CN113471525A - Wide-temperature range type electrolyte for lithium iron phosphate battery - Google Patents
Wide-temperature range type electrolyte for lithium iron phosphate battery Download PDFInfo
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- CN113471525A CN113471525A CN202110698435.8A CN202110698435A CN113471525A CN 113471525 A CN113471525 A CN 113471525A CN 202110698435 A CN202110698435 A CN 202110698435A CN 113471525 A CN113471525 A CN 113471525A
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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
- H01M10/05—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
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0563—Liquid materials, e.g. for Li-SOCl2 cells
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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
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- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/002—Inorganic electrolyte
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Abstract
The invention belongs to the technical field of lithium ion batteries, and discloses a wide-temperature electrolyte for a lithium iron phosphate battery, which is characterized by comprising the following components: lithium salt 10-20 wt%, organic solvent 80-85 wt% and additive 0.5-5 wt%, and the organic solvent includes cyclic carbonate and chain carbonate. The electrolyte system is used in the temperature range of-50 ℃ to 70 ℃. In a low-temperature environment, the electrolyte system has higher conductivity, and lithium salt has higher diffusion rate in the electrolyte and in an electrode surface film; in a high-temperature environment, a stable SEI film can be formed on one side of the negative electrode, side reactions of lithium salts in the electrolyte and a solvent are inhibited, the surface chemical reaction rate of positive and negative electrode materials and the electrolyte is reduced, and the internal kinetic stability of the battery is enhanced, so that the cyclic charge and discharge capacity of the battery at high and low temperatures is improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a wide-temperature electrolyte for a lithium iron phosphate battery.
Background
With the development of science and technology, the global requirement for energy storage technology is increasingly stringent, and a lithium ion battery is one of battery systems with the best comprehensive performance, has the advantages of high specific energy, long cycle life, small volume, light weight, no memory effect, no pollution and the like, and is rapidly developing into a new generation of energy storage technology. It is obvious that the operating temperature range often limits the field of use of lithium ion batteries. The working temperature required by consumer-grade electronic equipment is usually-20-60 ℃, and is basically consistent with the limit working temperature of a conventional lithium ion battery; however, in order to adapt to temperature differences caused by regions and seasons, the electric automobile generally works in a temperature range of-30 ℃ to 70 ℃; aerospace and military equipment need stronger adaptability, and the carried battery system is required to have a wider working temperature range, and particularly the low temperature limit is expanded to be below minus 50 ℃.
The anode, the electrolyte and the cathode can all affect the wide-temperature performance of the lithium ion battery, wherein the electrolyte is used as a necessary condition for the wide-temperature work of the lithium ion battery to play an important role in transferring lithium ions and communicating internal circuits. Wide temperature electrolytes often have the following requirements: 1) a higher boiling point; 2) a lower freezing point; 3) higher ionic conductivity; 4) the charge and discharge chemistry of the anode and the cathode is met; 5) electrochemical stability. In addition, the electrolyte can generate reduction reaction on the surfaces of the negative electrode and the positive electrode, SEI films are respectively generated on the interface of the electrolyte solution of the negative electrode, and PI interface films are respectively generated on the interface of the electrolyte solution of the positive electrode, so that the cycle stability of the positive electrode and the negative electrode materials is enhanced.
However, ester-based electrolytes adopted by commercial lithium ion batteries are extremely flammable, and lithium salts in the electrolytes cannot meet application requirements of low temperature or extreme conditions in winter, so that market popularization is greatly limited. In addition, by analysis, lithium salt LiPF is commonly used6Poor thermal stability and sensitivity to moisture, and is a main cause of poor high-temperature performance of the electrolyte. The wide temperature performance of the battery needs to take both the high temperature performance and the low temperature performance of the battery into consideration. Literature indicates that lithium ion batteries mainly have diffusion problems at low temperatures, and that the diffusion is a reversible process and does not significantly damage the original battery composition and structure. Li+Diffusion rate in electrolyte and in electrode surface film, and Li+And the charge transfer rate of electrons (e) at the electrode electrolyte interface is obviously reduced along with the reduction of the temperature, so that a wide-temperature electrolyte for a lithium iron phosphate battery is designed to solve the problems.
Disclosure of Invention
In order to solve the problems of flammability and explosiveness, narrow working temperature region and the like of the conventional lithium ion battery, the invention adopts the highly fluorinated solvent and the lithium salt, greatly reduces the flammability, and improves the thermal stability and the electrochemical stability of the electrolyte at high temperature, the rate capability and the stable discharge capability at low temperature and the like. The technical scheme is as follows:
the wide-temperature electrolyte for the lithium iron phosphate battery is characterized by comprising the following components: lithium salt 10-20 wt%, organic solvent 80-85 wt% and additive 0.5-5 wt%, and the organic solvent includes cyclic carbonate and chain carbonate.
Further, the mass fractions of the lithium salt, the organic solvent and the additive are respectively as follows: 14.3 percent of lithium salt, 81.2 percent of organic solvent and 4.5 percent of additive.
