CN104600359A - Nonaqueous electrolytic solution of high-voltage lithium ion battery - Google Patents
Nonaqueous electrolytic solution of high-voltage lithium ion battery Download PDFInfo
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- CN104600359A CN104600359A CN201410520398.1A CN201410520398A CN104600359A CN 104600359 A CN104600359 A CN 104600359A CN 201410520398 A CN201410520398 A CN 201410520398A CN 104600359 A CN104600359 A CN 104600359A
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- carbonate
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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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- 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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Abstract
The invention discloses a nonaqueous electrolytic solution of a high-voltage lithium ion battery. The nonaqueous electrolytic solution comprises, by weight, 100 parts of a solvent which is cyclic carbonate and/or chain carbonate, 0.2-10 parts of a sulfonate additive, 0.2-10 parts of a fluorocarbonate additive, 0.2-10 parts of an organic ether nitrile additive, 0-5 parts of a common lithium battery electrolyte additive, and a lithium salt, wherein a mole concentration of the lithium salt in the solvent is in a range of 0.8-1.5mol/L. Through combination of the sulfonate additive, the fluorocarbonate additive and the organic ether nitrile additive, the nonaqueous electrolytic solution improves SEI film oxidization resistance in electrolyte primary-formation and obviously improves normal temperature and low temperature cycle performances of the high-voltage electrolyte.
Description
[technical field]
The present invention relates to the electrolyte of lithium ion battery, particularly relate to a kind of nonaqueous electrolytic solution of high-voltage lithium ion batteries.
[background technology]
The anode material for lithium-ion batteries of current use, as LiCoO
2, LiMn
2o
4, LiCoNiMnO
2, LiFePO
4low etc. operating voltage at below 4V, gram volume is 90-150mg/g.The way promoting battery energy density mainly contains 2 kinds, a kind of is the charge cutoff voltage improving traditional 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 be limited by promoting the way of charge cutoff voltage, further lifting can cause cobalt acid lithium excessively de-lithium time structure poor stability.
But along with the raising of operating voltage and charge cutoff voltage, the oxidation activity of positive electrode improves, the reaction of positive active material and electrolyte is also accelerated thereupon, inflatable is serious under high voltages to cause battery, and 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 lithium ion batteries of a kind of charge-discharge performance.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is, a nonaqueous electrolytic solution for high-voltage lithium ion batteries, is made up of solvent, lithium salts, sulfonic acid esters additive, fluoroester class additive, organic ether nitrile additive and lithium battery electrolytes additive; Wherein,
Solvent is cyclic carbonate and/or linear carbonate, and lithium salts molar concentration is in a solvent 0.8-1.5mol/L.
The nonaqueous electrolytic solution of above-described high-voltage lithium ion batteries, described cyclic carbonate is at least one in ethylene carbonate, propene carbonate and fluorinated ethylene carbonate or gamma-butyrolacton.
The nonaqueous electrolytic solution of above-described high-voltage lithium ion batteries, described linear carbonate is at least one in dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, methyl propyl carbonate and ethyl propyl carbonic acid ester.
1. the nonaqueous electrolytic solution of above-described high-voltage lithium ion batteries, at least one in described fluoroester class additive to be described fluoro carbonic ester class additive be fluorinated ethylene carbonate and difluorinated ethylene carbonate.
The nonaqueous electrolytic solution of above-described high-voltage lithium ion batteries, described sulfonic acid esters is added to 1, at least one in 3 propane sultones, Isosorbide-5-Nitrae butyl sultone, methane-disulfonic acid methylene ester, BDO sulfuric ester, propenyl-1,3-sulfonic acid lactone.
2. the nonaqueous electrolytic solution of above-described high-voltage lithium ion batteries, described ether nitrile is added to 3,3'-oxydipropionitrile (CAS:1656-48-0), ethylene glycol bis (propionitrile) ether (CAS:3386-87-6), 1, at least one in 2,3-tri-(2-cyanato-) propane (2465-93-2).
3. the nonaqueous electrolytic solution of above-described high-voltage lithium ion batteries, described lithium salts is LiPF
6, LiBF
4, LiC
1o
4, LiAsF
6, LiCF
3sO
2, LiN (CF
3sO
2)
2, LiBOB, LiDFOB, LiPF
4c
2o
4or LiN (C
2f
5sO
2)
2in at least one.
