CN110336078B - Silicon-based negative electrode electrolyte and lithium ion power battery - Google Patents
Silicon-based negative electrode electrolyte and lithium ion power battery Download PDFInfo
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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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- 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
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- H—ELECTRICITY
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- 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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M2300/0017—Non-aqueous electrolytes
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Abstract
The invention discloses a silicon-based negative electrode electrolyte and a lithium ion power battery, wherein the silicon-based negative electrode electrolyte comprises: lithium salt, organic solvent containing fluorinated ether, film forming additive, degassing additive and lithium nitrate; characterized in that the film forming additive is lithium difluorophosphate and pentafluorophenyl isocyanate (PFPI). The lithium salt used in the electrolyte takes high-conductivity lithium bis (fluorosulfonyl) imide, lithium hexafluorophosphate and lithium difluorooxalato borate as main components, the three lithium salts can work under higher voltage and temperature after being mixed, the lithium difluorooxalato borate can form SEI films on a positive electrode and a negative electrode at the same time, the battery still has good electrochemical performance even under the condition of not adding other film-forming additives, and the electrolyte also has certain oxidation resistance due to the existence of fluorinated ether and adiponitrile; the presence of the degassing additive can reduce the gas production of the cell during cycling and during high temperature storage.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a silicon-based negative electrode electrolyte and a lithium ion power battery.
Background
With the gradual development of new energy automobiles, the energy density of the current power battery is difficult to meet the requirement of high endurance of the automobiles, and most power battery manufacturers gradually use silicon-based negative electrode materials with very high theoretical gram capacity in order to improve the energy density of the power battery. Although the silicon-based negative electrode has a high theoretical capacity, the silicon-based negative electrode has a large volume expansion, so that an SEI film on the surface of the negative electrode is continuously broken and formed, and thus the cycle performance of the silicon-based negative electrode is poor. Therefore, the preparation of electrolyte with good performance is very important for the battery using the silicon-based negative electrode. The main components of the currently commonly used power battery electrolyte comprise lithium salt, organic solvent and additive, wherein the lithium salt mainly comprises lithium hexafluorophosphate, the organic solvent mainly comprises carbonate solvents such as ethylene carbonate, dimethyl carbonate and ethyl methyl carbonate, and the common additive mainly comprises film forming additive, flame retardant additive, overcharge additive, high and low temperature additive and degassing additive, wherein the common additive comprises ethylene carbonate, fluoro-carbonate, biphenyl, cyclohexylbenzene, lithium difluorophosphate and ethylene sulfate.
At present, a silicon-based electrolyte lithium salt or lithium hexafluorophosphate is taken as a main solvent, a carbonate solvent and a fluoroethylene carbonate solvent are taken as main solvents, the electrolyte is easy to form an SEI film continuously in the battery circulation process, so that the battery capacity is attenuated quickly, the internal resistance of the battery is increased continuously, and the fluoroethylene carbonate is easy to perform defluorination reaction at a high temperature state to generate hydrogen fluoride and generate more gases.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a silicon-based negative electrode electrolyte and a lithium ion power battery. The invention adopts the method of adding fluorinated ether, degassing additive and lithium nitrate into the electrolyte to improve the cycle performance of the battery.
In order to achieve the purpose, the specific technical scheme of the invention is as follows:
a silicon-based negative electrode electrolyte comprising: lithium salt, organic solvent containing fluorinated ether, film forming additive, degassing additive and lithium nitrate; wherein the film forming additive is lithium difluorophosphate (LiPF)2O2) And Pentafluorophenyl Isocyanate (PFPI).
As a preferable technical scheme of the invention, the concentration of the lithium salt is 0.8-3 mol/L.
Further, the concentration of the lithium salt is 0.9-2.5 mol/L.
In a preferred embodiment of the present invention, the lithium salt is selected from lithium hexafluorophosphate (LiPF)6) One or more of lithium bis (fluorosulfonyl) imide (LiFSI) and lithium difluoro (oxalato) borate (LiODFB).
In a preferred embodiment of the present invention, the organic solvent is composed of cyclic carbonate, chain carbonate, fluoro carbonate and fluorinated ether solvent, the cyclic carbonate is one or two of Ethylene Carbonate (EC) and Propylene Carbonate (PC), and accounts for 10% to 40% of the electrolyte by mass. Preferably, the cyclic carbonate is Ethylene Carbonate (EC).
