CN105703007A - Non-aqueous electrolyte for high-voltage rapid-charging type lithium ion battery - Google Patents
Non-aqueous electrolyte for high-voltage rapid-charging type lithium ion battery Download PDFInfo
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- CN105703007A CN105703007A CN201610192798.3A CN201610192798A CN105703007A CN 105703007 A CN105703007 A CN 105703007A CN 201610192798 A CN201610192798 A CN 201610192798A CN 105703007 A CN105703007 A CN 105703007A
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a non-aqueous electrolyte for a high-voltage rapid-charging type lithium ion battery. The non-aqueous electrolyte comprises a solvent, a commonly-used lithium salt, a positive electrode film-forming additive, lithium bis(polyfluoroalkyloxysulfonyl) imide, a fluoro-ester additive, an organic nitrile additive and a lithium battery electrolyte additive, wherein the ingredients are as follows in parts by weight: 100 parts of solvent, 0.2-10 parts of positive electrode film-forming additive, 0.2-10 parts of lithium bis(polyfluoroalkyloxysulfonyl) imide, 0.2-10 parts of fluoro-ester additive and 0.2-10 parts of organic nitrile additive; the solvent is cyclic carbonate and/or chain carbonate; and the molar concentration of the commonly-used lithium salt in the solvent is 0.8-1.5mol/L. According to the non-aqueous electrolyte provided by the invention, the oxidation resistance and wettability of the electrolyte, the oxidation resistance of the positive electrode SEI film in initial formation and the stability of the negative electrode SEI film can be improved; and the normal temperature rapid-charging circulation, the high-temperature 45-DEG C rapid-charging circulation and the high-temperature storage of the high-voltage electrolyte can be greatly improved.
Description
[technical field]
The present invention relates to the electrolyte of lithium ion battery, particularly relate to the nonaqueous electrolytic solution of a kind of high voltage fast charging type lithium ion battery。
[background technology]
Currently used anode material for lithium-ion batteries, such as LiCoOO、LiMn2O4,LiCoNiMnO2,LiFePO4Low etc. running voltage at below 4V, gram volume is 90-150mg/g。The way promoting battery energy density mainly has 2 kinds, a kind of charge cutoff voltage being to improve tradition positive electrode, such as cobalt acid lithium charging voltage is promoted to 4.35V, 4.4V, the capacity of its battery can promote about 15%, but being limited by promoting the way of charge cutoff voltage, further lifting can cause the poor stability of structure during cobalt acid lithium excessively de-lithium。
But, along with the raising of running voltage and charge cutoff voltage, the oxidation activity of positive electrode improves, the reaction of positive active material and electrolyte is also accelerated therewith, causing that battery flatulence under high voltages is serious, cycle performance reduces, and seriously constrains the performance of positive electrode performance。
[summary of the invention]
The technical problem to be solved in the present invention is to provide the nonaqueous electrolytic solution of the excellent high voltage fast charging type lithium ion battery of a kind of charge-discharge performance, and the room temperature to improve lithium ion battery fills cycle performance soon, and 45 ° of high temperature fill cycle performance and high-temperature storage performance soon。
In order to solve above-mentioned technical problem, the technical solution used in the present invention is, the nonaqueous electrolytic solution of a kind of high voltage fast charging type lithium ion battery, including solvent, conventional lithium salts, positive pole film for additive, double; two (polyfluoroalkoxy sulphonyl) imines lithium salts, fluoro esters additive, organic nitrile additive and lithium battery electrolytes additive；Wherein,
Solvent is cyclic carbonate and/or linear carbonate, and conventional lithium salts molar concentration in a solvent is 0.8-1.5mol/L。
Above-described nonaqueous electrolytic solution, described cyclic carbonate is at least one in ethylene carbonate, Allyl carbonate, fluorinated ethylene carbonate and gamma-butyrolacton。
Above-described nonaqueous electrolytic solution, described linear carbonate is at least one in dimethyl carbonate, diethyl carbonate, Ethyl methyl carbonate, methyl propyl carbonate and ethyl propyl carbonic acid ester。
Above-described nonaqueous electrolytic solution, described fluoro carbonic ester class additive is fluorinated ethylene carbonate and/or difluorinated ethylene carbonate。