4. the nonaqueous electrolytic solution of above-described high-voltage lithium ion batteries, conventional lithium battery electrolytes additive comprises vinylene carbonate (VC), vinyl ethylene carbonate (VEC), sulfuric acid vinyl ester (DTD), at least one in ethylene sulfite (ES).
The present invention, by the conbined usage of sulfonic acid esters additive, fluoro carbonic ester class additive and organic ether nitrile additive, can improving the oxidative resistance of the SEI film of electrolyte when changing into for the first time, obviously improving high-voltage electrolyte normal temperature and high/low temperature cycle performance.
[embodiment]
The nonaqueous electrolytic solution of high-voltage lithium ion batteries of the present invention, is formed and commonly uses lithium battery electrolytes additive formed by solvent, lithium salts, sulfonic acid esters additive, fluoro carbonic ester class additive, ether nitrile additive.Wherein, solvent 100 weight portion; Sulfonic acid esters additive 0.2-10 weight portion; Fluoro carbonic ester class additive 0.2-10 weight portion; Organic ether 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 lithium salts molar concentration is in a solvent 0.8-1.5mol/L.
Sulfonic acid esters additive is mainly used in changing into and forming stable SEI film in negative terminal surface in cyclic process, to ensure that battery has excellent cycle performance, containing sulphur compound in its SEI film formed, form SEI and there is better thermal stability, therefore show good high-temperature storage performance and high temperature cyclic performance.
Fluoro carbonic ester class additive is by the sucting electronic effect of F element, also help and improve the reduction potential of solvent molecule 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, significantly can improve the cycle performance of high-voltage battery.
Although organic ether nitriles substance can suppress the decomposition of electrolyte, suppress flatulence, and can catch the metal ion of stripping, after positive pole film forming, positive pole impedance becomes large, and cycle performance decreases.Therefore, the addition of adiponitrile (ADN) is chosen as 0.2 ~ 10 weight portion, although FEC can improve cycle performance, FEC at high temperature can produce HF, the decomposition of HF to electrolyte solvent has catalytic action, thus adds 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, although sulfonic acid esters can form fine and close SEI film in negative terminal surface, suppress high temperature flatulence, improve the high-temperature storage performance under high voltage, and the stripping of PC can be inhibit, improve the cycle performance under high voltage, but when adding too much, the SEI film of negative pole is thicker, has influence on high rate performance with regard to cryogenic property, therefore, the addition of sulfonic acid esters is chosen as 0.2 ~ 10 weight portion.We find when above three uses jointly, can be there is certain between them mutually act synergistically, the product formed forms excellent compound both positive and negative polarity SEI film in initial charge process, makes it work under high voltages and has good thermal stability and cycle performance.
Ether nitriles substance can absorb a small amount of water and HF, forms amide substance, reduces the catalysis due to HF and POF3 etc., make electrolyte solvent decompose the high temperature flatulence caused; Nitriles substance can form stabilising membrane at positive electrode surface in first charge-discharge process, effectively suppresses positive pole oxidation electrolyte, thus suppresses high temperature flatulence.Ether nitrile additive can form clad type chelate with lithium ion because ehter bond exists, lithium salts solubility in organic solvent can be improved, improve the conductivity of electrolyte, simultaneously the electro-chemical activity of ether nitrile is also high than traditional succinonitrile, adiponitrile, therefore has better high-temperature behavior and cycle performance.
The conbined usage of above three kinds of additives significantly can improve the stability of the both positive and negative polarity SEI film of electrolyte under high voltage condition, effectively suppresses solvent oxidation to be decomposed, thus improves the cycle performance of electrolyte under high voltage condition.
Lithium salts is LiPF
6, LiBF
4, LiC
1o
4, LiAsF
6, LiCF
3sO
2, LiN (CF
3sO
2)
2, LiBOB, LiDFOB, LiPF
4c
2o
4or LiN (C
2f
5sO
2)
2in one or more mix arbitrarily, concentration is 0.8 ~ 1.5mol/L.
Cyclic carbonate is preferably at least one in ethylene carbonate (EC), propene carbonate (PC), fluorinated ethylene carbonate (FEC) and gamma-butyrolacton (GBL);
Linear carbonate is preferably at least one in dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), methyl propyl carbonate (MPC) and ethyl propyl carbonic acid ester (EPC).