In a preferred embodiment of the present invention, the chain carbonate is one or more of Ethyl Methyl Carbonate (EMC) and dimethyl carbonate (DMC) diethyl carbonate (DEC), and accounts for 20% to 50% by mass of the electrolyte. Preferably, the chain carbonate is EMC.
In a preferable technical scheme of the invention, the fluorinated carbonate is mainly fluoroethylene carbonate (FEC) which accounts for 0-15% of the mass fraction of the electrolyte, the fluorinated ether is one or two of hydrofluoroether tetrafluoroethyl tetrafluoropropyl ether (HFE) and hexafluoroisopropyl ethyl ether (HFPE), and the cosolvent mainly used is lithium nitrate which accounts for 1-10% of the mass of the electrolyte.
As a preferable technical scheme of the invention, the content of the film forming additive accounts for 0.5-4% of the mass of the electrolyte. Preferably, lithium difluorophosphate (LiPF)2O2) And Pentafluorophenyl Isocyanate (PFPI) in a 1:1 mass ratio.
According to a preferable technical scheme of the invention, the flatulence inhibiting additive is mainly hexamethyldisilazane or adiponitrile which accounts for 1-3% of the mass of the electrolyte, wherein the adiponitrile can also be used as a high-voltage additive, and the hexamethyldisilazane can be used for removing water and acid to reduce the generation of gas in the electrolyte. The lithium nitrate (LiNO3) is used as an SEI film which has small and good stability in the surface performance of the negative electrode, and can improve the cycle stability and the coulombic efficiency of the battery.
The invention also provides a lithium ion power battery, which comprises a positive pole piece, a negative pole piece, a diaphragm and the electrolyte for the lithium ion power battery, wherein the positive pole piece comprises an aluminum foil current collector and a positive pole diaphragm, the negative pole piece comprises a copper foil current collector and a negative pole diaphragm, the positive pole diaphragm comprises a positive active substance, a conductive agent and a binder, the negative pole diaphragm comprises a negative active substance, a conductive agent and a binder, and the positive active substance is a ternary material LiNi0.6Co0.2Mn0.2O2(NCM), the negative active material is a silica/C composite (SiO/C).
By adopting the technical scheme of the invention, the invention has the following beneficial effects:
(1) the lithium salt used in the electrolyte of the invention is high-conductivity lithium bis (fluorosulfonyl) imide (LiFSI) or lithium hexafluorophosphate (LiPF)6) Lithium difluoro (oxalato) borate (LiODFB) is used as a main component, the three lithium salts can work under higher voltage and temperature after being mixed, and the lithium difluoro (oxalato) borate (LiODFB) can simultaneously form SEI films on a positive electrode and a negative electrode even under the condition that other film-forming additives are not addedThe battery still has good electrochemical performance, and the electrolyte also has certain oxidation resistance due to the existence of fluorinated ether and adiponitrile;
(2) in the electrolyte, besides a conventional carbonate solvent, fluoroethylene carbonate and fluorinated ether are also contained, film forming additives such as fluoroethylene carbonate (FEC) and pentafluorophenyl isocyanate (PFPI) can form a stable SEI film on the surface of a negative electrode material, fluorinated ether can promote the dissolution of lithium nitrate, lithium nitrate can be decomposed on the surface of a negative electrode to form a stable SEI film with small internal resistance, lithium element can be provided, and the cycle performance and the coulombic efficiency of the battery can be improved;
(3) the presence of the degassing additive can reduce the gas production of the cell during cycling and during high temperature storage.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The electrolyte for a power battery provided in this example includes a high-stability mixed lithium salt and an organic solvent containing fluorinated ether, where the lithium salt is lithium bis (fluorosulfonyl) imide (LiFSI), lithium bis (fluorooxalato) borate (LiODFB) and lithium hexafluorophosphate, the molar concentration ratio of the lithium salt to the lithium bis (fluorosulfonyl) imide to the lithium bis (fluorooxalato) borate is 6:3:1, the concentration of the lithium salt is 1.1mol/L, and the organic solvent is ethylene carbonate, ethyl methyl carbonate, fluoroethylene carbonate and hydrofluoroether tetrafluoroethyl tetrafluoropropyl ether (HFE) and is mixed in a mass ratio of 3:5:1: 1. The film forming additive is lithium difluorophosphate (LiPF)2O2) And Pentafluorophenyl Isocyanate (PFPI), the two film forming additives accounting for 2% of the electrolyte, the degassing additive being hexamethyldisilazane accounting for 2% of the electrolyte, and lithium nitrate (LiNO)3) The mass of (b) was 2.5% of the mass of the electrolyte.
