CN104064810A - Non-aqueous electrolyte, preparing method of non-aqueous electrolyte and lithium secondary battery - Google Patents
Non-aqueous electrolyte, preparing method of non-aqueous electrolyte and lithium secondary battery Download PDFInfo
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- CN104064810A CN104064810A CN201410314883.3A CN201410314883A CN104064810A CN 104064810 A CN104064810 A CN 104064810A CN 201410314883 A CN201410314883 A CN 201410314883A CN 104064810 A CN104064810 A CN 104064810A
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- electrolytic solution
- nonaqueous electrolytic
- carbonate
- lithium
- organic solvent
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M10/058—Construction or manufacture
-
- 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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a non-aqueous electrolyte, a preparing method of the non-aqueous electrolyte and a lithium secondary battery. The non-aqueous electrolyte mainly comprises an organic solvent, conductive lithium salt and an additive. The organic solvent is composed of cyclic carbonate and a linear carbonic ester solvent. The concentration of the conductive lithium salt in the organic solvent is 0.8-1.5 mol/L, the additive is one or more of compounds, of which the dosage is 0.01-8.0 percent by weight, shown in the following general formula (1), and the formula can be seen in the specifications. The compounds are added into the non-aqueous electrolyte so that the service life of a lithium ion battery can be prolonged, the high voltage (larger than 4.2 V) can be improved, the high and low temperature performance can be enhanced, and the air expansion problem of the battery can be solved.
Description
Technical field
The present invention relates to lithium ion battery preparation field, be specifically related to a kind of nonaqueous electrolytic solution and preparation method thereof and a kind of lithium secondary battery.
Background technology
Lithium ion battery is with fastest developing speed also the most valued current novel high-energy storage battery because the advantages such as its specific energy is high, have extended cycle life become.Current commercial lithium ion battery can meet the demand of most of domestic type electronic equipment substantially, as: digital camera, mobile phone and notebook computer etc.But, flourish along with the continuous renewal of digital product and electric vehicle in recent years, the performances such as useful life to lithium ion battery, high temperature performance, fail safe, multiplying power propose more and more higher requirement.Therefore, significant to the research and development of lithium ion battery material.
Lithium ion battery is mainly made up of positive pole, negative pole and electrolyte three parts, and their structure and performance have directly determined the combination property of battery.Current commercial lithium-ion battery electrolytes is mainly that mixed solvent taking chain type and ring type carbonic ester is as solvent, with LiPF
6for supporting electrolyte, for lithium ion shuttling back and forth between battery plus-negative plate provides necessary guarantee.The negative material that lithium ion battery adopts is mainly divided into two classes: a class be can removal lithium embedded metallic compound (alloy of metal simple-substance, oxide and lithium etc.), another kind of is carbon materials, as coke, Delanium, native graphite and MCMB etc. that can removal lithium embedded.But organic electrolyte can be in negative terminal surface generation reduction decomposition in the process of battery charging, covering is even destroyed negative material by the solid decomposer of generation and gas, causes the increase of battery irreversible capacity and the reduction of cycle life.Conventional anode material for lithium-ion batteries mainly contains cobalt acid lithium (LiCoO at present
2), LiMn2O4 (LiMn
2o
4), trielement composite material and LiFePO4 (LiFePO
4) four kinds.Although wide (the 0.7-4.5V vs Li of the electrochemical window of lithium ion battery organic carbonate electrolyte
+/ Li).But research shows, even if organic carbonate electrolyte is at the lower (～3.5V vs Li of operating voltage
+/ Li) LiFePO
4on material, also can there is oxidation reaction.In addition, battery is at high temperature and under the catalytic action of some transition metals, and the further aggravation of the oxidation Decomposition of organic electrolyte on positive pole, even destroys positive electrode, the stripping of aggravation transition metal.In addition, decompose the solid decomposer or the gas that produce and will cover electrode surface or cause cell expansion, hinder the migration of lithium ion, worsen the chemical property of battery.
