CN112582674A - 12V start-stop lithium ion battery electrolyte - Google Patents
12V start-stop lithium ion battery electrolyte Download PDFInfo
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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
- H01M10/052—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
- H01M10/05—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
- H01M10/0568—Liquid materials characterised by the solutes
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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
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- 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
- H01M2300/0028—Organic electrolyte characterised by the solvent
- H01M2300/0037—Mixture of solvents
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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
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to the technical field of lithium ion batteries, and discloses a 12V start-stop lithium ion battery electrolyte which comprises 14-18% of lithium salt by mass, 80-84% of organic solvent by mass, and 1-3% of additive by mass. The lithium salt is lithium hexafluorophosphate and lithium bis (fluorosulfonyl) imide, and the ratio of the lithium salt to the lithium bis (fluorosulfonyl) imide is 1: 1-1.2; the organic solvent is ethylene carbonate, methyl ethyl carbonate and n-hexanoic acid-2, 2, 2-trifluoroethyl ester, and the proportion of the organic solvent is 1: 3.5-3.8: 1.5-1.7; the functional additive is beta-sulfopropionic anhydride, lithium difluorophosphate and vinylene carbonate, and the ratio of the functional additive to the vinylene carbonate is 1: 1-1.3: 1.5-1.8. The electrolyte has higher conductivity and lower interface impedance, can realize that a 12V start-stop battery can exert good pulse discharge performance at low temperature, can well run at high temperature of 45 ℃ or above, and realizes long-term balance of high and low temperature performance of the battery.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a 12V start-stop lithium ion battery electrolyte.
Background
In the face of increasingly serious energy and environmental crisis, the state implements a double-integral policy, and provides an oil consumption index of an automobile which needs to reach 5L/100km in 2020, obviously, the emission target can not be achieved by simply improving the fuel efficiency of an engine, and the hybrid and pure electromotion of the automobile are the optimal technical route. The most economical development of 48V and 12V light hybrid power systems.
At present, a 48V start-stop system is mounted on a plurality of vehicle types, but because most of electric elements on the vehicle are 12V, the system still needs DC conversion and is mounted with a 12V battery, and the 12V battery cannot be replaced in a short period of time. The 12V start-stop lithium ion battery directly replaces lead-acid start-stop, can realize weight reduction of the battery, has relatively better low-temperature power, and can effectively reduce the low-speed running fuel value of an engine, which requires the battery to have very high output characteristic in a cold period, so that the improvement of the low-temperature characteristic of the battery is particularly important, and the characteristic is required to be maintained even if the battery runs in a high-temperature environment (the internal resistance of the battery is slightly increased so as to ensure that the battery still has excellent low-temperature characteristic after running at high temperature).
At present, in order to meet the start-stop technical requirements, research is mainly carried out on the aspects of cell design, anode and cathode material modification, electrolyte additives and the like. The electrolyte is mainly prepared from various additives
The degradation caused by the decomposition of the anode and cathode materials on the surfaces is inhibited, and the high-temperature performance of the battery is improved, but the internal resistance of the battery is obviously increased, the low-temperature performance of the battery is reduced, and the normal operation of the battery in a cold period cannot be ensured. Therefore, the development of the electrolyte with low impedance, high conductivity, high stability and long-term balance of high and low temperature performance has important significance for the application development of the 12V start-stop battery.
Disclosure of Invention
The invention aims to provide a lithium ion battery electrolyte which is applied to a 12V start-stop lithium ion battery of a lithium iron phosphate LFP/graphite material system, realizes the balance of high and low temperature performances, and can meet the requirement of stable operation of the battery within a wide temperature range of-35-60 ℃.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a 12V opens stops lithium ion battery electrolyte which characterized in that includes: lithium salts, which are lithium hexafluorophosphate and lithium bis-fluorosulfonylimide; organic solvents which are ethylene carbonate, methyl ethyl carbonate and n-hexanoic acid-2, 2, 2-trifluoroethyl ester; additives which are beta-sulfopropionic anhydride, lithium difluorophosphate and vinylene carbonate.
