CN112635831A - Non-aqueous electrolyte and lithium ion battery - Google Patents
Non-aqueous electrolyte and lithium ion battery Download PDFInfo
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- CN112635831A CN112635831A CN202011528453.3A CN202011528453A CN112635831A CN 112635831 A CN112635831 A CN 112635831A CN 202011528453 A CN202011528453 A CN 202011528453A CN 112635831 A CN112635831 A CN 112635831A
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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Abstract
The invention relates to a non-aqueous electrolyte and a lithium ion battery, wherein the non-aqueous electrolyte comprises electrolyte lithium salt, a non-aqueous solvent, a first additive and a second additive, the first additive comprises one or more compounds shown in formulas (i) - (iii), and the second additive comprises lithium difluorophosphate bis (LiODFP), wherein the formulas (i) - (iii) are respectively as follows:wherein R is1、R2And R3Each independently selected from hydrogen and C1‑C5Saturated hydrocarbon group, C1‑C5Unsaturated hydrocarbon group, C1‑C5Alkoxy, halogen or C6‑C18An aromatic group.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a non-aqueous electrolyte and a lithium ion battery.
Background
The electrolyte is one of four key materials of the lithium ion battery, is called as blood of the lithium ion battery, has the function of conducting electrons between an anode and a cathode in the battery, and is also an important guarantee for the lithium ion battery to obtain the advantages of high voltage, high specific energy and the like. The electrolyte for lithium ion batteries should generally meet the following basic requirements: 1. high ionic conductivity, typically up to 1X 10-3~2×10-2S/cm; 2. high thermal and chemical stability, no separation over a wide voltage range; 3. the electrochemical window is wide, and the stability of the electrochemical performance is kept in a wide voltage range; 4. the electrolyte has good compatibility with other parts of the battery, such as electrode materials, electrode current collectors, separators and the like; 5. safe, nontoxic and pollution-free.
At present, people carry out a series of researches on high-temperature resistant electrolyte, in order to improve high-temperature performance, additives such as vinylene carbonate, ethylene carbonate and the like are generally used, but the additives cause higher battery impedance, and the balance of other electrochemical performances such as capacity, internal resistance and the like is difficult to be considered. In order to improve the low-temperature performance of the battery, generally, carboxylic acid esters having a low melting point, such as ethyl acetate and ethyl propionate, are selected as the main solvent of the electrolyte, but these solvents have a relatively low boiling point and are disadvantageous to the high-temperature performance of the battery. Therefore, it is necessary to develop an electrolyte that has both high and low temperature performance.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a non-aqueous electrolyte and a lithium ion battery, wherein the non-aqueous electrolyte has the stability during high-temperature and low-temperature (-30-60 ℃) storage, and the prepared lithium ion battery has good cyclicity at-30-60 ℃.
The first object of the present invention is to provide a nonaqueous electrolytic solution which is resistant to a temperature of-30 ℃ to 60 ℃ and comprises an electrolytic lithium salt, a nonaqueous solvent, a first additive and a second additive,
the first additive comprises one or more compounds represented by formulas (i) - (iii),
the second additive comprises lithium difluorophosphate bis (oxalato) phosphate (LiODFP),
wherein the structural formulas (i) to (iii) are respectively as follows:
wherein R is1、R2And R3Each independently selected from hydrogen and C1-C5Saturated hydrocarbon group, C1-C5Unsaturated hydrocarbon group, C1-C5Alkoxy, halogen or C6-C18An aromatic group.
Further, C1-C5The saturated hydrocarbon group is selected from methyl, ethyl, n-propyl or n-butyl.
Further, C1-C5The unsaturated hydrocarbon group is selected from vinyl or allyl.
Further, halogen is fluorine, chlorine or bromine.
Further, C6-C18The aryl is phenyl.
Preferably, in formulae (i) and (ii), R1、R2And R3At least one of (a) is vinyl; in the formula (iii), R1And R2At least one of (a) is a vinyl group.
Further, the mass ratio of the first additive to the second additive is 0.1-5: 0.1-5.
