CN111129590A - High-voltage lithium ion battery non-aqueous electrolyte and high-voltage lithium ion battery - Google Patents
High-voltage lithium ion battery non-aqueous electrolyte and high-voltage lithium ion 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
- H01M10/056—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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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- 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
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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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Abstract
The invention discloses a high-voltage lithium ion battery non-aqueous electrolyte, which comprises electrolyte lithium salt, a non-aqueous organic solvent and an additive, wherein the additive comprises the following components in percentage by mass in the high-voltage lithium ion battery non-aqueous electrolyte: 0.5 to 1.0% of a sulfur compound, 0.5 to 3.0% of a positive electrode protective additive, and 0.1 to 8.0% of a negative electrode film forming additive. The invention also discloses a high-voltage lithium ion battery. The high-voltage lithium ion battery non-aqueous electrolyte can effectively inhibit the dissolution of metal ions, reduce the decomposition and gas production of the electrolyte, improve the cycle performance of the battery under high voltage, reduce the impedance of the battery and improve the low-temperature performance of the lithium ion battery.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a high-voltage lithium ion battery non-aqueous electrolyte and a high-voltage lithium ion battery.
Background
Lithium ion batteries are widely used in digital 3C products such as mobile phones, cameras, notebook computers and the like due to their advantages of light weight, small size, high energy density, long cycle life, large output power, small environmental pollution and the like. However, with the development of scientific technology, people have higher energy density requirements on lithium ion batteries, and increasing the working voltage of lithium ion batteries is one of effective means for increasing the energy density.
However, as the voltage of the lithium ion battery increases, the oxidative decomposition reaction of the electrolyte is accelerated, a large amount of gas is generated, and the internal pressure of the battery increases, thereby causing the performance degradation of the battery. Particularly, during long-term high-temperature storage or high-temperature cycles, the elution of positive electrode metal ions is more serious, resulting in rapid degradation of the performance of the battery.
In order to suppress the degradation of battery performance due to the elution of the positive electrode metal ions and the decomposition of the electrolyte, a positive and negative electrode film-forming additive may be added to the electrolyte. Film-forming additives added in the field of lithium ion batteries are mainly 1, 3-propane sultone (1,3-PS), Vinylene Carbonate (VC) and the like, but the film formed by the additives at high temperature and high pressure is not firm and is easy to break.
For example, chinese patent publication No. CN107359368A discloses a lithium battery electrolyte based on a sulfate additive, which includes a solvent a, a lithium salt B, and a sulfate additive C. The invention utilizes sulfate ester additive C to participate in the formation of SEI on the surface of the lithium metal cathode, and modifies/modifies the SEI film on the surface of the electrode, wherein the sulfate ester additive C comprises compounds such as vinyl sulfate, methyl ethylene sulfite, propylene sulfate and the like, has lower lowest unoccupied molecular orbital energy, is easy to obtain electrons, is easier to reduce, and the decomposition product of the sulfate ester additive C is rich in Li2S and Li2And O, introducing an inorganic component on the surface of the lithium negative electrode, and improving the mechanical strength of the SEI by regulating and controlling the SEI component, so that the stability of the SEI is enhanced, the growth of lithium dendrites is inhibited, and the service life and the cycle performance of the lithium metal battery are improved. The disadvantages are that the above-mentioned additivesThe film formed by the agent under high temperature and high pressure is not firm and is easily broken.
Disclosure of Invention
In order to overcome the defects of the background art, the invention provides a high-voltage lithium ion battery non-aqueous electrolyte and a high-voltage lithium ion battery. The electrolyte additive has good anode film-forming property, can effectively solve the problem of dissolving out of anode metal ions, and improves the normal-temperature cycle performance, high-temperature cycle performance and high-temperature storage performance of a high-voltage lithium ion battery.
In order to achieve the purpose, the invention adopts the technical scheme that: the non-aqueous electrolyte of the high-voltage lithium ion battery comprises electrolyte lithium salt, a non-aqueous organic solvent and an additive, wherein the additive comprises the following components in percentage by mass in the non-aqueous electrolyte of the high-voltage lithium ion battery:
0.5 to 1.0% of a sulfur-based compound
0.5-3.0% of positive electrode protection additive
0.1-8.0% of negative electrode film forming additive
As a preferred embodiment of the present invention, the sulfur-based compound has a structural formula shown below:
wherein R1 and R2 are independently selected from alkyl, alkenyl, alkynyl and fluorine-containing alkyl.
