CN113839089B - Lithium ion battery electrolyte and lithium ion battery containing same - Google Patents
Lithium ion battery electrolyte and lithium ion battery containing same 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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a lithium ion battery electrolyte and a lithium ion battery containing the same, and relates to the technical field of lithium ion batteries. The lithium ion battery electrolyte comprises a non-aqueous organic solvent, an electrolyte lithium salt and an additive. The additive comprises a phosphate derivative additive with a structure shown in a formula I, and a stable solid electrolyte interface film (SEI) can be formed on the surface of a positive electrode material and a negative electrode material by adding the phosphate derivative additive, so that the dissolution of transition metal elements in a high-nickel system at high temperature is reduced, and the cycle and high-temperature shelf performance of the battery are improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a lithium ion battery electrolyte and a lithium ion battery containing the same.
Background
Since the advent of lithium ion batteries, lithium ion batteries have been widely used in mobile devices, electric vehicles, notebook computers, and other mobile portable devices, with advantages of high energy storage, long cycle life, and environmental friendliness.
With the rapid development of new energy automobiles and mobile portable fields, people put higher requirements on the safety performance and energy density of lithium ion batteries, and the main coping way for solving the requirements is to improve the voltage of the lithium ion batteries at present, but the lithium ion batteries face the problems of gas expansion, transition metal ion dissolution, rapid decay of cycle performance and the like under high pressure, even high temperature and high pressure, so that the wider application of the lithium ion batteries is severely limited.
In order to solve the above problems, phosphate additives such as tris (trimethylsilyl) phosphate, perfluoroalkylethyl phosphate, and the like are often selected for the electrolyte of lithium ion batteries. The phosphorus-oxygen double bond in the phosphate additive has lone pair electrons, is Lewis base and can react on the surface of the anode material to form a protective film, so that the dissolution of transition metal ions of the lithium ion battery at high temperature and high pressure is reduced, the oxidative decomposition of an organic solvent in the electrolyte and the damage to the anode material structure are effectively inhibited, the high-temperature cycle and shelf performance of the lithium ion battery are improved, the electrochemical window of the electrolyte is widened, the working voltage of the battery is improved, and the stability of the high-voltage cycle of the battery is improved. However, the addition of the phosphate additive can obviously increase the internal resistance of the battery, reduce the first irreversible capacity of the battery, be not beneficial to improving the cycle efficiency of the battery, and be not ideal for storing the battery at high temperature and high pressure. On the other hand, acid anhydrides such as 4-methylphthalic anhydride, succinic anhydride, glutaric anhydride, and 4, 5-difluorophthalic anhydride are also often added. Acid anhydride can consume trace moisture and hydrofluoric acid in the pole piece or the electrolyte, and the dissolution of inorganic components in the protective film by strong acid is reduced; under high potential, the anhydride additive can also form a stable protective film on the surface of the positive electrode material, so that the generation of gas in the circulation process is reduced, but the circulation performance of the battery under high-temperature conditions is not obviously improved by the anhydride.
Disclosure of Invention
The invention aims to provide a battery electrolyte, which can effectively reduce the problem of gas expansion of a lithium ion battery and improve the battery cycle performance and high-temperature shelving performance of the lithium ion battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a lithium ion battery electrolyte, which comprises a nonaqueous organic solvent, a lithium salt and an additive, wherein the additive comprises one or more of phosphate derivatives with a structure shown in a formula I:
wherein R is 1 、R 2 、R 3 、R 4 And R 5 Each independently selected from any one of linear or non-linear alkyl, fluoroalkyl, alkenyl, cyano, fluorine atom and hydrogen atom with less than 4 carbon atoms, and R 4 And R 5 At least one of which is a fluoroalkyl group.
Preferably, in the phosphate ester derivative with the structure of formula I, R 1 、R 2 And R 3 At least one of which is H.
Preferably, in the phosphate ester derivative with the structure of formula I, R 4 And R 5 At least one of which is perfluoroalkyl.
In the invention, the structure of the formula I is obtained by esterification reaction of a formula II and a formula III in a solvent containing inorganic strong base under the action of a catalyst;
the structures of the formulas II and III are as follows:
wherein, the catalyst is selected from one of 2-dimethylamino pyridine or 4-dimethylamino pyridine, the strong inorganic alkali is alkali metal hydroxide, and the solvent is water.