Further, the mass ratio of the electrolyte lithium salt, the non-aqueous solvent, the first additive and the second additive is 10-20:60-90:0.1-5: 0.1-5.
Further, the electrolyte lithium salt is selected from one or more of lithium hexafluorophosphate, lithium bis-fluorosulfonyl imide, lithium tetrafluoroborate and lithium perchlorate.
Further, the non-aqueous solvent is selected from a fluorinated non-cyclic carboxylic acid ester and/or a fluorinated non-cyclic carbonate.
Further, the fluorinated acyclic carboxylic acid ester is selected from trifluoromethyl-containingAcyclic carboxylic acid esters, trifluoromethyl-containing acyclic carboxylic acid esters including H-COO-CH2CF3、CH3-COO-CH2CF3、CH3CH2-COO-CH2CF3And CH3CH2CH2-COO-CH2CF3One or more of them.
Further, the fluorinated acyclic carbonate is selected from the group consisting of trifluoromethyl group-containing acyclic carbonates, and the trifluoromethyl group-containing acyclic carbonates are selected from the group consisting of CH3-OCOO-CH2CF3And/or CF3CH2-OCOOCH2CH3。
A second object of the present invention is to provide a lithium ion battery comprising a positive electrode containing a positive electrode active material, a negative electrode containing a negative electrode active material, a separator disposed between the positive electrode and the negative electrode, and an electrolyte; the electrolyte solution includes the nonaqueous electrolyte solution of the present invention.
Further, the positive active substance is selected from one or more of lithium cobaltate, lithium nickelate, lithium manganate, lithium vanadate, lithium iron phosphate, lithium iron manganese phosphate, lithium nickel manganese oxide, lithium cobalt manganese oxide, lithium-rich manganese-based material and ternary positive material, and the structural formula of the ternary positive material is LiNi1-x-y-zCoxMnyAlzO2Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, and x + y + z is more than or equal to 0 and less than or equal to 1.
Further, the negative active material is selected from one or more of artificial graphite, natural graphite, silicon-oxygen compound, silicon-based alloy and active carbon.
Further, in the lithium ion battery, the type of the isolation film is not particularly limited, and may be selected according to actual requirements. Preferably, the diaphragm comprises a base film and a nano alumina coating coated on the base film, wherein the base film is at least one of PP, PE and PET, and the thickness of the nano alumina coating is 1.0-6.0 μm.
By the scheme, the invention at least has the following advantages:
the non-aqueous electrolyte disclosed by the invention controls the stability of the electrolyte when the electrolyte is stored at low temperature and high temperature (-30-60 ℃) through the combination of the first additive and the second additive, inhibits high-temperature gas generation, and the prepared lithium ion battery has good cyclicity at-30-60 ℃.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a preferred embodiment of the present invention and is described in detail below.
Drawings
Fig. 1 is a high temperature cycle life test result of the batteries prepared in the respective examples;
fig. 2 is a result of a high-temperature storage capacity retention and recovery test of batteries prepared according to the examples;
fig. 3 is a low-temperature discharge test result of the batteries prepared in the respective examples.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the following examples of the present invention, a method of manufacturing a lithium ion secondary battery is as follows:
LiNi as positive electrode active material0.5Co0.2Mn0.3O2(LNCM), conductive agent carbon nano tube (50-80 μm), adhesive polyvinylidene fluoride (PVDF) according to the mass ratio of 8: 1, fully stirring and mixing evenly in N-methyl pyrrolidone solvent system, coating on aluminum foil, drying, cold pressing, obtaining the positive pole piece, wherein the compaction density is 3.5g/cm3。
Fully stirring and uniformly mixing a negative active material graphite, a conductive agent Keqin black, a binder PVDF and a thickening agent sodium carboxymethyl cellulose (CMC) in a deionized water solvent system according to a mass ratio of 8: 1, coating the mixture on a copper foil, drying and cold pressing to obtain a negative pole piece, wherein the compaction density of the negative pole piece is 1.5g/cm3。
Polyethylene (PE) with the thickness of 9 mu m is taken as a base film, and a nano aluminum oxide coating layer with the thickness of 3 mu m is coated on the base film to obtain the diaphragm.