Comparative example 1
The electrolyte used in this example was completely the same as the electrolyte used in example 1 except that lithium nitrate (LiNO3) was not added.
Example 2
The electrolyte for a power battery provided in this example includes a high-stability mixed lithium salt and an organic solvent containing fluorinated ether, where the lithium salt is lithium bis (fluorosulfonyl) imide (LiFSI), lithium bis (fluorooxalato) borate (LiODFB) and lithium hexafluorophosphate, the molar concentration ratio of the lithium salt to the lithium bis (fluorosulfonyl) imide to the lithium bis (fluorooxalato) borate is 6:3:1, the concentration of the lithium salt is 1.5mol/L, and the organic solvent is ethylene carbonate, ethyl methyl carbonate, fluoroethylene carbonate and hydrofluoroether tetrafluoroethyl tetrafluoropropyl ether (HFE) and is mixed in a mass ratio of 3:5:1: 1. The film forming additive is lithium difluorophosphate (LiPF)2O2) And Pentafluorophenyl Isocyanate (PFPI), the mass of each of the two film forming additives accounting for 2% of the mass of the electrolyte, the degassing additive being hexamethyldisilazane, which accounts for 2% of the mass of the electrolyte, and the mass of lithium nitrate (LiNO3) accounting for 2.5% of the mass of the electrolyte.
Comparative example 2
The electrolyte used in this example was identical to example 2 except that no film-forming additive was added.
Example 3
The electrolyte for a power battery provided in this example includes a high-stability mixed lithium salt and an organic solvent containing fluorinated ether, where the lithium salt is lithium bis (fluorosulfonyl) imide (LiFSI), lithium bis (fluorooxalato) borate (LiODFB) and lithium hexafluorophosphate, the molar concentration ratio of the lithium salt to the lithium bis (fluorosulfonyl) imide to the lithium bis (fluorooxalato) borate is 8:1:1, the lithium salt concentration is 1.1mol/L, and the organic solvent is ethylene carbonate, ethyl methyl carbonate, fluoroethylene carbonate and hydrofluoroether tetrafluoroethyl tetrafluoropropyl ether (HFE) and is mixed in a mass ratio of 4:4:1.5: 0.5. The film forming additive is lithium difluorophosphate (LiPF)2O2) And Pentafluorophenyl Isocyanate (PFPI), the two film forming additives accounting for 2% of the electrolyte, the degassing additive being hexamethyldisilazane accounting for 2% of the electrolyte, and lithium nitrate (LiNO)3) The mass of (B) is 2.5%
Comparative example 3
The electrolyte used in this example was identical to that used in example 3 except that no degassing additive was added.
Example 4
The electrolyte for a power battery provided in this example includes a high-stability mixed lithium salt and an organic solvent containing fluorinated ether, where the lithium salt is lithium bis (fluorosulfonyl) imide (LiFSI), lithium bis (fluorooxalato) borate (LiODFB) and lithium hexafluorophosphate, the molar concentration ratio of the lithium salt to the lithium bis (fluorosulfonyl) imide to the lithium bis (fluorooxalato) borate is 6:1:3, the concentration of the lithium salt is 1.1mol/L, and the organic solvent is ethylene carbonate, ethyl methyl carbonate, fluoroethylene carbonate and hydrofluoroether tetrafluoroethyl tetrafluoropropyl ether (HFE) and is mixed in a mass ratio of 3:5:1: 1. The film forming additive is lithium difluorophosphate (LiPF)2O2) And Pentafluorophenyl Isocyanate (PFPI), the two film forming additives accounting for 2% of the electrolyte, the degassing additive being hexamethyldisilazane accounting for 2% of the electrolyte, and lithium nitrate (LiNO)3) The mass of the components is 5 percent
Comparative example 4
The present example was completely the same as example 4 except that fluoroethylene carbonate was not added.