The nonaqueous electrolytic solution of above high-voltage lithium ion batteries, at least one in fluoroester class additive to be fluoro carbonic ester class additive be fluorinated ethylene carbonate and difluorinated ethylene carbonate.
The nonaqueous electrolytic solution of above high-voltage lithium ion batteries, sulfonic acid esters is added to 1,3 propane sultones (CAS:1120-71-4), 1,4 butyl sultones (CAS:1633-83-6), methane-disulfonic acid methylene ester (CAS:99591-74-9), 1, at least one in 4-butanediol sulfuric ester, propenyl-1,3-sulfonic acid lactone (CAS:21806-61-1).
The nonaqueous electrolytic solution of above high-voltage lithium ion batteries, ether nitrile is added to 3,3'-oxydipropionitrile (CAS:1656-48-0), ethylene glycol bis (propionitrile) ether (CAS:3386-87-6), 1, at least one in 2,3-tri-(2-cyanato-) propane (CAS:2465-93-2).
Except above high voltage additive, can also add lithium battery electrolytes typical additives is vinylene carbonate, vinyl ethylene carbonate vinegar, sulfuric acid vinyl ester (DTD), at least one in ethylene sulfite (ES).
Embodiment 1
In BRAUN glove box, prepare electrolyte, be full of the nitrogen that purity is 99.999% in glove box, in glove box, moisture controls at≤5ppm, and temperature is in room temperature.By 30 grams of EC, 70 grams of EMC, mix, and sealing, puts into refrigerator after it is cooled to 8 DEG C, be transferred in glove box, then add LiPF in two batches
6abundant mixing, form the nonaqueous electrolytic solution that lithium salts molar concentration is the lithium ion battery of 1mol/L, the FEC of solvent gross mass 3% is added in above nonaqueous electrolytic solution, 3% propane sultone, ethylene glycol bis (propionitrile) ether of 2%, after Homogeneous phase mixing, obtain high-voltage lithium ion nonaqueous electrolytic solution.
The compound method of other embodiments and comparative example is carried out with reference to the compound method of embodiment 1 below.
Wherein, FEC (CAS:114435-02-8), 3, 3'-oxydipropionitrile (CAS:1656-48-0), ethylene glycol bis (propionitrile) ether (CAS:3386-87-6), 1, 2, 3-tri-(2-cyanato-) propane (CAS:2465-93-2), 1, 3 propane sultones (CAS:1120-71-4), 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., 1, 4-butanediol sulfuric ester is purchased from Fujian Chuangxin Science and Technology Development Co., Ltd..
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: the anode pole piece preparing lithium ion battery: by mass percent be 3% Kynoar (PVDF) be dissolved in 1-methyl-9-pyrrolidone solution, the cobalt of mass percent 96% acid lithium (LiCoO2), mass percent 3% conductive agent carbon black are added above-mentioned solution and mix, after the slurry of mixed system being coated on the two sides of the plus plate current-collecting body that aluminium foil is formed, dry compacting as anode pole piece, the compacted density of positive pole is 4.05g/cm
3.
The preparation of cathode pole piece: be the binding agent of 4%SBR (polystyrene, butadiene suspension) by mass percent, mass percent is in the water-soluble solution of thickener of 1%CMC (sodium carboxymethylcellulose), be that 95% graphite adds above-mentioned solution by mass percent, mix, after the slurry of mixed system being coated on the two sides of the negative current collector that Copper Foil is formed, dry compacting as cathode pole piece.
Dry battery core is with high pressure cobalt acid lithium for positive pole, and take graphite as negative pole, microporous polyethylene film is that square dry battery core made by barrier film.Dry battery core is moved into glove box 80-85 DEG C of oven for drying after 48 hours stand-by.Respectively the various embodiments described above and comparative example gained electrolyte are injected the good dry battery core of above-mentioned oven dry, then leave standstill 24 hours, preliminary filling once changes into, and sealing, after secondary changes into, obtains embodiment and comparative example experimental cell.
