/0.2 C of front 10 circulations the average discharge capacity of front 10 circulations) under * 100%, 3 C=(under 3 C under average discharge capacity/0.2 C of front 10 circulations the average discharge capacity of front 10 circulations) * 100%.In the time of 60 ℃, the discharge capacitance under different multiplying is in Table 2.
Discharge capacitance under table 2. different multiplying (60 ℃)
Figure 404690DEST_PATH_IMAGE002

Claims (4)

1. a high temperature electrolyte for high multiplying power lithium ion battery, is characterized in that this electrolyte usings di-oxalate lithium borate, difluorine oxalic acid boracic acid lithium or their mixture as basic lithium salts; Using several solvents in ethylene carbonate, propene carbonate, gamma-butyrolacton, sulfolane, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, dimethyl sulfite, sulfurous acid diethyl ester combination as mixing aprotic organic solvent; Using sulfuric acid difluoro lithium borate or sulfurous acid difluoro lithium borate or their mixture as functional additive; The molality of basis lithium salts is 0.5 ~ 1.2 mol/kg.
2. high temperature electrolyte for high multiplying power lithium ion battery according to claim 1, is characterized in that: the molality of described basic lithium salts is 0.5 ~ 1.2 mol/kg.
3. high temperature electrolyte for high multiplying power lithium ion battery according to claim 1, it is characterized in that: in described mixing aprotic organic solvent, need to contain the ring-type organic solvent of at least one, i.e. ethylene carbonate, propene carbonate, gamma-butyrolacton, sulfolane simultaneously; With the chain organic solvent of at least one, i.e. dimethyl carbonate, or diethyl carbonate, or methyl ethyl carbonate, or dimethyl sulfite, or sulfurous acid diethyl ester; And the total organic solvent that contains element sulphur, i.e. sulfolane, or dimethyl sulfite, or sulfurous acid diethyl ester, be not less than 1/3 with the volume ratio of always mixing aprotic organic solvent.
4. high temperature electrolyte for high multiplying power lithium ion battery according to claim 1, is characterized in that: the quality of functional additive accounts for 1% ~ 10% of solution and additive quality summation.
CN201310507641.1A 2013-10-24 2013-10-24 Electrolytic solution for high-temperature high-magnification type lithium ion battery Pending CN103531843A (en)

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Cited By (10)

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CN103825049A (en) * 2014-03-04 2014-05-28 东风商用车有限公司 High temperature-resistant electrolyte solution of lithium ion battery
CN105789703A (en) * 2016-03-10 2016-07-20 广州市香港科大霍英东研究院 Lithium difluoborate containing sulfonate group and battery employing lithium salt
CN106328999A (en) * 2016-11-29 2017-01-11 河南省法恩莱特新能源科技有限公司 High-rate electrolyte of lithium-ion battery
CN107293782A (en) * 2016-04-11 2017-10-24 宁德新能源科技有限公司 Nonaqueous electrolytic solution and lithium ion battery
CN108110321A (en) * 2017-12-27 2018-06-01 河南省法恩莱特新能源科技有限公司 A kind of lithium battery high-voltage electrolyte
JP2019106250A (en) * 2017-12-11 2019-06-27 トヨタ自動車株式会社 Nonaqueous electrolyte secondary battery
CN112086685A (en) * 2020-10-26 2020-12-15 长兴中俄新能源材料技术研究院 Three-lithium salt-quaternary solvent system performance complementary type 5V lithium ion battery electrolyte
CN113793918A (en) * 2021-09-08 2021-12-14 远景动力技术(江苏)有限公司 Lithium ion battery and preparation method thereof
WO2021248903A1 (en) * 2020-06-12 2021-12-16 厦门大学 High-temperature-resistant lithium ion battery system and charging and discharging method therefor
CN117293395A (en) * 2023-11-24 2023-12-26 中国第一汽车股份有限公司 Electrolyte and lithium ion battery comprising same

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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103825049A (en) * 2014-03-04 2014-05-28 东风商用车有限公司 High temperature-resistant electrolyte solution of lithium ion battery
CN103825049B (en) * 2014-03-04 2017-10-27 东风商用车有限公司 A kind of lithium-ion electric pool high temperature resistant electrolyte
CN105789703A (en) * 2016-03-10 2016-07-20 广州市香港科大霍英东研究院 Lithium difluoborate containing sulfonate group and battery employing lithium salt
CN107293782A (en) * 2016-04-11 2017-10-24 宁德新能源科技有限公司 Nonaqueous electrolytic solution and lithium ion battery
CN106328999A (en) * 2016-11-29 2017-01-11 河南省法恩莱特新能源科技有限公司 High-rate electrolyte of lithium-ion battery
JP2019106250A (en) * 2017-12-11 2019-06-27 トヨタ自動車株式会社 Nonaqueous electrolyte secondary battery
JP6994153B2 (en) 2017-12-11 2022-02-03 トヨタ自動車株式会社 Non-aqueous electrolyte secondary battery
CN108110321A (en) * 2017-12-27 2018-06-01 河南省法恩莱特新能源科技有限公司 A kind of lithium battery high-voltage electrolyte
CN113823829B (en) * 2020-06-12 2023-11-07 厦门大学 High-temperature-resistant lithium ion battery system and charging and discharging method thereof
WO2021248903A1 (en) * 2020-06-12 2021-12-16 厦门大学 High-temperature-resistant lithium ion battery system and charging and discharging method therefor
CN113823829A (en) * 2020-06-12 2021-12-21 厦门大学 High-temperature-resistant lithium ion battery system and charging and discharging method thereof
CN112086685A (en) * 2020-10-26 2020-12-15 长兴中俄新能源材料技术研究院 Three-lithium salt-quaternary solvent system performance complementary type 5V lithium ion battery electrolyte
CN112086685B (en) * 2020-10-26 2024-03-08 长兴中俄新能源材料技术研究院 Trilithium salt-quaternary solvent system performance complementary type 5V lithium ion battery electrolyte
CN113793918A (en) * 2021-09-08 2021-12-14 远景动力技术(江苏)有限公司 Lithium ion battery and preparation method thereof
CN113793918B (en) * 2021-09-08 2023-04-07 远景动力技术(江苏)有限公司 Lithium ion battery and preparation method thereof
CN117293395A (en) * 2023-11-24 2023-12-26 中国第一汽车股份有限公司 Electrolyte and lithium ion battery comprising same
CN117293395B (en) * 2023-11-24 2024-04-12 中国第一汽车股份有限公司 Electrolyte and lithium ion battery comprising same

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Application publication date: 20140122