More preferably, the sulfur-based compound is one or more of the compounds represented by the following structural formula:
as a preferred embodiment of the present invention, the positive electrode protection additive is one or more of Adiponitrile (AN), Succinonitrile (SN), Hexanetricarbonitrile (HTCN).
As a preferred embodiment of the present invention, the negative electrode film forming additive is selected from one or more of Vinylene Carbonate (VC), fluoroethylene carbonate (FEC), vinylethylene carbonate (VEC), 1, 3-Propanesultone (PS), 1, 3-propanesultone (1,3-PST), vinyl sulfite (ES), tris (trimethylsilane) phosphate (TMSP), tris (trimethylsilane) borate (TMSB), and methanedisulfonic acid methylene ester (MMDS).
The negative film-forming additive is preferably one or more of fluoroethylene carbonate, 1, 3-propane sultone and vinylene carbonate.
In a preferred embodiment of the present invention, the electrolyte lithium salt is at least two of lithium hexafluorophosphate, lithium bis-fluorosulfonylimide, lithium tetrafluoroborate and lithium difluorophosphate.
In a preferred embodiment of the present invention, the electrolyte lithium salt is contained in the non-aqueous electrolyte of the high-voltage lithium ion battery in an amount of 12 to 16.0% by mass.
As a preferred embodiment of the present invention, the non-aqueous organic solvent includes cyclic carbonate selected from one or more of ethylene carbonate and propylene carbonate, chain carbonate selected from one or more of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, and carboxylic ester; the carboxylic ester is selected from one or more of propyl propionate, ethyl propionate and butyl propionate.
The non-aqueous organic solvent is more preferably a mixture of ethylene carbonate, propylene carbonate, diethyl carbonate, ethyl propionate, propyl propionate.
The invention also provides a high-voltage lithium ion battery which comprises a cathode pole piece, an anode pole piece, an isolating membrane arranged between the cathode pole piece and the anode pole piece and the non-aqueous electrolyte of the high-voltage lithium ion battery.
Further, the cathode plate comprises an aluminum foil current collector and a cathode membrane, and the anode plate comprises a copper foil current collector and an anode membrane.
Preferably, the cathode membrane includes a cathode active material, a conductive agent, and a binder, and the anode membrane includes an anode active material, a conductive agent, and a binder.
More preferably, the anode active material of the high voltage lithium ion battery is lithium cobaltate, and the cathode active material is artificial graphite.
Preferably, the upper cut-off voltage of the high voltage lithium ion battery is greater than or equal to 4.45V or 4.5V.
Compared with the prior art, the invention has the following advantages:
1. the sulfur compound in the non-aqueous electrolyte of the high-voltage lithium ion battery can well modify an SEI film of a positive electrode, and effectively inhibit the occurrence of side reactions on the surface of the electrode and the dissolution of metal ions;
2. the complex type positive electrode protection additive in the non-aqueous electrolyte of the high-voltage lithium ion battery, such as Adiponitrile (AN), Succinonitrile (SN), Hexanetrinitrile (HTCN) and other nitriles, has high bond energy of carbon-nitrogen triple bonds in cyano groups, is not easy to oxidize, can have good stability on a positive electrode, and has strong oxidation resistance; meanwhile, the cyano group has stronger coordination capacity and can be combined with active sites (such as some high-valence metal ions, such as nickel/cobalt/manganese and the like) on the surface of the electrode to mask the active ions on the surface of the positive electrode, so that the decomposition effect of the electrode on the electrolyte is reduced.