In the scheme, the components are calculated according to the mass percentage: 14-18% of lithium salt, 80-84% of organic solvent and 1-3% of functional additive.
In the scheme, the ratio of the ethylene carbonate, the methyl ethyl carbonate and the n-hexanoic acid-2, 2, 2-trifluoroethyl ester in the organic solvent is 1: 3.5-3.8: 1.5-1.7.
In the scheme, the ratio of lithium hexafluorophosphate to lithium bis (fluorosulfonyl) imide in the lithium salt is 1: 1-1.2.
In the scheme, the ratio of beta-sulfopropionic anhydride, lithium difluorophosphate and vinylene carbonate in the functional additive is 1: 1-1.3: 1.5-1.8.
The invention has the beneficial effects that:
a mixed solvent of fluorocarboxylic acid ester and carbonate is used. The n-hexanoic acid-2, 2, 2-trifluoroethyl ester TFENH is used as a cosolvent, has a low freezing point (minus 76 ℃) and a high boiling point (150 ℃), ensures the electrochemical stability by controlling the addition amount of the cosolvent, and can effectively widen the working temperature range of the electrolyte. Compared with the traditional single carbonate-based solvent, the addition of the carbonate-based solvent can obviously reduce the viscosity of the solvent at low temperature, obviously improve the ionic conductivity and the film forming property of the electrolyte and improve the low-temperature and multiplying power charge and discharge capacity of the battery.
A complex lithium salt is used. The lithium bis (fluorosulfonyl) imide LiFSI has higher conductivity and thermal stability, and can improve the conductivity and the stability at high temperature of the electrolyte, so that the power and the high-temperature storage and cycle performance of the battery are improved; the partial use of lithium hexafluorophosphate LiPF6 on the one hand for cost reasons and on the other hand passivates the aluminium foil to inhibit corrosion of the aluminium foil by lithium bis (fluorosulfonyl imide), LiFSI.
A combination of additives beta-sulfopropionic anhydride, lithium difluorophosphate and vinylene carbonate is used. The lithium salt additive lithium difluorophosphate LiPO2F2 can inhibit the decomposition of lithium hexafluorophosphate LiPF6, and the formed SEI film has low impedance, so that the battery has good power performance and low temperature rise under high multiplying power. The sulfur-containing additive beta-sulfopropionic anhydride SPA can generate an SEI film containing more disulfide compounds, the formed SEI film has lower impedance and better interface stability, the increase rate of the SEI film impedance in the circulating process can be obviously reduced, the circulating life of a battery is prolonged, and the SEI film partially replaces vinylene carbonate VC, so that the consumption of the additive and the irreversible capacity loss of the battery can be reduced.
The electrolyte of the formula combination system can give consideration to low-temperature and high-temperature performance and low-temperature starting performance after high-temperature circulation.
Drawings
FIG. 1 is a cold start test chart of 50% SOC 10C 30S discharge at-29 ℃ for cells prepared according to various examples and comparative examples of the present invention;
FIG. 2 is a cold start test chart of 50% SOC 15C 30S discharge at-18 ℃ for cells prepared according to various examples and comparative examples of the present invention;
FIG. 3 is a graph showing the 1C charge-discharge cycle at 45 ℃ for batteries prepared according to examples of the present invention and comparative examples.
Detailed Description
The technical solutions in the examples will be clearly and completely described below. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Example 1
A12V start-stop lithium ion battery electrolyte comprises lithium salt, an organic solvent and a functional additive. The mass fractions of the components in the lithium salt in the electrolyte are respectively as follows: lithium hexafluorophosphate LiPF67.5% and lithium bis (fluorosulfonyl) imide LiFSI 8.4%. The mass fraction of each component of the organic solvent in the electrolyte is respectively as follows: ethylene carbonate EC 13%, ethyl methyl carbonate EMC 48% and n-hexanoic acid-2, 2, 2-trifluoroethyl ester TFENH 21%. The functional additive comprises the following components in percentage by mass: lithium difluorophosphate LiPO2F20.6%, vinylene carbonate VC 0.9% and beta-sulfopropionic anhydride SPA 0.6%.