Example 5
The electrolyte for a power battery provided in this example includes a high-stability mixed lithium salt and an organic solvent containing fluorinated ether, where the lithium salt is lithium bis (fluorosulfonyl) imide (LiFSI), lithium bis (fluorooxalato) borate (LiODFB) and lithium hexafluorophosphate, the molar concentration ratio of the lithium salt to the lithium bis (fluorosulfonyl) imide to the lithium bis (fluorooxalato) borate is 6:1:3, the concentration of the lithium salt is 1.1mol/L, and the organic solvent is ethylene carbonate, ethyl methyl carbonate, fluoroethylene carbonate and hydrofluoroether tetrafluoroethyl tetrafluoropropyl ether (HFE) and is mixed in a mass ratio of 3:5:1: 1. The film forming additive is lithium difluorophosphate (LiPF)2O2) And Pentafluorophenyl Isocyanate (PFPI), the two film forming additives accounting for 2% of the electrolyte, the degassing additive being hexamethyldisilazane accounting for 2% of the electrolyte, and lithium nitrate (LiNO)3) The mass of the components is 10 percent
Comparative example 5
The degassing additive added in this example was adiponitrile, the rest being the same as in example 5.
Example 6
The electrolyte for a power battery provided in this example includes a high-stability mixed lithium salt and an organic solvent containing fluorinated ether, where the lithium salt is lithium bis (fluorosulfonyl) imide (LiFSI), lithium bis (fluorooxalato) borate (LiODFB) and lithium hexafluorophosphate, the molar concentration ratio of the lithium hexafluorophosphate, the lithium bis (fluorosulfonyl) imide and the lithium bis (fluorooxalato) borate is 8:1:1, the lithium salt concentration is 1.1mol/L, and the organic solvent is ethylene carbonate, ethyl methyl carbonate, fluoroethylene carbonate and hexafluoroisopropyl ether (HFPE) mixed in a mass ratio of 5:3:1: 1. The film forming additive is lithium difluorophosphate (LiPF)2O2) And Pentafluorophenyl Isocyanate (PFPI), the two film forming additives accounting for 2% of the electrolyte, the degassing additive being hexamethyldisilazane accounting for 2% of the electrolyte, and lithium nitrate (LiNO)3) The mass of (B) is 2.5%
Comparative example 6
This example was the same as example 6 except that no fluorinated ether was added.
Respectively adding the prepared electrolyte in the embodiments 1-6 and the middle electrolyte in the comparative examples 1-6 into the prepared soft package battery cell, wherein the rated capacity of the soft package battery cell is 10Ah, and the positive electrode active material of the battery cell is LiNi0.6Co0.2Mn0.2O2(NCM), the negative active material is a silica/carbon composite. The prepared batteries were injected with the electrolytes of examples 1 to 6 and comparative examples 1 to 6, and after formation, capacity and OCV tests, were taken to make the following tests:
1) and (3) testing the normal-temperature cycle performance: and (3) at 25 ℃, charging the battery after capacity grading to 4.2V at a constant current and a constant voltage of 1C, stopping the current to 0.05C, then discharging to 2.75V at a constant current of 1C, recording the first 1C discharge median voltage of the battery, circulating according to the cycle, and calculating the capacity retention rate after the 500 th cycle.
2) High temperature discharge at 55 ℃/1C: the cell was charged and discharged once at 25 ℃ at 1C with a cutoff current of 0.02C, and the 1C discharge capacity at 25 ℃ was recorded. And then fully charging the battery at a constant current and a constant voltage of 1C, placing the fully charged battery in a thermostat at 55 ℃ for standing for 6 hours, discharging the battery to 3.0V at 1C, and recording the 1C discharge capacity at 55 ℃.
3) -20 ℃/1C high temperature discharge: the cell was charged and discharged once at 25 ℃ at 1C with a cutoff current of 0.02C, and the 1C discharge capacity at 25 ℃ was recorded. And then fully charging the battery at constant current and constant voltage of 1C, placing the fully charged battery in a constant temperature box at the temperature of minus 20 ℃ for standing for 6 hours, discharging the battery to 3.0V at the temperature of minus 20 ℃ according to 1C, and recording the 1C discharge capacity at the temperature of minus 20 ℃.