In electrolyte system, add a small amount of " chemical substance " formation function electrolyte to improve some macro property of battery, " chemical substance " that this class has some special efficacy is called " functional additive ".Due to adding of new function additive, the performance of the each fermentation of lithium ion battery has obtained obvious improvement.Functional additives for Li-ion battery electrolytes has become current Study on Li-ion batteries using person's a focus.Use pyrrolidone-2 compounds as Chinese patent ZL200410045142.6 discloses in the organic electrolyte of lithium ion battery, shown that pyrrolidone-2 compounds can suppress the inflatable problem that battery high-temperature stores, and improve the discharge capacity of battery.But, the lithium ion battery of preparing containing this material organic electrolyte, the more Li of loss in its first charge-discharge process
+, cause coulomb efficiency lower, the interfacial film impedance of formation is higher, has affected the chemical property of battery.
Summary of the invention
In view of the existing problem of background technology, the object of the present invention is to provide a kind of nonaqueous electrolytic solution and preparation method thereof, this electrolyte can increase the wettability of nonaqueous electrolytic solution to lithium ion cell electrode, improve the efficiency for charge-discharge of lithium ion battery, and can suppress the inflatable problem of battery after high temperature storage.These character have ensured that lithium ion battery has the performance of good cycle life and high voltage (being greater than 4.2V), high low temperature.
Another object of the present invention is to provide a kind of lithium secondary battery.
The present invention is achieved through the following technical solutions:
A kind of nonaqueous electrolytic solution, comprises organic solvent, electric conducting lithium salt and additive, and wherein: described organic solvent is selected from more than one of cyclic carbonate ester solvent, aromatic hydrocarbon solvent and linear solvent, described additive structural formula is as follows:
Wherein R
1and R
2for hydrogen, halogen, C
1-C
6alkyl and haloalkyl, C
1-C
4itrile group, C
1-C
6any of thiazolinyl, alkoxyl, carboxyl, phenyl ring, halogeno-benzene.
The concentration of described electric conducting lithium salt in organic solvent is 0.8-1.5mol/L, and the consumption of described additive is the 0.1-8.0% of organic solvent weight.
Described additive can be selected from more than one of 5-methyl mercapto tetrazole, 5-ethylmercapto group tetrazole, 5-benzylthio tetrazole and 5-sulfydryl-1-phenyl tetrazole.
Described cyclic carbonate ester solvent be ethylene carbonate, propene carbonate, fluorinated ethylene carbonate, gamma-butyrolacton and γ-penta Inner ester more than one.
Described aromatic hydrocarbon solvent is more than one of benzene, fluorobenzene, difluoro-benzene, toluene, trifluoro-benzene, dimethylbenzene; Described line style solvent is more than one of dimethyl carbonate, methyl ethyl carbonate, diethyl carbonate, ethyl acetate, methyl propyl carbonate, ethers and fluoro-ether.
Described electric conducting lithium salt is LiPF
6, LiBF
4, LiSO
3cF
3, LiClO
4, Li (CF
3sO
2)
2n, LiC (CF
3sO
2)
3in more than one.
Described electrolyte also comprises typical additives, described typical additives is more than one in vinylene carbonate, vinylethylene carbonate, fluorinated ethylene carbonate, propane sultone, butyl sultone, adiponitrile, succinonitrile, LiBOB, LiODFB etc., and described typical additives accounts for the 0.1-5.0% of nonaqueous electrolytic solution gross mass.
A kind of preparation method of electrolyte, the compound method of electrolyte is:
(1) organic solvent is mixed to rear use in proportion
molecular sieve, calcium hydride, lithium hydride clarification, dewater;
(2) at ambient temperature, electric conducting lithium salt is dissolved in above-mentioned organic solvent, and stirs;
(3) add typical additives, and stir.
(4) add additive, make nonaqueous electrolytic solution of the present invention.
A kind of lithium secondary battery, comprises positive pole, negative pole and barrier film, and wherein: positive electrode is lithium-containing transition metal oxide, negative material is more than one in material with carbon element, lithium metal, silicon or tin and the oxide thereof that can embed/deviate from lithium ion; Barrier film be weave cotton cloth, the one of nonwoven fabrics, synthetic resin micro-porous film; Lithium battery also comprises nonaqueous electrolytic solution of the present invention.