3. The non-aqueous electrolyte of the high-voltage lithium ion battery is also added with a novel conductive lithium salt difluorophosphate with low impedance characteristic, and compared with the single use of LiPF6The invention combines and uses various novel film-forming lithium salts, and is beneficial to improving the high-low temperature performance, the rate capability and the long cycle performance of the power battery.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
The structural formulas of the sulfur-based compounds in the examples and comparative examples of the present invention are characterized as follows:
compound 1 structural formula:
compound 2 structural formula:
compound 3 structural formula:
example 1
Preparing electrolyte: preparation of electrolyte in argon-filled glove box (H)2O＜0.1ppm，O2< 0.1ppm), mixing Ethylene Carbonate (EC), Propylene Carbonate (PC), diethyl carbonate (DEC), Ethyl Propionate (EP) and Propyl Propionate (PP) in a mass ratio of EC/PC/DEC/EP/PP of 3:1:4:1:1 to obtain a mixed solution, and slowly adding lithium hexafluorophosphate (LiPF) to the mixed solution6) And lithium difluorophosphate (LiPO)2F2) The lithium ion battery electrolyte of example 1 is obtained by adding the lithium salt mixture, then adding the sulfur compound 1, finally adding the negative film-forming additives fluoroethylene carbonate (FEC), 1, 3-Propane Sultone (PS) and the positive protective additive Succinonitrile (SN) and stirring uniformly. Wherein the mass percent of lithium hexafluorophosphate in the electrolyte is 14%, the mass percent of lithium difluorophosphate in the electrolyte is 1.0%, the mass percent of the compound 1 in the electrolyte is 0.5%, the mass percent of 1, 3-Propane Sultone (PS) in the electrolyte is 3.0%, the mass percent of fluoroethylene carbonate (FEC) in the electrolyte is 5.0%, and the mass percent of Succinonitrile (SN) in the electrolyte is 2.0%. The electrolyte formulation is shown in table 1.
Examples 2 to 8
Examples 2-8 are also specific examples of electrolyte preparation, and the parameters and preparation method are the same as example 1 except for the parameters in Table 1. The electrolyte formulation is shown in table 1.
Comparative examples 1 to 11
In comparative examples 1 to 11, the parameters and preparation method were the same as in example 1 except for the parameters shown in Table 1. The electrolyte formulation is shown in table 1.
TABLE 1 composition ratios of the components of the electrolytes of examples 1-8 and comparative examples 1-11
Note: the concentration of each component in the sulfur compound and the lithium salt is the mass percentage content in the electrolyte;
the content of the positive electrode protection additive is the mass percentage content in the electrolyte;
the content of each component in the negative electrode film forming additive is the mass percentage content in the electrolyte;
the proportion of each component in the solvent is mass ratio.
Lithium ion battery performance testing
Preparing a lithium ion battery:
and determining the coating surface density according to the size of the battery, the capacity design and the capacities of the anode and cathode materials. The positive active material is lithium cobaltate; the negative electrode active material is artificial graphite.
The steps of preparing the positive electrode, preparing the negative electrode, preparing the diaphragm and preparing the battery are as follows:
(1) the preparation method of the anode comprises the following steps: weighing an active substance (lithium cobaltate), polyvinylidene fluoride (PVDF) and conductive carbon black (Super-P) according to a mass ratio of 96:1:3, adding the mixture into an N-methylpyrrolidone (NMP) solvent, mixing, stirring to obtain slurry, filtering the slurry, uniformly coating the slurry on two sides of an aluminum foil by using a coating machine, drying, cold flat pressing and splitting to obtain the positive plate.
(2) The preparation steps of the negative electrode are as follows: mixing artificial graphite, conductive carbon black, Styrene Butadiene Rubber (SBR) as a binder and carboxymethyl cellulose (CMC) as a thickener according to a mass ratio of 93:1.3:1.7:1, dispersing the mixture in deionized water, uniformly mixing to obtain negative electrode slurry, filtering the negative electrode slurry, uniformly coating the negative electrode slurry on two sides of a copper foil by using a coating machine, drying, carrying out cold flat pressing, and dividing the copper foil into strips to obtain the negative electrode sheet.
(3) The preparation steps of the diaphragm are as follows: the diaphragm adopts a PP/PE/PP three-layer double-check diaphragm.