Above-described nonaqueous electrolytic solution, described double; two (polyfluoroalkoxy sulphonyl) imines lithium salts are double; two pentafluoroethyl group sulfimide lithium (Li (C2F5SO2)2N), trifluoromethyl pentafluoroethyl group sulfimide lithium (Li (CF3SO2)(C2F5SO2) N), bis trifluoromethyl sulfimide lithium (Li (CF3SO2)2N) at least one and in double; two (fluorine sulphonyl) imine lithium (LiFSI)。
Above-described nonaqueous electrolytic solution, described organic nitrile be added to succinonitrile (110-61-2), adiponitrile (111-69-3), glutaronitrile (544-13-8), 3,3'-oxydipropionitrile (CAS:1656-48-0), ethylene glycol bis (propionitrile) ether (CAS:3386-87-6), 1,2,3-tri-(2-cyanato-) propane (2465-93-2), 1,3,5 penta trimethylsilyl nitriles (4379-04-8), 1,2,3 third trimethylsilyl nitriles (62872-44-0), 1, at least one in 3,6 hexanes three nitrile (1772-25-4)。
Above-described nonaqueous electrolytic solution, described positive pole film for additive is at least one in vinyl ethylene carbonate (VEC), methane-disulfonic acid methylene ester (MMDS), three (trimethyl silane) borate (TMSB), three (trimethyl silane) phosphate ester (TMSP) and three (trimethyl silane) phosphate ester (TMSPi)。
Above-described nonaqueous electrolytic solution, described conventional lithium salts is LiPF6、LiBF4、LiC1O4、LiAsF6, LiBOB, LiDFOB and LiPF4C2O4In at least one。
Above-described nonaqueous electrolytic solution, including conventional lithium battery electrolytes additive, the content of conventional lithium battery electrolytes additive is 0-10 weight portion；Conventional lithium battery electrolytes additive is vinylene carbonate (VC), sulfuric acid vinyl ester (DTD), ethylene sulfite (ES), 1,3 propane sultones, 1,3 propene sultone, 1,4 butyl sultones, 1, at least one in 4-butanediol sulfuric ester and acrylic-1,3-sultones。
The present invention passes through being used in combination of positive pole film for additive, double; two (polyfluoroalkoxy sulphonyl) imines lithium salts fluoro carbonic ester class additive and organic nitrile additive, the oxidative resistance of the oxidative resistance of electrolyte, the wellability of electrolyte, positive pole SEI film when first chemical conversion can be improved, the stability of negative pole SEI film, hence it is evident that improve high-voltage electrolyte room temperature fill soon circulation, high temperature 45 ° soon fill circulation and high-temperature storage performance。
[detailed description of the invention]
The nonaqueous electrolytic solution of the high voltage fast charging type lithium ion battery of the present invention by solvent, lithium salts, improve high temperature circulation class additive, double; two (polyfluoroalkoxy sulphonyl) imines lithium salts, fluoro esters additive, organic nitrile additive and lithium battery electrolytes additive and form。Wherein, solvent 100 weight portion；Double; two (polyfluoroalkoxy sulphonyl) imines lithium salts 0.2-10 weight portion；Improve high temperature circulation class additive 0.2-10 weight portion；Fluoro carbonic ester class additive 0.2-10 weight portion；Organic nitrile additive 0.2-10 weight portion；Conventional lithium battery electrolytes additive 0-5 weight portion；Solvent is cyclic carbonate and/or linear carbonate, and conventional lithium salts molar concentration in a solvent is 0.8-1.5mol/L。
Double; two (polyfluoroalkoxy sulphonyl) imines lithium salts is for being melted into and forming stable SEI film in negative terminal surface in cyclic process, to ensure that battery has the cycle performance of excellence, containing sulphur compound in the SEI film of its formation, form SEI and there is better heat stability, therefore show good high-temperature storage performance and high temperature cyclic performance。
Positive pole film for additive (improves high temperature circulation class additive) for forming stable SEI film at positive electrode surface in chemical conversion and cyclic process, has good high temperature and cycle performance。
Fluoro carbonic ester class additive is by the sucting electronic effect of F element, also advantageously improve the solvent molecule reduction potential on Carbon anode surface, optimize solid electrolyte interface film, improve the compatibility of electrolyte and active material, and then the chemical property of stabilized electrodes, there is good resistance to oxidation resistance, it is possible to significantly improve the cycle performance of high-voltage battery。