Example 2
A12V start-stop lithium ion battery electrolyte comprises lithium salt, an organic solvent and a functional additive. The mass fractions of the components in the lithium salt in the electrolyte are respectively as follows: lithium hexafluorophosphate LiPF68.8% and lithium bis (fluorosulfonyl) imide LiFSI 9%. The mass fraction of each component of the organic solvent in the electrolyte is respectively as follows: ethylene carbonate EC 12.5%, ethyl methyl carbonate EMC 47.5% and n-hexanoic acid-2, 2, 2-trifluoroethyl ester TFENH 20%. The functional additive comprises the following components in percentage by mass: lithium difluorophosphate LiPO2F20.7%, vinylene carbonate VC 0.95% and beta-sulfopropionic anhydride SPA 0.55%.
Example 3
A12V start-stop lithium ion battery electrolyte comprises lithium salt, an organic solvent and a functional additive. The mass fractions of the components in the lithium salt in the electrolyte are respectively as follows: lithium hexafluorophosphate LiPF 67% and lithium bis (fluorosulfonyl) imide LiFSI 7.4%. The mass fraction of each component of the organic solvent in the electrolyte is respectively as follows: ethylene carbonate EC 13.5%, ethyl methyl carbonate EMC 49% and n-hexanoic acid-2, 2, 2-trifluoroethyl ester TFENH 21.5%. The functional additive comprises the following components in percentage by mass: lithium difluorophosphate LiPO2F20.5%, vinylene carbonate VC 0.7% and beta-sulfopropionic anhydride SPA 0.4%.
Comparative example 1
A12V start-stop lithium ion battery electrolyte used conventionally comprises lithium salt, carbonate organic solvent and functional additive. The lithium salt is lithium hexafluorophosphate LiPF6, and the mass of the electrolyte accounts for 17%. The carbonate organic solvent comprises the following components in percentage by mass: ethylene carbonate EC 20%, ethyl methyl carbonate EMC 30% and dimethyl carbonate DMC 30.5%. The functional additive comprises the following components in percentage by mass: lithium difluorophosphate LiPO2F20.7% and vinylene carbonate VC 1.8%.
The electrolytes of examples 1 to 3 and comparative example 1 were applied to 12V start-stop lithium ion batteries, respectively. The battery includes a positive electrode, a negative electrode, a separator, and the like. The active material used by the anode is super nanometer lithium iron phosphate LFP, the active material used by the cathode is a mixture of artificial graphite and soft carbon, and the diaphragm used is a wet-process bare diaphragm. The laminated battery is assembled according to the prior art to prepare a Z-shaped 20Ah laminated battery, and the laminated battery is activated to prepare a corresponding lithium ion battery.
And performing DCR test, low-temperature cold start test and high-temperature cycle test on the finished battery.
1. Room temperature DCR test
The finished batteries prepared in the above examples and comparative examples were adjusted to 50% SOC at normal temperature with 1C current, left for 60 minutes, discharged at 10C constant current for 10 seconds, left for 60 minutes, charged at 10C constant current for 10 seconds, the voltage of the battery before and after charging and discharging at 10C current was recorded, and the charging and discharging DCR of the battery was calculated from the voltage and current, and the test results are shown in table 1.
Table 1 results of room temperature DCR test for cells prepared in each example and comparative example
2. -29 ℃ 50% SOC 10C 30S discharge test
The finished batteries prepared in the above examples and comparative examples are adjusted to 50% SOC at normal temperature by 1C current, the batteries are placed at-29 ℃ for 16 hours, then discharged at 10C constant current for 30 seconds, placed for 10 minutes, discharged at 10C constant current for 30 seconds, placed for 30 seconds, discharged at 10C constant current for 30 seconds, placed for 1 hour, and then the test is finished, and the voltage of the batteries in the discharging process is recorded (the cut-off voltage of the batteries is required to be more than or equal to 2.0V for the first discharge 30S), and the test results are shown in figure 1.