Further preferably, the phosphate derivative is one or more of compounds (a) to (C) shown in the following structures:
preferably, the mass fraction of the phosphate ester derivative with the structure of formula I is 0.5-3% based on 100% of the total mass of the battery electrolyte.
More preferably, the mass fraction of the phosphate ester derivative with the structure of the formula I is 0.5-2%.
Preferably, the additive further comprises other additives.
Further preferably, the other additive is one or more selected from the group consisting of lithium dioxalate borate (LiBOB), lithium difluorooxalate borate, lithium tetrafluorooxalate phosphate, 1, 3-Propane Sultone (PS), ethylene sulfate, ethylene carbonate, propylene sulfite, 1, 4-butane sultone, tris (trimethylsilane) phosphate (TMSP), tris (trimethylsilane) phosphite (TMSPI), fluoroethylene carbonate, vinylene Carbonate (VC), fluoroethylene carbonate (FEC), and lithium difluorophosphate.
More preferably, the mass fraction of the other additives is 0.2 to 8%, more preferably 0.5 to 6%, and still more preferably 1 to 5%, based on 100% by mass of the total mass of the battery electrolyte.
Preferably, the total mass fraction of the additives is 0.5 to 10%, more preferably 0.5 to 8%, and still more preferably 0.5 to 5.6%.
Preferably, the lithium salt is LiPF 6 、LiBF 4 、LiClO 4 、LiBOB、LiDFOB、LiCF 3 SO 3 One or more of LiBETI, liTFSI and LiFSI.
Further preferably, the lithium salt is LiPF 6 。
Preferably, the mass fraction of the lithium salt is 9-15%.
More preferably, the mass fraction of the lithium salt is 10 to 12.5%.
Preferably, the non-aqueous organic solvent is at least one of ethylene carbonate, propylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, ethyl methyl carbonate, propyl ethyl carbonate, 1, 4-butyrolactone, methyl formate, ethyl acetate, methyl propionate, ethyl propionate, butyl propionate and ethyl butyrate.
Further preferably, the non-aqueous organic solvent is a mixed solvent of ethylene carbonate, dimethyl carbonate and ethyl methyl carbonate.
More preferably, the mass ratio of the ethylene carbonate, the dimethyl carbonate and the methyl ethyl carbonate is 1.
The invention also provides a lithium ion battery containing the lithium ion battery electrolyte.
In the invention, the lithium ion battery also comprises a cathode, an anode and a diaphragm.
Preferably, the cathode comprises a cathode material and an aluminum foil supporting the cathode material.
Preferably, the anode comprises an anode material and a copper foil loaded with the anode material.
Further, the cathode material comprises an active material, a binder and a conductive agent.
Still more preferably, the cathode active material is LiNi 1-x-y-z Co x Mn y Al z O 2 Wherein: 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.
The anode active substance is artificial graphite, natural graphite or SiO w And a silicon-carbon composite material compounded with graphite.
Preferably, the anode active material substance is artificial graphite.
In the invention, the lithium ion battery also comprises an aluminum plastic film packaged outside the cathode, the anode and the diaphragm.
The upper limit cut-off voltage of the lithium ion battery is greater than or equal to 4.35V.
The added phosphate derivative additive can be prior to a solvent in the electrolyte to form a compact solid electrolyte interface film (SEI film) on the surfaces of a positive electrode and a negative electrode, so that the dissolution of transition metal ions in a positive electrode material at high temperature is reduced, the continuous decomposition of the electrolyte on the surfaces of the positive electrode and the negative electrode is prevented, the swelling of the battery at high temperature and high pressure is reduced, the circulation stability of the battery is improved, and the voltage window of the electrolyte is widened; the acid anhydride in the derivative can consume trace moisture and hydrofluoric acid in the electrolyte, so that the corrosion of strong acid to a solid film formed on the surface of the anode and the cathode is weakened, and the stability of an interface film is strengthened; meanwhile, the addition of other additives can be cooperated with the phosphate derivatives, so that the high-temperature performance of the battery is further improved.
