CN104064810B - A kind of nonaqueous electrolytic solution and preparation method thereof and a kind of lithium secondary battery - Google Patents
A kind of nonaqueous electrolytic solution and preparation method thereof and a kind of lithium secondary battery Download PDFInfo
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- CN104064810B CN104064810B CN201410314883.3A CN201410314883A CN104064810B CN 104064810 B CN104064810 B CN 104064810B CN 201410314883 A CN201410314883 A CN 201410314883A CN 104064810 B CN104064810 B CN 104064810B
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
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Abstract
The invention discloses a kind of nonaqueous electrolytic solution and preparation method thereof and a kind of lithium secondary battery, mainly comprise following raw material: organic solvent, electric conducting lithium salt and additive, described organic solvent is made up of cyclic carbonate and linear carbonates solvent, described electric conducting lithium salt concentration in organic solvent is 0.8-1.5mol/L, described additive is at least one in the compound that the following formula (I) of consumption 0.01-8.0wt.% represents, in formula
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 becomes with fastest developing speed also the most valued novel high-energy accumulator at present because of advantages such as its specific energy are high, have extended cycle life. Current commercial lithium ion battery disclosure satisfy that the demand of major part household type electronic equipment substantially, as: digital camera, mobile phone and notebook computer etc. But, flourish recently as the continuous renewal of digital product and electric vehicle, the performances such as the service life of lithium ion battery, high temperature performance, safety, multiplying power are proposed increasingly higher requirement. Therefore, the research and development of lithium ion battery material are significant.
Lithium ion battery is mainly made up of positive pole, negative pole and electrolyte three part, and their structure and performance directly determine the combination property of battery. Current commercial lithium-ion battery electrolytes mainly with the mixed solvent of chain type and ring type carbonic ester be solvent, with LiPF6For supporting electrolyte, for the lithium ion the shuttling back and forth guarantee providing necessary between battery plus-negative plate. The negative material that lithium ion battery adopts is broadly divided into two classes: a class is can the metallic compound (alloy etc. of metal simple-substance, oxide and lithium) of removal lithium embedded, another kind of is carbon materials, as can the coke of removal lithium embedded, Delanium, native graphite and MCMB etc. But, covering can even be destroyed negative material at negative terminal surface generation reduction decomposition, the solid decomposer of generation and gas by organic electrolyte in the process that battery charges, and causes the increase of battery irreversible capacity and the reduction of cycle life. Anode material for lithium-ion batteries conventional at present mainly has cobalt acid lithium (LiCoO2), LiMn2O4 (LiMn2O4), trielement composite material and LiFePO4 (LiFePO4) four kinds. Although the electrochemical window width (0.7-4.5VvsLi of lithium ion battery organic carbonate electrolyte+/ Li). But research shows, even if organic carbonate electrolyte is at the relatively low (～3.5VvsLi of running voltage+/ Li) LiFePO4Material also can occur oxidation reaction.It addition, battery is at high temperature and under the catalytic action of some transition metals, organic electrolyte oxidation Decomposition on positive pole can be further exacerbated by, and even destroys positive electrode, the dissolution of aggravation transition metal. It addition, the solid decomposer of decomposition generation or gas will cover electrode surface or cause cell expansion, hinder the migration of lithium ion, worsen the chemical property of battery.
Adding a small amount of " chemical substance " in electrolyte system and form function electrolyte to improve some macro property of battery, this kind of " chemical substance " with some special efficacy is called " functional additive ". Due to the addition of new function additive, the performance that lithium ion battery is respectively leavened dough obtains obvious improvement. Functional additives for Li-ion battery electrolytes has become a focus of current Study on Li-ion batteries person. In the organic electrolyte of lithium ion battery, pyrrolidone-2 compounds is employed, it was shown that pyrrolidone-2 compounds can suppress the flatulence problem that battery high-temperature stores, and improves the discharge capacity of battery as Chinese patent ZL200410045142.6 discloses. But, containing lithium ion battery prepared by this material organic electrolyte, the Li that in its first charge-discharge process, loss is more+, causing that coulombic efficiency is relatively low, the interfacial film impedance of formation is higher, have impact on the chemical property of battery.