The test of high voltage cycle performance is room temperature 25 ± 2 DEG C, under the condition of relative humidity 45-75%, the test of 3-4.35V cycle performance of battery is carried out to embodiment and comparative example experimental cell, testing procedure is: a.1C constant current charge is to 4.35V, and then constant voltage charge is to cut-off current 0.05C; Leave standstill 10 minutes; B.1C constant-current discharge is to 3.0V, leaves standstill 10 minutes; C. circulation step a and b, cycle-index is 300-400 time.Test result sees attached list 3.
High-temperature storage performance is tested, room temperature 25 ± 2 DEG C, carry out the test of 3-4.35V cycle performance of battery to embodiment and comparative example experimental cell under the condition of relative humidity 45-75%, testing procedure is: a.1C constant current charge is to 4.35V, and then constant voltage charge is to cut-off current 0.05C test battery thickness; Battery is transferred in 60 DEG C of insulating boxs by b, stores the rear thickness of test battery cooling after 7 days, calculates cold Thickness Measurement by Microwave expansion rate.
From table 3 high voltage cycle performance test data and 60 DEG C of 7 days high-temperature storage data, the capability retention after embodiment battery 300 circulations of nonaqueous electrolytic solution of the present invention is adopted to be greater than 80%, 60 ° of thickness swellings of 30 days, below 3%, meet the actual user demand of battery; And adopt the capability retention of the comparative example battery of prior art electrolyte on the low side, and high-temperature behavior and cycle performance can not be taken into account simultaneously.60 DEG C of storage datas can find out that except the storage adding PS in contrast sample is slightly good (but circulation extreme difference) other expansion rate is all far away higher than the thickness swelling of embodiment.As can be seen from the results, time a kind of in independent employing sulfonic acid esters, organic ether nitrile, fluoro carbonic ester class additive, the cycle performance of battery and high-temperature storage performance can not reach our instructions for use, but by the conbined usage of three kinds of additives, the same with our result of predictive analysis, can reach while taking into account cycle performance, there is extraordinary high-temperature storage performance.
Table 3: embodiment and comparative example loop test result
The additive sulfonic acid esters additive, fluoroester, the organic ether nitrile that use in the electrolyte of the above embodiment of the present invention, the normal temperature and high temperature cyclic performance performance that improve battery under voltage can be worked in coordination with, therefore, electrolyte of the present invention ties up to comparatively has high discharge capacity, good normal-temperature circulating performance and high-temperature storage performance under high charge-discharge voltage.
The present invention has following advantage and effect relative to prior art:
(1) the high-voltage lithium normal temperature charge-discharge performance using the nonaqueous electrolytic solution of the above high-voltage lithium ion batteries of the present invention to prepare and high-temperature storage performance.
(2) use the nonaqueous electrolytic solution of the above high-voltage lithium ion batteries of the present invention compared with solvent being used the high-voltage electrolyte of fluorinated solvents, there is larger cost advantage.
Claims (8)
1. a nonaqueous electrolytic solution for high-voltage lithium ion batteries, is characterized in that, is made up of solvent, lithium salts, sulfonic acid esters additive, fluoro carbonic ester class additive, organic ether nitrile additive and lithium battery electrolytes additive; Wherein,
Solvent is cyclic carbonate and/or linear carbonate, and lithium salts molar concentration is in a solvent 0.8-1.5mol/L.
2. the nonaqueous electrolytic solution of high-voltage lithium ion batteries according to claim 1, is characterized in that, described cyclic carbonate is at least one in ethylene carbonate, propene carbonate and fluorinated ethylene carbonate or gamma-butyrolacton.
3. the nonaqueous electrolytic solution of high-voltage lithium ion batteries according to claim 1, is characterized in that, described linear carbonate is at least one in dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, methyl propyl carbonate and ethyl propyl carbonic acid ester.
4. the nonaqueous electrolytic solution of high-voltage lithium ion batteries according to claim 1, is characterized in that, described fluoro carbonic ester class additive is at least one in fluorinated ethylene carbonate and difluorinated ethylene carbonate.
5. the nonaqueous electrolytic solution of high-voltage lithium ion batteries according to claim 1, it is characterized in that, described sulfonic acid esters additive is 1,3 propane sultones, 1,4 butyl sultones, methane-disulfonic acid methylene ester, 1, at least one in 4-butanediol sulfuric ester, propenyl-1,3-sulfonic acid lactone.