Compared with the prior art, the invention has the following beneficial effects:
the phosphate ester derivative is used as a novel electrolyte additive, compared with the conventional additive, the phosphate ester derivative is less in use amount, and the problem of battery flatulence can be obviously inhibited. The acid anhydride can neutralize residual alkali of the anode material and can also react with moisture in an anode sheet or electrolyte to generate organic acid substances, so that the formation of strong acid is reduced, and the dissolution of the acid to the material is reduced; in addition, the acid anhydride additive can form a stable protective film on the surface of the positive electrode material at a high potential. The phosphate compound can be matched with hydrofluoric acid to consume the hydrofluoric acid and block continuous generation of subsequent side reactions, so that the phosphate compound has better water and acid removing functions. The additive contains phosphate and anhydride groups at the same time, so that a synergistic effect can be achieved, and the performance of the battery is optimized. The electrolyte additive can be well compatible with anode and cathode materials, can participate in forming a stable anode and cathode interface film, and obviously improves the high-temperature cycle performance of the battery.
The phosphate ester acid anhydride derivatives are used as novel electrolyte additives, and compared with other conventional additives, the swelling problem of the lithium ion battery can be obviously improved, and the high-temperature cycle performance and high-temperature shelf performance of the battery are improved.
Detailed Description
The present invention will be further described with reference to the following examples. However, the present invention is not limited to the following examples. The implementation conditions adopted in the embodiments may be further adjusted according to different requirements of specific applications, and the implementation conditions not noted are conventional conditions in the industry. The technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Comparative example 1
Preparing an electrolyte: in a glove box filled with argon (water, oxygen content are less than 0.1 ppm), ethylene Carbonate (EC), dimethyl carbonate (DEC), ethyl Methyl Carbonate (EMC) were mixed at a mass ratio of 3 6 After being stirred evenlyThe lithium ion battery electrolyte of comparative example 1 was obtained.
Comparative examples 2 to 6 and examples 1 to 11
Comparative examples 2 to 6 and examples 1 to 11 were the same as in example 1 except that the electrolyte additive component composition ratios were added as shown in Table 1.
Table 1 the electrolyte of comparative examples 1 to 8 and examples 1 to 11 had the following composition ratios:
preparing a lithium ion battery:
LiNi as positive electrode active material 0.5 Co 0.2 Mn 0.3 O 2 And the acetylene black and polyvinylidene fluoride (PVDF) are fully stirred and uniformly mixed in an N-methyl pyrrolidone solvent system according to the mass ratio of 95.
Preparing negative active material artificial graphite, conductive agent acetylene black, binder Styrene Butadiene Rubber (SBR), and thickener carboxymethyl cellulose sodium (CMC) according to a mass ratio of 96:2:1:1, fully stirring and uniformly mixing in a deionized water solvent system, coating on a copper foil, drying, and cold pressing to obtain the negative plate.
Polyethylene (PE) is used as a base film, and a nano aluminum oxide coating is coated on the base film to be used as a diaphragm.
And sequentially laminating the positive plate, the isolating membrane and the negative plate, winding the positive plate, the isolating membrane and the negative plate along the same direction to obtain a bare cell, placing the bare cell in an outer package, respectively injecting the electrolytes of comparative examples 1-8 and examples 1-12 into the prepared battery, and performing the processes of packaging, shelving, high-temperature clamp formation, secondary packaging, capacity grading and the like to obtain the ternary high-nickel positive material soft package lithium ion battery (NCM 523/AG) with the voltage of 4.35V.
The following performance tests were performed on the lithium ion batteries described above, respectively, and the test results are shown in table 2.
And (3) testing the normal-temperature cycle performance of the ternary high-nickel battery: and (3) charging the battery after capacity grading to 4.35V at a constant current and a constant voltage of 1C at 25 ℃, stopping current to 0.05C, then discharging to 2.75V at a constant current of 1C, and circulating according to the cycle, and calculating the cyclic capacity retention rate of 500 weeks after charging and discharging for 500 weeks. Wherein the calculation formula is as follows:
cycle capacity retention rate at week N (%) = (cycle discharge capacity at week N/cycle discharge capacity at week N) × 100%.