And stacking the positive pole piece, the diaphragm and the negative pole piece in sequence, so that the diaphragm is positioned between the positive pole piece and the negative pole piece to play an isolating role, and stacking the pieces to obtain the bare cell.
And (2) filling the bare cell into an aluminum plastic film, baking at 80 ℃ to remove water, injecting corresponding electrolyte, sealing, standing, hot-cold pressing, forming, clamping, capacity grading and other procedures to obtain the finished product of the flexibly-packaged lithium ion secondary battery.
In the following examples of the invention, the compounds a-r and their structural formulae are as follows:
example 1
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.2 part of compound a and 0.5 part of LiODFPP.
Example 2
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.2 part of compound b and 0.5 part of LiODFPP.
Example 3
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.2 part of compound c and 0.5 part of LiODFPP.
Example 4
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, compound d 0.2 parts and LiODFPP 0.5 parts.
Example 5
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, compound e 0.2 part and LiODFP0.5 part.
Example 6
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, compound f 0.2 parts and LiODFP0.5 parts.
Example 7
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, compound g 0.2 parts and LiODFPP 0.5 parts.
Example 8
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts of compound h 0.2 part of LiODFPP 0.5 part of the compound.
Example 9
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.2 part of compound i and 0.5 part of LiODFPP.
Example 10
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, compound j 0.2 part and LiODFP0.5 part.
Example 11
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.2 part of compound k and 0.5 part of LiODFPP.
Example 12
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.2 part of compound l and 0.5 part of LiODFPP.
Example 13
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.2 part of compound m and 0.5 part of LiODFPP.
Example 14
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.2 part of compound n and 0.5 part of LiODFPP.
Example 15
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.2 part of compound o and 0.5 part of LiODFPP.
Example 16
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, compound p 0.2 parts and LiODFPP 0.5 parts.
Example 17
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, compound q 0.2 parts and LiODFPP 0.5 parts.
Example 18
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.2 part of compound r and 0.5 part of LiODFPP.
Example 19
A nonaqueous electrolyte consists of the following components in parts by weight:
20 parts of lithium hexafluorophosphate and CH3-COO-CH2CF350 portions of CH3-OCOO-CH2CF330 parts of compound h 0.2 part of LiODFPP 0.5 part of the compound.
Example 20
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 15 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF345 parts, 0.1 part of compound h and 1 parts of LiODFP
Example 21
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-OCOO-CH2CF345 parts of compound h 05 parts and LiODFP2 parts.
Example 22
Lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 0.5 part of compound h and 0.5 part of LiODFP.
Example 23 lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts of compound h 0.5 part and 1 parts of LiODFP.
Example 24 a nonaqueous electrolytic solution, consisting of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts of compound h 0.2 part and 1 parts of LiODFP.
Example 25 a nonaqueous electrolytic solution, consisting of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts of compound h 0.2 part and 2 parts of LiODFP.
Comparative example 1
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 10 parts of a compound h and 2 parts of LiODFP.
Comparative example 2
A nonaqueous electrolyte consists of the following components in parts by weight:
lithium hexafluorophosphate 10 parts, CH3-COO-CH2CF330 portions of CH3-OCOO-CH2CF330 parts, 10 parts of a compound h and 10 parts of LiODFP.
The nonaqueous electrolyte is assembled into a battery, and the performance of the battery is tested by the following test method:
(1) high temperature cycle life test
The full-charged battery after capacity grading was placed in a 45 ℃ incubator and discharged to 3.0V at 1C, and the initial discharge capacity was recorded as DC (1). Charging to 4.2V at constant current and constant voltage of 1C, stopping current at 0.05C, standing for 5min, discharging to 3.0V at 1C, and recording discharge capacity DC (2). This is cycled through until dc (n) < 80%. And recording the discharge times N, wherein N is the high-temperature cycle life. The results of measurements of the batteries prepared in the respective examples are shown in table 1 below and fig. 1.