6. the nonaqueous electrolytic solution of high-voltage lithium ion batteries according to claim 1, it is characterized in that, described organic ether nitrile additive is 3,3'-oxydipropionitrile, ethylene glycol bis (propionitrile) ether, 1, at least one in 2,3-tri-(2-cyanato-) propane.
7. the nonaqueous electrolytic solution of high-voltage lithium ion batteries according to claim 1, is characterized in that, described lithium salts is LiPF
6, LiBF
4, LiC
1o
4, LiAsF
6, LiCF
3sO
2, LiN (CF
3sO
2)
2, LiBOB, LiDFOB, LiPF
4c
2o
4or LiN (C
2f
5sO
2)
2in at least one.
8. the nonaqueous electrolytic solution of high-voltage lithium ion batteries according to claim 1, is characterized in that, lithium battery electrolytes additive comprises vinylene carbonate, vinyl ethylene carbonate vinegar, sulfuric acid vinyl ester, at least one in ethylene sulfite.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104979589A (en) * | 2015-07-23 | 2015-10-14 | 东莞市凯欣电池材料有限公司 | High-voltage electrolyte and lithium ion battery using electrolyte |
| CN107221702A (en) * | 2017-04-28 | 2017-09-29 | 山东海容电源材料股份有限公司 | A kind of 4.45V high-voltage lithiums electrolyte |
| CN108666620A (en) * | 2018-04-09 | 2018-10-16 | 珠海市赛纬电子材料股份有限公司 | A kind of nonaqueous electrolytic solution of high-voltage lithium ion batteries |
| CN108878977A (en) * | 2018-06-29 | 2018-11-23 | 桑顿新能源科技有限公司 | Inhibit the chemical conversion of lithium battery high temperature to produce gas and improves the electrolyte and preparation method of cryogenic property |
| WO2020119808A1 (en) * | 2018-12-14 | 2020-06-18 | 宁德时代新能源科技股份有限公司 | Electrolyte, battery and device |
| CN112186260A (en) * | 2020-09-28 | 2021-01-05 | 苏州酷卡环保科技有限公司 | Formation method of lithium ion battery |
| CN112201853A (en) * | 2020-11-11 | 2021-01-08 | 江苏卫健信息科技有限公司 | Preparation method of power lithium ion battery |
| CN112768767A (en) * | 2020-12-30 | 2021-05-07 | 广东国光电子有限公司 | Electrolyte and lithium secondary battery using same |
| CN113451653A (en) * | 2021-08-17 | 2021-09-28 | 珠海冠宇电池股份有限公司 | Non-aqueous electrolyte and lithium ion battery comprising same |
-
2014
- 2014-09-30 CN CN201410520398.1A patent/CN104600359A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104979589A (en) * | 2015-07-23 | 2015-10-14 | 东莞市凯欣电池材料有限公司 | High-voltage electrolyte and lithium ion battery using electrolyte |
| CN107221702A (en) * | 2017-04-28 | 2017-09-29 | 山东海容电源材料股份有限公司 | A kind of 4.45V high-voltage lithiums electrolyte |
| CN108666620A (en) * | 2018-04-09 | 2018-10-16 | 珠海市赛纬电子材料股份有限公司 | A kind of nonaqueous electrolytic solution of high-voltage lithium ion batteries |
| CN108878977A (en) * | 2018-06-29 | 2018-11-23 | 桑顿新能源科技有限公司 | Inhibit the chemical conversion of lithium battery high temperature to produce gas and improves the electrolyte and preparation method of cryogenic property |
| WO2020119808A1 (en) * | 2018-12-14 | 2020-06-18 | 宁德时代新能源科技股份有限公司 | Electrolyte, battery and device |
| CN112186260A (en) * | 2020-09-28 | 2021-01-05 | 苏州酷卡环保科技有限公司 | Formation method of lithium ion battery |
| CN112201853A (en) * | 2020-11-11 | 2021-01-08 | 江苏卫健信息科技有限公司 | Preparation method of power lithium ion battery |
| CN112768767A (en) * | 2020-12-30 | 2021-05-07 | 广东国光电子有限公司 | Electrolyte and lithium secondary battery using same |
| CN113451653A (en) * | 2021-08-17 | 2021-09-28 | 珠海冠宇电池股份有限公司 | Non-aqueous electrolyte and lithium ion battery comprising same |
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