And (3) testing 45 ℃ cycle performance of the ternary high-nickel battery: and (3) charging the battery with the capacity divided to 4.35V at a constant current and a constant voltage of 1C and stopping the current at 0.05C at 45 ℃, then discharging the battery to 2.75V at a constant current of 1C, and calculating the capacity retention rate of the 300 th cycle after the battery is cycled, charged/discharged for 300 cycles. The calculation formula is as follows:
cycle capacity retention (%) at N-th week (= (cycle discharge capacity at N-th week/cycle discharge capacity at first week) × 100%
And (3) testing the thickness change, the capacity residual rate and the capacity recovery rate of the ternary high-voltage battery at a constant temperature of 60 ℃: firstly, charging and discharging the battery for 1 time by the normal-temperature cycle performance testing method, recording the discharge capacity C0 of the battery before the battery is placed, then charging the battery to a full 4.35V state under constant current and constant voltage, testing the thickness T1 of the battery before the battery is placed at high temperature by using a thickness gauge, then placing the battery in a constant-temperature oven at 60 ℃ for 7 days, taking out the battery, immediately testing the thickness T2 of the battery after the battery is placed at high temperature, and calculating the thickness change of the battery after the battery is placed at 60 ℃ for 7 days; after the battery is cooled at room temperature, performing constant current discharge to 2.75V at the normal temperature by using 1C, recording the discharge capacity C1 of the battery after the battery is placed, and calculating the capacity residual rate of the battery after the battery is placed at the constant temperature of 60 ℃ for 7 days; and then carrying out constant current charging and discharging on the battery for one week (2.75-4.35V) at the normal temperature by using 1C, recording the discharge capacity C2 of the battery, and calculating the capacity recovery rate after the battery is placed for 7 days at the constant temperature of 60 ℃, wherein the calculation formula is as follows:
the rate of change in cell thickness after 7 days of standing at 60 = (T2-T1)/T1 × 100%;
capacity remaining = C1/C0 100% after 7 days of constant temperature resting at 60 ℃.
Capacity recovery = C2/C0 x 100% after 7 days of constant temperature resting at 60 ℃.
And (4) disassembling and centrifuging the placed battery, and testing to obtain the concentration of metal ions in the electrolyte.
Table 2 results of testing cycle performance and high-temperature storage performance of the batteries of examples and comparative examples
As can be seen from the comparison of the results of the cell performance test of comparative example 1 and examples 1-3 in Table 2: the phosphate derivative additive can obviously improve the cycle performance and high-temperature shelving performance of the battery, and obviously reduce the concentration of metal ions in the electrolyte, so that the additive can form a layer of uniform and compact solid film on the surfaces of a positive electrode and a negative electrode, particularly on the surface of the positive electrode, so that the dissolution of a transition metal element at high temperature is inhibited, the continuous oxidation of an organic solvent in the electrolyte on the surface of an electrode material is prevented, the generation of gas in the high-temperature shelving process is reduced, and the safety performance of the battery is improved; the comparison of the examples 1 to 3 shows that the introduction of the fluorohydrocarbon in the phosphate derivative additive can obviously improve the film formation of the battery, particularly the film formation process of the negative electrode, play a certain role in inhibiting the generation of gas in the laying process, and improve the cycle performance of the battery.
The results of the battery performance tests in examples 3-5 show that the addition of the phosphate derivative additive requires a proper amount, and when the addition amount is too small, the solid films formed on the surfaces of the positive electrode and the negative electrode by the phosphate derivative additive are not stable enough, so that the corrosion of HF and the like generated in the circulation process to the solid films cannot be well prevented; excessive addition increases the internal resistance of the battery, and the electrochemical performance of the battery is deteriorated; the addition of low-impedance additives such as LiBOB in the additives containing the phosphate derivatives is more beneficial to the continuation of circulation.
Compared with the results of battery performance tests of examples 1-5, the phosphate derivative additive provided by the invention has more obvious effect no matter at normal temperature or high temperature compared with the effect produced by simply mixing phosphate and anhydride compounds, and the result of the reduction of the concentration of metal ions in the electrolyte shows that the phosphate derivative has higher molecular weight, so that an interface film formed by redox reaction of the phosphate derivative on the positive electrode is more compact, the metal ions in the positive electrode material are more difficult to dissolve out, and collapse of the positive electrode active material structure in the circulating process is reduced; meanwhile, the more compact interface film can also reduce the contact between the anode and the electrolyte, reduce the consumption of the electrolyte and ensure the normal circulation process.