Although organic nitriles substance can suppress the decomposition of electrolyte, it is suppressed that flatulence, it is possible to catch the metal ion of dissolution, but after positive pole film forming, positive pole impedance becomes big, and cycle performance decreases。Therefore, the addition of nitrile is chosen as 0.2～10 weight portion, although FEC can improve cycle performance, but FEC at high temperature can produce HF, the HF decomposition to electrolyte solvent and have catalytic action, thus add FEC and the high-temperature storage performance of battery can be made to be deteriorated。Therefore, the addition of FEC is chosen as 0.2～10 weight portion。
Organic nitriles substance can absorb a small amount of water and HF, forms amide substance, reduces due to HF and POF3Deng catalysis, make electrolyte solvent decompose the high temperature flatulence that causes；Nitriles substance can form stabilising membrane at positive electrode surface in first charge-discharge process, effectively suppressing positive pole oxidation electrolyte, thus suppressing high temperature flatulence, improving high temperature storage and cycle performance。The stability that the both positive and negative polarity SEI film that can significantly improve electrolyte under high voltage condition is used in combination of above four kinds of additives, effectively suppresses solvent oxidation to decompose, thus improving electrolyte cycle performance under high voltage condition。
Conventional lithium salts is LiPF6、LiBF4、LiC1O4、LiAsF6, LiBOB, LiDFOB, LiPF4C2O4In one or more arbitrarily mix, molar concentration in a solvent is concentration is 0.8～1.5mol/L。
Cyclic carbonate is preferably at least one in ethylene carbonate (EC), Allyl carbonate (PC), fluorinated ethylene carbonate (FEC) and gamma-butyrolacton (GBL)；
Linear carbonate is preferably at least one in dimethyl carbonate (DMC), diethyl carbonate (DEC), Ethyl methyl carbonate (EMC), methyl propyl carbonate (MPC) and ethyl propyl carbonic acid ester (EPC)。
Double; two (polyfluoroalkoxy sulphonyl) imines lithium salts is added to double; two pentafluoroethyl group sulfimide lithium (Li (C2F5SO2)2N), trifluoromethyl pentafluoroethyl group sulfimide lithium (Li (CF3SO2)(C2F5SO2) N), bis trifluoromethyl sulfimide lithium (Li (CF3SO2)2N) at least one in, double; two (fluorine sulphonyl) imine lithium (LiFSI)。
Organic nitrile be added to succinonitrile (110-61-2), adiponitrile (111-69-3), glutaronitrile (544-13-8), 3,3'-oxydipropionitrile (CAS:1656-48-0), ethylene glycol bis (propionitrile) ether (CAS:3386-87-6), 1,2,3-tri-(2-cyanato-) propane (2465-93-2), 1,3,5 penta trimethylsilyl nitriles (4379-04-8), 1,2,3 third trimethylsilyl nitriles (62872-44-0), 1, at least one in 3,6 hexanes three nitrile (1772-25-4)。
Described lithium salts is LiPF6、LiBF4、LiC1O4、LiAsF6, LiBOB, LiDFOB, LiPF4C2O4Or at least one。
Conventional lithium battery electrolytes additive includes vinylene carbonate (VC), sulfuric acid vinyl ester (DTD), ethylene sulfite (ES), 1,3 propane sultones, 1,3 propene sultone, Isosorbide-5-Nitrae butyl sultone, at least one in BDO sulfuric ester。
Embodiment 1
Preparing electrolyte in BRAUN glove box, being full of purity in glove box is the nitrogen of 99.999%, and in glove box, moisture Control is at≤5ppm, and temperature is in room temperature。By 30 grams of EC, 70 grams of EMC, mix homogeneously, seal, put in refrigerator after it is cooled to 8 DEG C, be transferred in glove box, then add LiPF in two batches6It is sufficiently mixed, forms the nonaqueous electrolytic solution of the lithium ion battery that conventional lithium salts molar concentration is 1mol/L, above nonaqueous electrolytic solution adds the FEC of solvent gross mass 3%, 2%LIFSI, 3% propane sultone, the adiponitrile 1.5 of 2%, after Homogeneous phase mixing, obtain high-voltage lithium ion nonaqueous electrolytic solution。
The compound method of other embodiments and comparative example carries out with reference to the compound method of embodiment 1 below。
Wherein, FEC (CAS:114435-02-8), 1, 3, 5 penta trimethylsilyl nitriles (4379-04-8), 1, 2, 3 third trimethylsilyl nitriles (62872-44-0), 1, 3, 6 hexanes three nitrile (1772-25-4), 1, 3 propene sultone (21806-61-1), 1, 3 propane sultones, 1, 8 LOMAR PWA EINECS 246-676-2 lactones (83-31-8), 1, 4 butyl sultones (1633-83-6), 1, 4 butyl sultones (CAS:1633-83-6), methane-disulfonic acid methylene ester (CAS:99591-74-9), 1, 4-butanediol sulfuric ester, acrylic-1, the materials such as 3-sultones (CAS:21806-61-1) are purchased from lark prestige Science and Technology Ltd., DFEC (CAS:311810-76-1), purchased from Su Wei (Shanghai) Co., Ltd., double, two pentafluoroethyl group sulfimide lithium (Li (C2F5SO2)2N), trifluoromethyl pentafluoroethyl group sulfimide lithium (Li (CF3SO2)(C2F5SO2) N), bis trifluoromethyl sulfimide lithium (Li (CF3SO2)2N), double; two (fluorine sulphonyl) imine lithium (LiFSI) purchased from Suzhou Yacoo Chemical Reagent Corporation。