The invention has the advantages that:
(1) additive sulfenyl tetrazole compound can increase the wettability of nonaqueous electrolytic solution to lithium ion battery electrode material and barrier film.
(2) sulfenyl tetrazotized zole compound can improve the electrode/electrolyte interfacial property of lithium ion battery, reduce interface resistance and improve ion mobility, improve low temperature performance, suppress organic solvent simultaneously and decompose the γ-ray emission causing, reduce the expansion of battery.
(3) sulfenyl tetrazotized zole compound and typical additives can form more firmly interfacial film; this interfacial film can reduce the stripping of transition metal from positive pole; suppress deposition and the reduction of transition metal on negative pole; guard electrode material, is conducive to improve the cyclical stability of lithium ion battery and high temperature, high voltage capability.
Embodiment
Below by exemplary embodiment, the present invention will be further elaborated; But scope of the present invention should not be limited to the scope of embodiment, any variation or change that does not depart from purport of the present invention can be understood by those skilled in the art, all in protection scope of the present invention.
Embodiment 1
A kind of nonaqueous electrolytic solution, consist predominantly of machine solvent, electric conducting lithium salt and additive, described organic solvent is made up of cyclic carbonate ester solvent (ethylene carbonate EC) and linear carbonate solvent (methyl ethyl carbonate EMC), and the weight ratio of EC and linear carbonate is EC:EMC=1:2.Described electric conducting lithium salt LiPF
6concentration in organic solvent is 1.0mol/L, and described typical additives is the vinylene carbonate of 1.0wt.% consumption and the propane sultone that consumption is 1.0wt.%, and described additive is 5-methyl mercapto tetrazole, consumption 0.5wt.%.The chemical formula of described additive is as follows:
The compound method of electrolyte is:
(1) organic solvent is mixed to rear use in proportion
molecular sieve, calcium hydride, lithium hydride clarification, dewater;
(2) at ambient temperature, electric conducting lithium salt is dissolved in above-mentioned organic solvent, and stirs;
(3) add typical additives vinylene carbonate and propane sultone, and stir.
(4) add additive 5-methyl mercapto tetrazole, obtain non-aqueous electrolyte for lithium ion cell described in the present embodiment.
Nonaqueous electrolytic solution of the present invention, for cobalt acid lithium/graphite flexible-packed battery, is tested to cobalt acid lithium/graphite flexible-packed battery 3.0-4.2V under normal temperature environment, the cycle performance of 1C rate charge-discharge.
Embodiment 2
The preparation method of the nonaqueous electrolytic solution of the present embodiment is identical with embodiment 1, and difference is, uses the 5-methyl mercapto tetrazole of 1.0wt.% consumption, and the nonaqueous electrolytic solution of so preparation is applied to and in full battery, tests its performance according to the method identical with embodiment 1.
Embodiment 3
The preparation method of the nonaqueous electrolytic solution of the present embodiment is identical with embodiment 1, and difference is, uses the 5-methyl mercapto tetrazole of 3.0wt.% consumption, and the nonaqueous electrolytic solution of so preparation is applied to and in full battery, tests its performance according to the method identical with embodiment 1.
Embodiment 4
The preparation method of the nonaqueous electrolytic solution of the present embodiment is identical with embodiment 1, and difference is, uses the 5-ethylmercapto group tetrazole of 1.0wt.% consumption, and chemical formula is:
The nonaqueous electrolytic solution of so preparation is applied to and in full battery, tests its performance according to the method identical with embodiment 1.
Embodiment 5
The preparation method of the nonaqueous electrolytic solution of the present embodiment is identical with embodiment 1, and difference is, uses the 5-ethylmercapto group tetrazole of 3.0wt.% consumption, and the nonaqueous electrolytic solution of so preparation is applied to and in full battery, tests its performance according to the method identical with embodiment 1.
Embodiment 6
The preparation method of the nonaqueous electrolytic solution of the present embodiment is identical with embodiment 1, and difference is, uses the 5-benzylthio tetrazole of 2.0wt.% consumption, and chemical formula is:
The nonaqueous electrolytic solution of so preparation is applied to and in full battery, tests its performance according to the method identical with embodiment 1.