Further, the cyclic carbonate is fluoroethylene carbonate (FEC), and the chain carbonate is composed of Ethyl Trifluoroacetate (ETFA), Ethyl Methyl Carbonate (EMC), and dimethyl carbonate (DMC).
Further, methyl ethyl carbonate, dimethyl carbonate, ethyl trifluoroacetate and fluoroethylene carbonate are mixed according to the mass ratio of 3-5: 3-5: 13-21: 7-11, and mixing.
Further, the mass ratio of ethyl methyl carbonate, dimethyl carbonate, ethyl trifluoroacetate and fluoroethylene carbonate is 4: 4: 15: 7.
further, the concentration of the lithium salt is 0.5 to 1.2 mol/L.
Further, the lithium salt is a high-temperature lithium salt and a low-temperature lithium salt in a molar concentration ratio of 1: 0.5 to 1.0.
Further, the high temperature lithium salt is LiSiF3(CF3CF3)3、LiSiF4SO4One or more of; the low temperature lithium salt is LiSiF4C2O4。
Further, the additive is 2,2, 2-trifluoroethyl n-butyl ester (TFENB).
The technical indexes of the components in the additive of the invention are particularly described as follows:
fluoroethylene carbonate: the purity is more than or equal to 99 percent, the water content is less than or equal to 100ppm, and the acidity is less than or equal to 200 ppm;
ethyl trifluoroacetate: the purity is more than or equal to 98.5 percent, the water content is less than or equal to 100ppm, and the acidity is less than or equal to 200 ppm;
ethyl methyl carbonate: the purity is more than or equal to 99.9 percent, the water content is less than 10ppm, and the acidity is less than 10 ppm;
dimethyl carbonate: the purity is more than or equal to 99.9 percent, the water content is less than 10ppm, and the acidity is less than 10 ppm;
ethylene carbonate: the purity is more than or equal to 99.5 percent; water content is less than or equal to 100ppm, and acidity is less than or equal to 200 ppm.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a wide-temperature electrolyte for a lithium iron phosphate battery, wherein the electrolyte system is used in a temperature range of-50-70 ℃. In a low-temperature environment, the electrolyte system has higher conductivity, and lithium salt has higher diffusion rate in the electrolyte and in an electrode surface film; in a high-temperature environment, a stable SEI film can be formed on one side of the negative electrode, side reactions of lithium salts in the electrolyte and a solvent are inhibited, the surface chemical reaction rate of positive and negative electrode materials and the electrolyte is reduced, and the internal kinetic stability of the battery is enhanced, so that the cyclic charge and discharge capacity of the battery at high and low temperatures is improved.
2. The invention selects cyclic carbonate as solvent and chain carbonate as cosolvent, the solvent system has higher lithium ion conductivity under low temperature, Li+The solvent has higher migration rate, and the fluorinated ester solvent has higher flash point and has excellent flame retardant property at high temperature. Selecting LiSiF with good low-temperature performance4C2O4Lithium salt of oxalic acid radical substituted LiSiF6The lithium salt has higher solubility in a linear carbonate solvent, so that the rate capability of the battery in a low-temperature environment is improved. Selecting LiSiF with good high-temperature performance3(CF3CF3)3LiSiF4SO4 lithium salt, which is prepared by substituting fluoroalkyl and sulfate radicals for LiSiF6In which two fluorine atoms give rise to a novel lithium salt, LiSiF3(CF3CF3)3The lithium salt not only has high thermal stability, but also can be used inLow impedance at high temperature of 80 ℃ while LiSiF4SO4The lithium salt can form a compact passive film in a high-temperature and high-pressure environment, so that the dissolution of metal ions of the anode material and the oxidative decomposition of the electrolyte are inhibited, the high-temperature cycle performance of the lithium ion battery is improved, and meanwhile, a certain protection effect on the cathode material is achieved.
3. The invention selects 2,2, 2-trifluoroethyl n-butyl ester as an additive, not only expands the use temperature range, but also can reduce the flammability of the electrolyte and is beneficial to forming a compact and stable film on an electrode. The 2,2, 2-trifluoroethyl n-butyl ester has lower viscosity compared with the fluorine-free ester, so that the conductivity and electrochemical stability of the electrolyte can be improved.
4. The invention selects the mode of combining chain carbonate and cyclic carbonate, which can not only improve the solubility of lithium salt, but also improve the conductivity of the electrolyte in low temperature environment; introduction of LiSiF4C2O4、LiSiF3(CF3CF3)3And LiSiF4SO4As lithium salt, a uniform and compact SEI film can be formed on the surfaces of the anode material and the cathode material, so that the side reaction of the electrolyte and the electrode material is inhibited, and the electrochemical stability of the electrolyte and the high-low temperature performance of the lithium ion battery are improved; 2,2, 2-trifluoroethyl n-butyl ester serving as an additive can effectively improve the safety performance and the application temperature range of the electrolyte. In a word, the electrolyte system can improve the cycle performance and the rate capability of the lithium ion battery under high-temperature and low-temperature conditions, and maintain the charge and discharge efficiency of the lithium ion battery.