The constituent content table of table 1: embodiment 1-5
The constituent content table of table 2: comparative example 1-3
Performance test
The preparation of positive plate: prepare the anode pole piece of lithium ion battery: be dissolved in 1-methyl-9-pyrrolidone solution by the Kynoar (PVDF) that mass percent is 3%, by the cobalt acid lithium (LiCoO of mass percent 96%2), mass percent 3% conductive agent white carbon black add above-mentioned solution mix homogeneously, after the slurry being blended is coated on the two sides of the plus plate current-collecting body that aluminium foil is constituted, dry compacting as anode pole piece, the compacted density of positive pole is 4.05g/cm3。
The preparation of cathode pole piece: the thickening agent of mass percent to be the binding agent of 4%SBR (polystyrene, butadiene suspension), mass percent be 1%CMC (sodium carboxymethyl cellulose) is dissolved in aqueous solution, it is that 95% graphite adds above-mentioned solution by mass percent, mix homogeneously, after the slurry being blended is coated on the two sides of the negative current collector that Copper Foil is constituted, dry compacting as cathode pole piece。
Dry battery core is with high pressure cobalt acid lithium for positive pole, and with graphite for negative pole, microporous polyethylene film is that square dry battery core made by barrier film。Dry battery core is moved into after 80-85 DEG C of oven for drying 48 hours glove box stand-by。Respectively the various embodiments described above and comparative example gained electrolyte being injected the dry battery core that above-mentioned drying is good, then stand 24 hours, preliminary filling is once melted into, sealing, after secondary chemical conversion, obtains embodiment and comparative example experimental cell。
High voltage 2C fills cycle performance soon to be tested room temperature 25 ± 2 DEG C, when relative humidity 45-75%, embodiment and comparative example experimental cell are carried out 3-4.35V cycle performance of battery test, testing procedure is: a.2C constant-current charge is to 4.35V, and then constant-voltage charge is to cut-off current 0.05C；Stand 10 minutes；B.1C constant-current discharge is to 3.0V, stands 10 minutes；C. circulation step a and b, cycle-index is 300-400 time。Test result sees attached list 1。
High voltage 2C fills cycle performance soon to be tested room temperature 25 ± 2 DEG C, when relative humidity 45-75%, embodiment and comparative example experimental cell is carried out 3-4.35V cycle performance of battery test, and testing procedure is:
A.2C constant-current charge is to 4.35V, and then constant-voltage charge is to cut-off current 0.05C；Stand 10 minutes；
B.1C constant-current discharge is to 3.0V, stands 10 minutes；
C. circulation step a and b, cycle-index is 300-400 time。Test result sees attached list 1。
High-temperature storage performance is tested, and room temperature 25 ± 2 DEG C, when relative humidity 45-75%, embodiment and comparative example experimental cell is carried out 3-4.35V cycle performance of battery test, and testing procedure is:
A.1C constant-current charge is to 4.35V, and then constant-voltage charge tests cell thickness to cut-off current 0.05C；
Battery is transferred in 85 DEG C of calorstats by b, tests thickness after battery cools down, calculate cold Thickness Measurement by Microwave expansion rate after storing 4H。
Fill cycle performance test data soon from watch 2 high voltage, 45 ° of high voltage 2C of high temperature fill cycle performance test data and 60 DEG C of 7 days high-temperature storage data soon, adopt the capability retention after 300 circulations of embodiment battery of nonaqueous electrolytic solution of the present invention more than 80%, the thickness swelling of 85 ° of 4H high temperature stocks, below 5%, meets the actually used demand of battery；And adopt the capability retention of the comparative example battery of prior art electrolyte on the low side, and high temperature rapid charging performance and room temperature rapid charging performance can not be taken into account simultaneously。As can be seen from the results, individually adopt a kind of in positive pole film for additive, organic nitrile, fluoro carbonic ester class additive, two kinds, three kinds time, the room temperature of battery fills cycle performance, high temperature soon and fills cycle performance soon and high-temperature storage performance can not reach our instructions for use, but by being used in combination of four kinds of additives, can reach to take into account room temperature and high temperature fills while cycle performance soon, there is extraordinary high-temperature storage performance。