(4) Preparing a lithium ion battery: stacking the prepared positive plate, the diaphragm and the negative plate in sequence to enable the diaphragm to be positioned between the positive plate and the negative plate, and preparing a naked electric core in a winding mode; placing the bare cell in an aluminum-plastic film outer package, injecting the electrolyte prepared in each embodiment and comparative example into the fully dried lithium ion battery, standing the battery at 45 ℃, forming the battery by a high-temperature clamp, sealing the battery for the second time, and performing conventional capacity grading to obtain the lithium ion battery. Electrical performance tests were performed and the results are shown in table 2, wherein:
(1) and (3) testing the normal-temperature cycle performance of the battery: and (3) charging the battery with the capacity divided to 4.45V at a constant current and a constant voltage of 1C and stopping the current at 0.05C at 25 ℃, then discharging the battery to 3.0V at a constant current of 1C, and calculating the capacity retention rate of the battery in the 300 th cycle after the battery is cycled for 300 times. The calculation formula is as follows:
the 300 th cycle capacity retention (%) was (300 th cycle discharge capacity/first cycle discharge capacity) × 100%;
(2) and (3) testing the thickness expansion and capacity residual rate and capacity recovery rate at constant temperature of 60 ℃: firstly, the battery is placed at normal temperature and is circularly charged and discharged for 1 time (4.45V-3.0V) at 0.5C, and the discharge capacity C before the battery is stored is recorded0Then charging the battery to 4.45V full-voltage at constant current and constant voltage, testing the internal resistance R1 of the battery before high-temperature storage by using an internal resistance tester, and testing the thickness d of the battery before high-temperature storage by using a vernier caliper1(the two diagonals of the battery are respectively connected through a straight line, and the intersection point of the two diagonals is a battery thickness test point), then the battery is placed in a 60 ℃ incubator for storage for 7 days, and after the storage is finished, the battery is taken out and the thermal thickness d of the stored battery is tested2Calculating the battery thickness expansion rate after the battery is stored for 28 days at the constant temperature of 60 ℃; after the battery is cooled for 24 hours at room temperature, the internal resistance R2 after storage is tested, and the battery is carried out at 0.5C againDischarging to 3.0V at constant current, and recording the discharge capacity C after the battery is stored1And calculating the capacity residual rate of the battery after the battery is stored for 28 days at the constant temperature of 60 ℃, then carrying out constant-current constant-voltage charging on the battery to 4.45V at the temperature of 0.5 ℃, carrying out constant-current discharging on the battery to 3.0V at the temperature of 0.5 ℃, and recording the discharge capacity C of the battery2And calculating the capacity recovery rate of the battery after the battery is stored for 28 days at the constant temperature of 60 ℃, wherein the calculation formula is as follows:
thickness expansion rate of battery after 28 days of storage at 60 ═ d2-d1)/d1*100％；
After being stored for 28 days at constant temperature of 60 ℃, the residual capacity rate is C1/C0*100％。
Capacity recovery rate C after constant temperature storage at 60 ℃ for 28 days2/C0*100％
After being stored at the constant temperature of 60 ℃ for 28 days, the internal resistance change rate is (R2-R1)/R1 x 100%
(3) And (3) testing the 45 ℃ cycle performance of the battery: and (3) charging the battery with the capacity divided to 4.45V at a constant current and a constant voltage of 1C at 45 ℃, stopping the current at 0.05C, then discharging the battery to 3.0V at a constant current of 1C, and calculating the capacity retention rate of the battery in the 300 th cycle after the battery is cycled for 300 times. The calculation formula is as follows:
the 300 th cycle capacity retention (%) was (300 th cycle discharge capacity/first cycle discharge capacity) × 100%.
TABLE 2 Electrical Properties of the cells of examples 1-8 and comparative examples 1-11
As can be seen from the comparison of the electrical property test results in table 2:
(1) the addition of the chalcogenide compound can obviously improve the cycle performance of the battery and the capacity retention rate and recovery rate after high-temperature storage, can speculate that the chalcogenide additive can inhibit the oxidative decomposition of the electrolyte, has good modification effect on the anode CEI film, and can effectively inhibit the dissolution of the anode metal ions under the condition of high temperature and high pressure.
(2) The addition amount of the sulfur compound is preferably 0.5 to 1.0%. When the addition amount is too small, the film forming quality of the novel additive on the positive electrode is poor, the electrolyte can still be oxidized and decomposed on the surface of the positive electrode material, and metal ions in the positive electrode material can be dissolved out, so that the electrical property of the battery can not meet the requirement. When the addition amount is too large, the impedance of a formed passivation film on the positive electrode material is too large, so that the intercalation and deintercalation of lithium ions are hindered, the concentration difference polarization inside the battery is too large, and the electrochemical performance effect in the invention can not be achieved.
(3) Use of LiPF alone as compared to comparative example 16As the conductive lithium salt, the novel conductive lithium salt difluorophosphate with good film forming property is added in the comparative example 2, the novel conductive lithium salt difluorophosphate and the lithium bis-fluorosulfonylimide with good film forming property are added in the example 6, and the combination of various novel film forming lithium salts effectively improves the cycle performance and the high-temperature storage performance of the battery.
(4) The addition of the nitrile additive SN can obviously improve the cycle performance of the battery, and the capacity retention rate and recovery rate after high-temperature storage, because the bond energy of carbon-nitrogen triple bonds in cyano groups is high, the nitrile additive SN is not easy to be oxidized, and the nitrile additive SN can have good stability on a positive electrode and strong oxidation resistance. Meanwhile, the cyano group has stronger coordination capacity and is used for complexing cobalt ions, so that the decomposition effect of the electrode on the electrolyte is reduced.