3. -18 ℃ 50% SOC 15C 30S Cold Start test
The finished batteries prepared in the above examples and comparative examples are adjusted to 50% SOC at normal temperature by 1C current, the batteries are placed at-18 ℃ for 16 hours, then discharged at 15C constant current for 30 seconds, placed for 10 minutes, discharged at 15C constant current for 30 seconds, placed for 30 seconds, discharged at 15C constant current for 30 seconds, placed for 1 hour, the test is finished, and the voltage of the batteries in the discharging process is recorded (the cut-off voltage of the batteries is required to be more than or equal to 2.0V for the first discharge of 30S), and the test results are shown in FIG. 2.
4. 45 ℃ 1C Charge-discharge cycle test
The finished cells prepared in the above examples and comparative examples were subjected to 1C charge-discharge cycle test at 45C, with a charge-discharge voltage range of 2.5V to 3.65V, and the test results are shown in fig. 3 and table 2.
TABLE 2 test results after 1200 weeks at 45 ℃ and 1C cycling of each example and comparative example fabricated cells
As can be seen from the test results of tables 1 to 2 and fig. 1 to 3, the low-temperature cold start performance, the high-temperature cycle performance and the cold start performance after high-temperature cycle of the batteries prepared in examples 1 to 3 used in the present invention are significantly higher than those of the batteries prepared in the comparative example, and the balance and long-term stability of the high-low temperature performance of the 12V start-stop lithium ion battery are realized.
The n-hexanoic acid-2, 2, 2-trifluoroethyl ester TFENH cosolvent adopted in the invention can obviously reduce the viscosity of the solvent at low temperature, improve the ionic conductivity and the film forming property of the electrolyte and improve the low-temperature performance of the battery; an SEI film formed by the additive beta-sulfopropionic anhydride SPA has lower impedance and better interface stability, the increase rate of the SEI film impedance in the cycle process can be obviously reduced, and the cycle life of the battery is prolonged; the novel lithium salt lithium bis (fluorosulfonyl) imide LiFSI has high conductivity and thermal stability, can improve the conductivity and the stability at high temperature of electrolyte, and improves the high-temperature cycle performance of the battery. The components have combined action, so that the high-low temperature performance of the fresh battery and the low-temperature starting performance after high-temperature circulation can be considered at the same time.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (4)
1. The 12V start-stop lithium ion battery electrolyte is characterized by comprising the following components: 14-18 mass% of lithium salt, 80-84 mass% of organic solvent and 1-3 mass% of functional additive;
the lithium salt is lithium hexafluorophosphate and lithium bis-fluorosulfonyl imide;
the organic solvent is ethylene carbonate, methyl ethyl carbonate and n-hexanoic acid-2, 2, 2-trifluoroethyl ester; the functional additive is beta-sulfopropionic anhydride, lithium difluorophosphate and vinylene carbonate.
2. The 12V start-stop lithium ion battery electrolyte according to claim 1, wherein the ratio of lithium hexafluorophosphate to lithium bis (fluorosulfonyl) imide in the lithium salt is 1: 1-1.2.
3. The 12V start-stop lithium ion battery electrolyte according to claim 1, wherein the proportion of ethylene carbonate, methyl ethyl carbonate and n-hexanoic acid-2, 2, 2-trifluoroethyl ester in the organic solvent is 1: 3.5-3.8: 1.5-1.7.
4. The 12V start-stop lithium ion battery electrolyte according to claim 1, wherein the ratio of beta-sulfopropionic anhydride, lithium difluorophosphate and vinylene carbonate in the functional additive is 1: 1-1.3: 1.5-1.8.
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| WO2022193179A1 (en) * | 2021-03-17 | 2022-09-22 | 宁德新能源科技有限公司 | Electrolyte and electrochemical device comprising same |
| CN113659205A (en) * | 2021-08-12 | 2021-11-16 | 湖州昆仑亿恩科电池材料有限公司 | Lithium ion battery non-aqueous electrolyte and lithium ion battery |
| CN114464889A (en) * | 2022-02-09 | 2022-05-10 | 香河昆仑新能源材料股份有限公司 | Non-aqueous electrolyte for high-voltage lithium ion battery and lithium ion battery thereof |
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| CN112582674B (en) | 2022-02-11 |
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