Summary of the invention
In view of the problem existing for background technology, it is an object of the invention to provide a kind of nonaqueous electrolytic solution and preparation method thereof, this electrolyte can increase the nonaqueous electrolytic solution wellability to lithium ion cell electrode, improve the efficiency for charge-discharge of lithium ion battery, and battery flatulence problem after storage at high temperatures can be suppressed. These character ensure that lithium ion battery has good cycle life and the performance of high voltage (more 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, including organic solvent, electric conducting lithium salt and additive, wherein: described organic solvent is selected from more than one of cyclic carbonate solvents, aromatic hydrocarbon solvent and linear solvent, and described additive structural formula is as follows:
Wherein R1And R2For hydrogen, halogen, C1-C6Alkyl and haloalkyl, C1-C4Itrile group, C1-C6Thiazolinyl, alkoxyl, carboxyl, phenyl ring, halogeno-benzene any one.
Described electric conducting lithium salt concentration 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 is 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 solvents be ethylene carbonate, Allyl carbonate, fluorinated ethylene carbonate, gamma-butyrolacton and gamma-valerolactone more than one.
Described aromatic hydrocarbon solvent be benzene, fluorobenzene, difluoro-benzene, toluene, trifluoro-benzene, dimethylbenzene more than one; Described linear solvents is more than one of dimethyl carbonate, Ethyl methyl carbonate, diethyl carbonate, ethyl acetate, methyl propyl carbonate, ethers and fluoro-ether.
Described electric conducting lithium salt is LiPF6、LiBF4、LiSO3CF3、LiClO4、Li(CF3SO2)2N、LiC(CF3SO2)3In more than one.
Described electrolyte also includes 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) use after organic solvent being mixed in proportionMolecular 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, prepare the nonaqueous electrolytic solution of the present invention.
A kind of lithium secondary battery, including positive pole, negative pole and barrier film, wherein: positive electrode is lithium-containing transition metal oxide, negative material is can more than one in the material with carbon element of intercalation/deintercalation lithium ion, lithium metal, silicon or stannum and oxide thereof; Barrier film be weave cotton cloth, the one of non-woven fabrics, synthetic resin micro-porous film; Lithium battery also includes the nonaqueous electrolytic solution of the present invention.
It is an advantage of the current invention that:
(1) additive sulfenyl tetrazole compound can increase the nonaqueous electrolytic solution wellability 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 to decompose the gas caused simultaneously and produce, reduce the expansion of battery.
(3) sulfenyl tetrazotized zole compound and typical additives can form more firmly interfacial film; this interfacial film can reduce transition metal from the dissolution positive pole; suppress transition metal deposition on negative pole and reduction; shield electrode material, is conducive to improving cyclical stability and high temperature, the high voltage capability of lithium ion battery.
Detailed description of the invention
Below by exemplary embodiment, the present invention will be further elaborated; But the scope of the present invention should not be limited to the scope of embodiment, any change not necessarily departing from present subject matter or change can be understood by those skilled in the art, all within 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 solvents (ethylene carbonate EC) and linear carbonate solvent (Ethyl methyl carbonate EMC), and the weight ratio of EC and linear carbonate is EC:EMC=1:2. Described electric conducting lithium salt LiPF6Concentration in organic solvent is 1.0mol/L, and described typical additives is the vinylene carbonate of 1.0wt.% consumption and consumption is the propane sultone of 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) use after organic solvent being mixed in proportionMolecular 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.
The nonaqueous electrolytic solution of the present invention is used for cobalt acid lithium/graphite flexible-packed battery, tests cobalt acid lithium/graphite flexible-packed battery cycle performance of 3.0-4.2V, 1C rate charge-discharge under normal temperature environment.
Embodiment 2
The preparation method of the nonaqueous electrolytic solution of the present embodiment and embodiment 1 are identical, institute the difference is that, use the 5-methyl mercapto tetrazole of 1.0wt.% consumption, the nonaqueous electrolytic solution so prepared be applied in full battery to test its performance according to the method identical with embodiment 1.
Embodiment 3
The preparation method of the nonaqueous electrolytic solution of the present embodiment and embodiment 1 are identical, institute the difference is that, use the 5-methyl mercapto tetrazole of 3.0wt.% consumption, the nonaqueous electrolytic solution so prepared be applied in full battery to test its performance according to the method identical with embodiment 1.
Embodiment 4
The preparation method of the nonaqueous electrolytic solution of the present embodiment and embodiment 1 are identical, institute the difference is that, use the 5-ethylmercapto group tetrazole of 1.0wt.% consumption, chemical formula is:
The nonaqueous electrolytic solution so prepared is applied in full battery to test its performance according to the method identical with embodiment 1.
Embodiment 5
The preparation method of the nonaqueous electrolytic solution of the present embodiment and embodiment 1 are identical, institute the difference is that, use the 5-ethylmercapto group tetrazole of 3.0wt.% consumption, the nonaqueous electrolytic solution so prepared be applied in full battery to test its performance according to the method identical with embodiment 1.