(2) High temperature storage capacity retention and recovery test
The full-state battery after capacity separation was discharged to 3.0V at room temperature at 1C, and the initial discharge capacity was recorded as DC (0). The cell was placed in an incubator at 60 ℃ for N days, the cell was taken out and discharged to 3.0V at room temperature, and the discharge capacity DC (N-1) was recorded, and the storage capacity Retention was 100% DC (N-1)/DC (0). Charging to 4.2V at constant current and constant voltage of 1C, stopping current at 0.05C, standing for 5min, and discharging to 3.0V at 1C. The average discharge capacity DC (N-2) was recorded after 3 cycles, and the storage capacity Recovery was 100% DC (N-2)/DC (0). The results of measurement of the batteries prepared in the respective examples are shown in table 1 below and fig. 2. In FIG. 2, a pair of results from left to right correspond to the results of examples 1 to 25 in order.
(3) Low temperature discharge test
The full-state battery after capacity separation was discharged to 3.0V at 25 ℃ at 1C, and the initial discharge capacity was recorded as DC (25 ℃). Then, the mixture was charged to 4.2V at 25 ℃ at a constant current and a constant voltage of 1C, and the current was cut off at 0.05C. The temperature is reduced to minus 20 ℃ and the mixture is kept for 4 hours, then the mixture is discharged to 3.0V at 1C, and the discharge capacity DC (-20 ℃) is recorded. The low-temperature discharge capacity retention rate was 100% DC (-20 ℃)/DC (25 ℃). The results of measurement of the batteries prepared in the respective examples are shown in table 1 below and fig. 3.
TABLE 1 results of Performance testing of batteries assembled with different nonaqueous electrolytes
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A nonaqueous electrolytic solution comprising an electrolytic lithium salt, a nonaqueous solvent, a first additive and a second additive,
the first additive comprises one or more compounds shown in formulas (i) to (iii),
the second additive comprises lithium bis (oxalato) difluorophosphate,
wherein the structural formulas (i) to (iii) are respectively as follows:
wherein R is1、R2And R3Each independently selected from hydrogen and C1-C5Saturated hydrocarbon group, C1-C5Unsaturated hydrocarbon group, C1-C5Alkoxy, halogen or C6-C18An aromatic group.
2. The nonaqueous electrolytic solution of claim 1, wherein: said C is1-C5The saturated hydrocarbon group is selected from methyl, ethyl, n-propyl or n-butyl.
3. The nonaqueous electrolytic solution of claim 1, wherein: said C is1-C5The unsaturated hydrocarbon group is selected from vinyl or allyl.
4. The nonaqueous electrolytic solution of claim 1, wherein: the mass ratio of the first additive to the second additive is 0.1-5: 0.1-5.
5. The nonaqueous electrolytic solution of claim 1, wherein: the electrolyte lithium salt is selected from one or more of lithium hexafluorophosphate, lithium bis-fluorosulfonyl imide, lithium tetrafluoroborate and lithium perchlorate.
6. The nonaqueous electrolytic solution of claim 1, wherein: the non-aqueous solvent is selected from a fluorinated non-cyclic carboxylic acid ester and/or a fluorinated non-cyclic carbonate.
7. The nonaqueous electrolytic solution of claim 6, wherein: the fluorinated acyclic carboxylic acid ester is selected from the group consisting of trifluoromethyl group-containing acyclic carboxylic acid esters including H-COO-CH2CF3、CH3-COO-CH2CF3、CH3CH2-COO-CH2CF3And CH3CH2CH2-COO-CH2CF3One or more of them.
8. The nonaqueous electrolytic solution of claim 6, wherein: the fluorinated acyclic carbonate is selected from an acyclic carbonate containing a trifluoromethyl group, and the acyclic carbonate containing a trifluoromethyl group is selected from CH3-OC(O)O-CH2CF3And/or CF3CH2-OCOOCH2CH3。
9. A lithium ion battery, characterized by: the battery comprises a positive electrode containing a positive electrode active material, a negative electrode containing a negative electrode active material, a diaphragm arranged between the positive electrode and the negative electrode and an electrolyte; the electrolyte includes the nonaqueous electrolyte solution described in any one of claims 1 to 9.
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Application publication date: 20210409 |