Embodiment 7
The preparation method of the nonaqueous electrolytic solution of the present embodiment is identical with embodiment 1, and difference is, uses 5-sulfydryl-1-phenyl tetrazole of 2.0wt.% consumption, and chemical formula is:
The nonaqueous electrolytic solution of so preparation is applied to and in full battery, tests its performance according to the method identical with embodiment 1.
Embodiment 8
The preparation method of the nonaqueous electrolytic solution of the present embodiment is identical with embodiment 1, difference is, use the 5-methyl mercapto tetrazole of 1.0wt.% consumption and the 5-ethylmercapto group tetrazole of 0.5wt.% consumption, the nonaqueous electrolytic solution of so preparation is applied to and in full battery, tests its performance according to the method identical with embodiment 1.
Comparative example 1,
The preparation method of the electrolyte of this comparative example is identical with embodiment 1, and difference is, does not use sulfenyl tetrazotized zole compound, and the nonaqueous electrolytic solution of so preparation is applied to and in full battery, tests its performance according to the method identical with embodiment 1.
The application experiment of embodiment and comparative example:
Charge-discharge test condition: in order to measure the battery charging and discharging performance that uses the electrolyte that makes of the present invention, carry out following operation: prepare lithium cobaltate cathode sheet, graphite cathode sheet according to conventional method, using embodiment 1 to prepare electrolyte fluid injection in glove box uses above-mentioned pole piece to prepare 053048 type flexible-packed battery, 053048 type battery of preparation is carried out to charge-discharge test with new prestige (BS-9300R type) battery test system, the battery of simultaneously preparing with comparative example electrolyte compares.Battery circulates with 1C charge-discharge magnification in the scope of voltage 3.0-4.2V.
High temperature storage experiment condition: battery is with 1C multiplying power constant current charge to cut-ff voltage, and constant voltage charges to cut-off current and is less than 0.1C and finishes.Being placed in 60 DEG C of high-temperature cabinets stores 7 days.Expansion rate account form is following formula:
Wherein, T is the cell thickness after high temperature storage, T
0for the cell thickness before high temperature storage.Lithium ion battery part of detecting result is referring to table 1.
Table 1 is the test result of embodiment:
Can obviously find out by above data, additive is obvious on lithium battery capacity conservation rate and high-temperature storage impact, the present invention adopts sulfenyl tetrazotized zole compound to have outstanding advantage as electrolysis additive, is mainly manifested in capability retention and the high temperature storage cell expansion rate of battery.Embodiment 1-8 is obviously better than comparative example, and the battery that therefore prepared by electrolyte of the present invention has high security performance and durability, has high market value and social benefit.Be more than for the illustrating of possible embodiments of the present invention, but can not limit the scope of the invention.
Claims (9)
1. a nonaqueous electrolytic solution, comprises organic solvent, electric conducting lithium salt and additive, and wherein: described organic solvent is selected from more than one of cyclic carbonate ester solvent, aromatic hydrocarbon solvent and linear solvent, described additive structural formula is as follows:
Wherein R
1and R
2for hydrogen, halogen, C
1-C
6alkyl and haloalkyl, C
1-C
4itrile group, C
1-C
6any of thiazolinyl, alkoxyl, carboxyl, phenyl ring, halogeno-benzene.
2. nonaqueous electrolytic solution according to claim 1, wherein: the concentration of described electric conducting lithium salt in organic solvent is 0.8-1.5mol/L, the consumption of described additive is the 0.1-8.0% of organic solvent weight.
3. nonaqueous electrolytic solution according to claim 1, is characterized in that: described additive can be selected from more than one of 5-methyl mercapto tetrazole, 5-ethylmercapto group tetrazole, 5-benzylthio tetrazole and 5-sulfydryl-1-phenyl tetrazole.
4. nonaqueous electrolytic solution according to claim 1, wherein: described cyclic carbonate ester solvent be ethylene carbonate, propene carbonate, fluorinated ethylene carbonate, gamma-butyrolacton and γ-penta Inner ester more than one.