(5) The sulfur compound alone cannot completely meet the requirement of obviously improving the electrical performance of the battery, and other additives are required to be added, so that the additives have a synergistic effect and jointly improve the electrical performance of the battery.
It will be understood by those skilled in the art that the foregoing is merely exemplary of the present invention, and is not intended to limit the invention to the particular forms disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The non-aqueous electrolyte of the high-voltage lithium ion battery comprises electrolyte lithium salt, a non-aqueous organic solvent and an additive, and is characterized in that the additive comprises the following components in percentage by mass in the non-aqueous electrolyte of the high-voltage lithium ion battery:
0.5 to 1.0% of a sulfur-based compound
0.5-3.0% of positive electrode protection additive
0.1-8.0% of negative electrode film forming additive
2. The nonaqueous electrolyte solution for a high-voltage lithium ion battery according to claim 1, wherein the sulfur-based compound has a structural formula shown in the following formula:
wherein R1 and R2 are independently selected from alkyl, alkenyl, alkynyl and fluorine-containing alkyl.
3. The nonaqueous electrolyte solution for a high-voltage lithium-ion battery according to claim 2, wherein the sulfur-based compound is one or more compounds selected from the group consisting of compounds represented by the following structural formulae:
4. the non-aqueous electrolyte for high-voltage lithium-ion batteries according to claim 1, wherein the positive electrode protection additive is one or more of adiponitrile, succinonitrile, hexanetrinitrile.
5. The non-aqueous electrolyte solution for high-voltage lithium ion batteries according to claim 1, wherein the negative electrode film-forming additive is one or more selected from vinylene carbonate, fluoroethylene carbonate, vinyl ethylene carbonate, 1, 3-propane sultone, vinyl sulfite, tris (trimethylsilane) phosphate, tris (trimethylsilane) borate, and methylene methanedisulfonate.
6. The nonaqueous electrolyte solution for a high-voltage lithium ion battery of claim 5, wherein the negative electrode film-forming additive is one or more selected from fluoroethylene carbonate, 1, 3-propane sultone, and vinylene carbonate.
7. The non-aqueous electrolyte solution for a high-voltage lithium ion battery according to claim 1, wherein the electrolyte lithium salt is at least two of lithium hexafluorophosphate, lithium bis-fluorosulfonylimide, lithium tetrafluoroborate, and lithium difluorophosphate.
8. The non-aqueous electrolyte solution for high-voltage lithium ion batteries according to claim 1, wherein the mass percentage of the electrolyte lithium salt in the non-aqueous electrolyte solution for high-voltage lithium ion batteries is 12-16.0%.
9. The nonaqueous electrolyte solution for a high-voltage lithium-ion battery of claim 1, wherein the nonaqueous organic solvent is a mixture of ethylene carbonate, propylene carbonate, diethyl carbonate, ethyl propionate and propyl propionate.
10. A high-voltage lithium ion battery, which is characterized by comprising a cathode pole piece, an anode pole piece, a separation film arranged between the cathode pole piece and the anode pole piece and the high-voltage lithium ion battery non-aqueous electrolyte as claimed in any one of claims 1 to 9.
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| CN114069046A (en) * | 2020-08-03 | 2022-02-18 | 中国科学院宁波材料技术与工程研究所 | Electrolyte for improving performance of lithium ion battery, preparation method of electrolyte and lithium ion battery |
| CN112038696A (en) * | 2020-08-07 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | High-voltage electrolyte and lithium ion battery comprising same |
| CN112038696B (en) * | 2020-08-07 | 2022-07-05 | 合肥国轩高科动力能源有限公司 | High-voltage electrolyte and lithium ion battery comprising same |
| CN114221037A (en) * | 2021-12-20 | 2022-03-22 | 山东海科创新研究院有限公司 | Solvent for electrolyte and application of solvent in high-voltage electrolyte of lithium ion battery |
| CN114583270A (en) * | 2022-01-25 | 2022-06-03 | 深圳新宙邦科技股份有限公司 | Lithium ion battery |
| CN114583270B (en) * | 2022-01-25 | 2023-12-15 | 深圳新宙邦科技股份有限公司 | Lithium ion battery |
| WO2023184071A1 (en) * | 2022-03-28 | 2023-10-05 | 宁德新能源科技有限公司 | Electrochemical device, and electronic device comprising same |
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