As can be seen from comparison of battery performance test results of comparative examples 1-5 and examples 6-11, when the phosphate derivative additive is combined with other additives such as VC, FEC and other conventional negative electrode film-forming additives, an SEI film can be better formed on the surface of a negative electrode material, the reduction reaction of a solvent on a negative electrode interface is inhibited, the interface impedance can be reduced, and the cycle performance and the high-temperature shelf performance of the lithium ion battery are effectively improved.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included within the scope of the present invention.
Claims (14)
1. A lithium ion battery electrolyte comprises a non-aqueous organic solvent, a lithium salt and an additive, and is characterized in that: the additive comprises one or more phosphate derivatives with the structure of formula I:
wherein R is 1 、R 2 、R 3 、R 4 And R 5 Each independently selected from any one of linear or non-linear alkyl, fluoroalkyl, alkenyl, cyano, fluorine atom and hydrogen atom with less than 4 carbon atoms, and R 4 And R 5 At least one of which is a fluoroalkyl group.
2. The lithium ion battery electrolyte of claim 1, wherein: r is 1 、R 2 And R 3 Is H.
3. The lithium ion battery electrolyte of claim 1, wherein: r is 4 And R 5 At least one of which is perfluoroalkyl.
4. The lithium ion battery electrolyte of claim 1, wherein: the phosphate derivative with the structure of the formula I is obtained by carrying out esterification reaction on a substance shown in the formula II and a substance shown in the formula III in a solvent containing inorganic strong base under the action of a catalyst; the structures of the formulas II and III are as follows:
wherein, the catalyst is selected from 2-dimethylaminopyridine or 4-dimethylaminopyridine, the inorganic strong base is alkali metal hydroxide, and the solvent is water.
5. The lithium ion battery electrolyte of any one of claims 1-3 wherein the phosphate derivative having the structure of formula I is one or more of the following:
6. the lithium ion battery electrolyte of claim 1, wherein: the mass fraction of the phosphate ester derivative with the structure shown in the formula I is 0.5-3% based on 100% of the total mass of the battery electrolyte.
7. The lithium ion battery electrolyte of claim 1 or 6, wherein: the additive also comprises other additives, and the other additives are one or more selected from lithium dioxalate borate, lithium difluorooxalate borate, lithium tetrafluorooxalate phosphate, 1, 3-propane sultone, ethylene sulfate, ethylene carbonate, propylene sulfite, 1, 4-butane sultone, tris (trimethylsilane) phosphate, tris (trimethylsilane) phosphite, fluoroethylene carbonate, vinylene carbonate, fluoroethylene carbonate and lithium difluorophosphate.
8. The lithium ion battery electrolyte of claim 7, wherein: the mass fraction of the other additives is 0.2-8% based on 100% of the total mass of the battery electrolyte.
9. The lithium ion battery electrolyte of claim 1, wherein: the mass fraction of the lithium salt is 9-15% based on 100% of the total mass of the battery electrolyte; the lithium salt is LiPF 6 、LiBF 4 、LiClO 4 One or more of LiBOB, liDFOB, liTFSI and LiFSI.
10. The lithium ion battery electrolyte of claim 1, wherein: the non-aqueous organic solvent is at least one of ethylene carbonate, propylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, ethyl propyl carbonate, 1, 4-butyrolactone, methyl formate, ethyl acetate, methyl propionate, ethyl propionate, butyl propionate and ethyl butyrate.
11. A lithium ion battery, characterized by: the electrolyte comprises the lithium ion battery electrolyte as defined in any one of claims 1 to 10.
12. The lithium ion battery of claim 11, wherein: the lithium ion battery also comprises a cathode, an anode and a diaphragm, wherein the cathode comprises a cathode material and an aluminum foil loaded with the cathode material; the anode comprises an anode material and a copper foil loaded with the anode material.
13. The lithium ion battery of claim 12, wherein: the cathode material comprises a cathode active material, a binder and a conductive agent; the anode material comprises an anode active material, a binder and a conductive agent; the cathode active material is LiNi 1-x-y-z Co x Mn y Al z O 2 Wherein: 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; the anode active material is artificial graphite, natural graphite or SiO w And the silicon-carbon composite material is compounded with graphite.
14. The lithium ion battery of any one of claims 11 to 13, wherein: the upper limit cut-off voltage of the lithium ion battery is greater than or equal to 4.35V.
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| CN111092256A (en) * | 2019-11-29 | 2020-05-01 | 天津力神电池股份有限公司 | High-temperature-resistant lithium ion battery |
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