5. nonaqueous electrolytic solution according to claim 1, wherein: described aromatic hydrocarbon solvent is more than one of benzene, fluorobenzene, difluoro-benzene, toluene, trifluoro-benzene, dimethylbenzene; Described line style solvent is more than one of dimethyl carbonate, methyl ethyl carbonate, diethyl carbonate, ethyl acetate, methyl propyl carbonate, ethers and fluoro-ether.
6. nonaqueous electrolytic solution according to claim 1, wherein: described electric conducting lithium salt is LiPF
6, LiBF
4, LiSO
3cF
3, LiClO
4, Li (CF
3sO
2)
2n, LiC (CF
3sO
2)
3in more than one.
7. nonaqueous electrolytic solution according to claim 1, wherein: also comprise typical additives, described typical additives is more than one in vinylene carbonate, vinylethylene carbonate, fluorinated ethylene carbonate, propane sultone, butyl sultone, adiponitrile, succinonitrile, LiBOB, LiODFB etc., and described typical additives accounts for the 0.1-5.0% of nonaqueous electrolytic solution gross mass.
8. a preparation method of electrolyte, the compound method of electrolyte is:
(1) organic solvent is mixed to rear use in proportion
molecular sieve, calcium hydride, lithium hydride clarification, dewater;
(2) at ambient temperature, electric conducting lithium salt is dissolved in above-mentioned organic solvent, and stirs;
(3) add typical additives, and stir.
(4) add additive, make the nonaqueous electrolytic solution described in claim 1-7 any one.
9. a lithium secondary battery, comprises positive pole, negative pole and barrier film, and wherein: positive electrode is lithium-containing transition metal oxide, negative material is more than one in material with carbon element, lithium metal, silicon or tin and the oxide thereof that can embed/deviate from lithium ion; Barrier film be weave cotton cloth, the one of nonwoven fabrics, synthetic resin micro-porous film; Lithium battery also comprises the nonaqueous electrolytic solution described in claim 1-8 any one.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106099192A (en) * | 2016-08-22 | 2016-11-09 | 周泽 | Utilize the electrolyte preventing box hat from corroding prepared by sulfenyl tetrazole compound |
| CN106299458A (en) * | 2016-08-22 | 2017-01-04 | 周泽 | Utilize the electrolyte preventing box hat from corroding prepared by dimethylamine borane |
| CN112864468A (en) * | 2021-01-28 | 2021-05-28 | 苏州酷卡环保科技有限公司 | Formation method of power lithium ion battery |
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| US20130149596A1 (en) * | 2011-12-12 | 2013-06-13 | E.I Du Pont De Nemours And Company | Electrolyte solvent containing ionic liquids |
| CN103181022A (en) * | 2010-10-25 | 2013-06-26 | 丰田自动车株式会社 | Electrolyte solution for lithium battery, lithium battery including electrolyte solution, electrolyte solution for lithium air battery, and lithium air battery including electrolyte solution |
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| CN103181022A (en) * | 2010-10-25 | 2013-06-26 | 丰田自动车株式会社 | Electrolyte solution for lithium battery, lithium battery including electrolyte solution, electrolyte solution for lithium air battery, and lithium air battery including electrolyte solution |
| JP2013053105A (en) * | 2011-09-05 | 2013-03-21 | Nagoya Institute Of Technology | Mesoionic compound, electrolytic solution comprising the same for use in cell, and cell comprising the electrolytic solution |
| US20130149596A1 (en) * | 2011-12-12 | 2013-06-13 | E.I Du Pont De Nemours And Company | Electrolyte solvent containing ionic liquids |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106099192A (en) * | 2016-08-22 | 2016-11-09 | 周泽 | Utilize the electrolyte preventing box hat from corroding prepared by sulfenyl tetrazole compound |
| CN106299458A (en) * | 2016-08-22 | 2017-01-04 | 周泽 | Utilize the electrolyte preventing box hat from corroding prepared by dimethylamine borane |
| CN106299458B (en) * | 2016-08-22 | 2019-01-08 | 宁夏天绿健知识产权运营有限公司 | Utilize the electrolyte for preventing steel shell from corroding of dimethylamine borane preparation |
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| CN104064810B (en) | 2016-06-15 |
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