Embodiment 6
The preparation method of the nonaqueous electrolytic solution of the present embodiment and embodiment 1 are identical, institute the difference is that, use the 5-benzylthio tetrazole of 2.0wt.% consumption, chemical formula is:
The nonaqueous electrolytic solution so prepared is applied in full battery to test its performance according to the method identical with embodiment 1.
Embodiment 7
The preparation method of the nonaqueous electrolytic solution of the present embodiment and embodiment 1 are identical, institute the difference is that, use the 5-sulfydryl-1-phenyl tetrazole of 2.0wt.% consumption, chemical formula is:
The nonaqueous electrolytic solution so prepared is applied in full battery to test 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, institute the difference is that, use the 5-methyl mercapto tetrazole of 1.0wt.% consumption and the 5-ethylmercapto group tetrazole of 0.5wt.% consumption, the nonaqueous electrolytic solution so prepared is applied in full battery to test its performance according to the method identical with embodiment 1.
Comparative example 1,
The preparation method of the electrolyte of this comparative example and embodiment 1 are identical, institute the difference is that, do not use sulfenyl tetrazotized zole compound, the nonaqueous electrolytic solution so prepared be applied in full battery to test 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 of the electrolyte using the present invention to prepare, carry out following operation: conventionally prepare lithium cobaltate cathode sheet, graphite cathode sheet, using embodiment 1 to prepare electrolyte fluid injection in glove box uses above-mentioned pole piece to prepare 053048 type flexible-packed battery, with new prestige (BS-9300R type) battery test system, 053048 type battery of preparation being carried out charge-discharge test, the battery simultaneously prepared 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 blanking voltage, and constant voltage charges to cut-off current to be terminated less than 0.1C. It is placed in 60 DEG C of high-temperature cabinets and stores 7 days. Expansion rate calculation is following formula:
Wherein, T is the cell thickness after high temperature storage, T0For 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:
By data above this it appears that, lithium battery capacity conservation rate and high-temperature storage are affected substantially by additive, the present invention adopts sulfenyl tetrazotized zole compound to have prominent advantage as electrolysis additive, is mainly manifested in capability retention and the high temperature storage cell expansion rate of battery. Embodiment 1-8 is substantially better than comparative example, and the battery that therefore prepared by the electrolyte of the present invention has high security performance and durability, has high market value and social benefit.It is above illustrating of the possible embodiments for the present invention, but can not limit the scope of the invention.
Claims (7)
1. a nonaqueous electrolytic solution, including organic solvent, electric conducting lithium salt and additive, wherein: described organic solvent is selected from more than one of cyclic carbonate solvents, aromatic hydrocarbon solvent and linear solvent, and described additive structural formula is as follows:
Wherein R1And R2For hydrogen, halogen, C1-C6Alkyl and haloalkyl, C1-C4Itrile group, C2-C6Thiazolinyl, alkoxyl, carboxyl, phenyl ring, halogeno-benzene any one, wherein R1And R2Has at least one for C1-C4Itrile group or carboxyl, described linear solvent is more than one of dimethyl carbonate, Ethyl methyl carbonate, diethyl carbonate, ethyl acetate, methyl propyl carbonate, ethers and fluoro-ether.
2. nonaqueous electrolytic solution according to claim 1, wherein: described electric conducting lithium salt concentration 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, wherein: described cyclic carbonate solvents be ethylene carbonate, Allyl carbonate more than one.
4. nonaqueous electrolytic solution according to claim 1, wherein: described aromatic hydrocarbon solvent be benzene, fluorobenzene, difluoro-benzene, toluene, trifluoro-benzene, dimethylbenzene more than one.
5. nonaqueous electrolytic solution according to claim 1, wherein: described electric conducting lithium salt is LiPF6、LiBF4、LiSO3CF3、LiClO4、Li(CF3SO2)2N、LiC(CF3SO2)3In more than one.
6. nonaqueous electrolytic solution according to claim 1, wherein: also include 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, and described typical additives accounts for the 0.1-5.0% of nonaqueous electrolytic solution gross mass.
7. a lithium secondary battery, including positive pole, negative pole and barrier film, wherein: positive electrode is lithium-containing transition metal oxide, negative material is can more than one in the material with carbon element of intercalation/deintercalation lithium ion, lithium metal, silicon or stannum and oxide thereof; Barrier film be weave cotton cloth, the one of non-woven fabrics, synthetic resin micro-porous film; Lithium battery also includes the nonaqueous electrolytic solution described in any one of claim 1-6.
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