The compositional battery tests of the electrolytes of examples 1 to 6 and comparative examples 1 to 6 gave the data shown in tables 1 and 2:
the data in the table show that the existence of the fluorinated ether and the lithium nitrate can ensure that the battery still has higher capacity retention rate after 500 cycles, the first efficiency of the battery can be improved, the influence of the content of the lithium nitrate on the battery is small, and the discharge capacity of the battery at high temperature and low temperature meets the requirement.
TABLE 1
TABLE 2
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the light of the present specification, or directly/indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (7)
1. A silicon-based negative electrode electrolyte comprising: lithium salt, organic solvent containing fluorinated ether, film forming additive, degassing additive and lithium nitrate; characterized in that the film forming additive is lithium difluorophosphate LiPF2O2And pentafluoroPhenyl isocyanate PFPI;
the lithium salt is selected from lithium hexafluorophosphate LiPF6One or more of lithium bis (fluorosulfonyl) imide LiFSI and lithium difluoro (oxalato) borate LiODFB;
the organic solvent consists of cyclic carbonate, chain carbonate, fluoro carbonate and fluorinated ether solvent, wherein the cyclic carbonate is one or two of ethylene carbonate EC and propylene carbonate PC, and accounts for 10-40% of the electrolyte by mass; the chain-like carbonate is one or more of Ethyl Methyl Carbonate (EMC) and dimethyl carbonate (DMC), diethyl carbonate (DEC), and accounts for 20-50% of the electrolyte by mass;
the fluorinated ether is one or two of hydrofluoroether tetrafluoroethyl tetrafluoropropyl ether HFE and hexafluoroisopropyl ether HFPE, and accounts for 1% -10% of the mass of the electrolyte.
2. The silicon-based negative electrode electrolyte of claim 1, wherein the lithium salt concentration is 0.8-3 mol/L.
3. The silicon-based negative electrode electrolyte of claim 2, wherein the lithium salt concentration is 0.9-2.5 mol/L.
4. The silicon-based negative electrode electrolyte according to claim 1, wherein the fluorinated carbonate is fluoroethylene carbonate FEC, and accounts for 0-15% of the mass fraction of the electrolyte.
5. The silicon-based negative electrode electrolyte as claimed in claim 1, wherein the film-forming additive is present in an amount of 0.5-4% by mass of the electrolyte.
6. The silicon-based negative electrode electrolyte of claim 1, wherein the degassing additive is hexamethyldisilazane or adiponitrile, which accounts for 1-3% of the electrolyte mass.
7. A lithium ion power battery comprises a positive electrodeThe silicon-based negative electrode electrolyte comprises a pole piece, a negative pole piece, a diaphragm and the silicon-based negative electrode electrolyte as claimed in any one of claims 1 to 6, wherein the positive pole piece comprises an aluminum foil current collector and a positive pole diaphragm, the negative pole piece comprises a copper foil current collector and a negative pole diaphragm, the positive pole diaphragm comprises a positive active material, a conductive agent and a binder, the negative pole diaphragm comprises a negative active material, a conductive agent and a binder, and the positive active material is a ternary material LiNi0.6Co0.2Mn0.2O2(NCM), the negative active material is a silica/C composite (SiO/C).
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| EP3076471A1 (en) * | 2014-09-26 | 2016-10-05 | LG Chem, Ltd. | Nonaqueous electrolyte and lithium secondary battery comprising same |
| CN106252716A (en) * | 2016-10-17 | 2016-12-21 | 东莞市凯欣电池材料有限公司 | A kind of safe lithium ion power battery electrolyte and lithium-ion-power cell |
| CN107681197A (en) * | 2017-09-08 | 2018-02-09 | 西安科技大学 | A kind of lithium-sulfur cell electrolyte |
| CN109873205A (en) * | 2019-02-27 | 2019-06-11 | 杉杉新材料（衢州）有限公司 | A kind of electrolyte suitable for silicon-carbon cathode and the lithium ion battery comprising the electrolyte |
| CN109755636A (en) * | 2019-03-15 | 2019-05-14 | 杉杉新材料（衢州）有限公司 | A kind of high temperature and pressure secure lithium ion battery electrolyte and lithium ion battery |
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