Table 2: embodiment and comparative example loop test result
The positive pole film for additive that uses in the electrolyte of above example of the present invention, fluoroester, organic nitrile, double; two (polyfluoroalkoxy sulphonyl) imines lithium salts, the room temperature improving battery under voltage can be worked in coordination with and high temperature fills cycle performance performance soon, high-temperature storage performance can be improved simultaneously, therefore, the electrolyte of the present invention ties up to relatively has high discharge capacity under high charge-discharge voltage, and good room temperature, high temperature fill cycle performance and high-temperature storage performance soon。
The present invention has such advantages as relative to prior art and effect:
(1) the high-voltage lithium room temperature for preparing of nonaqueous electrolytic solution of the above high-voltage lithium ion batteries of the present invention and high temperature 2C and above multiplying power is used to fill cycle performance soon better。
(2) use the high-voltage lithium high-temperature storage performance that the nonaqueous electrolytic solution of the above high-voltage lithium ion batteries of the present invention prepares better。
(3) the nonaqueous electrolytic solution cost rather moderate of the above high-voltage lithium ion batteries of the present invention is used。
Claims (8)
1. the nonaqueous electrolytic solution of a high voltage fast charging type lithium ion battery, it is characterized in that, including solvent, conventional lithium salts, positive pole film for additive, double; two (polyfluoroalkoxy sulphonyl) imines lithium salts, fluoro esters additive and organic nitrile additive, wherein
Solvent is cyclic carbonate and/or linear carbonate, and conventional lithium salts molar concentration in a solvent is 0.8-1.5mol/L。
2. nonaqueous electrolytic solution according to claim 1, it is characterised in that described cyclic carbonate is at least one in ethylene carbonate, Allyl carbonate, fluorinated ethylene carbonate and gamma-butyrolacton。
3. nonaqueous electrolytic solution according to claim 1, described linear carbonate is at least one in dimethyl carbonate, diethyl carbonate, Ethyl methyl carbonate, methyl propyl carbonate and ethyl propyl carbonic acid ester。
4. nonaqueous electrolytic solution according to claim 1, it is characterised in that described fluoro carbonic ester class additive is fluorinated ethylene carbonate and/or difluorinated ethylene carbonate。
5. nonaqueous electrolytic solution according to claim 1, it is characterized in that, described double; two (polyfluoroalkoxy sulphonyl) imines lithium salts are at least one in double; two pentafluoroethyl group sulfimide lithium, trifluoromethyl pentafluoroethyl group sulfimide lithium, bis trifluoromethyl sulfimide lithium and double; two (fluorine sulphonyl) imine lithium。
Nonaqueous electrolytic solution according to claim 1, it is characterized in that, described organic nitrile be added to succinonitrile, adiponitrile, glutaronitrile, 3,3'-oxydipropionitriles, ethylene glycol bis (propionitrile) ether, 1,2,3-tri-(2-cyanato-) propane, 1,3,5 penta trimethylsilyl nitrile, 1,2, at least one in 3 third trimethylsilyl nitriles, 1,3,6 hexane three nitrile。
6. nonaqueous electrolytic solution according to claim 1, it is characterized in that, described positive pole film for additive is at least one in vinyl ethylene carbonate, methane-disulfonic acid methylene ester, three (trimethyl silane) borate, three (trimethyl silane) phosphate esters and three (trimethyl silane) phosphate ester。
7. nonaqueous electrolytic solution according to claim 1, it is characterised in that described conventional lithium salts is LiPF6、LiBF4、LiC1O4、LiAsF6, LiBOB, LiDFOB and LiPF4C2O4In at least one。
8. nonaqueous electrolytic solution according to claim 1, it is characterised in that including conventional lithium battery electrolytes additive, the content of conventional lithium battery electrolytes additive is 0-10 weight portion；Conventional lithium battery electrolytes additive is vinylene carbonate, sulfuric acid vinyl ester, at least one in ethylene sulfite, 1,3 propane sultones, 1,3 propene sultone, 1,4 butyl sultones, 1,4-butanediol sulfuric ester and acrylic-1,3-sultones。
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