Description of the drawings:
fig. 1 is a dotted graph of the change of the specific discharge capacity of a lithium iron phosphate-lithium button cell battery provided in embodiment 1 of the present invention with temperature;
fig. 2 is a dotted graph of the change of the specific discharge capacity of the lithium iron phosphate-lithium button cell battery provided in embodiment 2 of the present invention with temperature;
fig. 3 is a dotted graph showing the change of the specific discharge capacity of the lithium iron phosphate-lithium button cell battery according to the comparative example of the present invention with temperature.
Detailed Description
Example 1:
a wide-temperature electrolyte for a lithium iron phosphate battery is capable of improving the cycle performance and the rate capability of the lithium ion battery under high-temperature and low-temperature conditions and maintaining the charge-discharge efficiency of the lithium ion battery. Specifically, the composition comprises the following components: methyl ethyl carbonate, dimethyl carbonate, ethyl trifluoroacetate and fluoroethylene carbonate according to a mass ratio of 4: 4: 15: 7, mixing, wherein the concentration of lithium salt in the electrolyte is 1.0mol/L, the additive is fluoroethylene carbonate, and the concentration is 4.5 percent of the electrolyte.
Wherein the lithium salt comprises LiSiF3(CF3CF3)3、LiSiF4C2O4Mixing according to a molar ratio of 1: 0.8.
Fig. 1 is a plot of specific discharge capacity of lithium iron phosphate-lithium button cell of this example as a function of temperature.
Example 2:
a wide temperature type electrolyte for a lithium iron phosphate battery, which is different from that of example 1. Specifically, the composition comprises the following components: methyl ethyl carbonate, dimethyl carbonate, ethyl trifluoroacetate and fluoroethylene carbonate according to a mass ratio of 4: 4: 15: 7, mixing, wherein the concentration of lithium salt in the electrolyte is 1.0mol/L, the additive is fluoroethylene carbonate, and the concentration is 4.5 percent of the electrolyte.
Wherein the lithium salt comprises LiSiF4SO4、LiSiF4C2O4Mixing according to a molar ratio of 1: 1.
Fig. 2 is a plot of specific discharge capacity of the lithium iron phosphate-lithium button cell of this example as a function of temperature.
Comparative example:
in the electrolyte system of this example, the solvent is a mixture of ethyl methyl carbonate and ethylene carbonate in a mass ratio of 1:1, and the concentration of lithium salt in the electrolyte is 1.0 mol/L.
Wherein the lithium salt is LiPF6。
Fig. 3 is a dot diagram showing the change of the specific discharge capacity of the lithium iron phosphate-lithium button cell with temperature in this embodiment.
The electrolytes in examples 1 and 2 and the comparative example were prepared into lithium iron phosphate-lithium CR2032 button half-cells, respectively, and tested.
Preparing a positive plate: mixing the positive electrode material lithium iron phosphate, the binder PVDF and the conductive carbon black according to the mass ratio of 8:1:1, adding 1% NMP as a solvent and stirring, forming slurry with proper viscosity by using a homogenizer, performing ultrasonic treatment for 15 minutes, coating the slurry on a current collector copper foil by using a tape casting coating machine, moving the current collector copper foil to a thickness of 150 mu m, translating the current collector copper foil to a vacuum drying box, drying the current collector copper foil for 24 hours at 80 ℃, cutting the current collector copper foil into a positive electrode piece with an electrode piece of 14mm by using a slicing machine, weighing, calculating and recording the mass of an active substance.
The electrochemical properties of the materials obtained in all the above examples and comparative examples are shown below.
FIG. 1 shows that at different temperatures, when the lithium salt is LiSiF4SO4、LiSiF4C2O4According to the influence on the specific discharge capacity of the battery when the mixture is mixed according to the molar ratio of 1:1 and ethyl trifluoroacetate and fluoroethylene carbonate are added into a solvent, the specific discharge capacity at 25 ℃ is 144mAh g-1(ii) a The specific discharge capacity of the material is 139 mAh.g when the material is cooled to-10 DEG C-1(ii) a The specific discharge capacity of the material is 136 mAh.g when the material is cooled to-22 DEG C-1(ii) a The specific discharge capacity of the material is 132mAh g when the material is cooled to-32 DEG C-1(ii) a The specific discharge capacity of the material is 125 mAh.g when the material is cooled to-48 DEG C-1(ii) a The discharge specific capacity returned to 25 ℃ is 144mAh g-1(ii) a The specific discharge capacity of the lithium ion battery is 144mAh g when the temperature is raised to 55 DEG C-1(ii) a The specific discharge capacity of the material heated to 70 ℃ is 145mAh g-1Therefore, the battery has excellent specific capacity retention rate at low temperature, the electrolyte does not have obvious change in a high-temperature environment, and the high-temperature stability is good.
FIG. 2 shows that at different temperatures, when the lithium salt is LiSiF3(CF3CF3)3、LiSiF4C2O4According to the influence on the discharge specific capacity of the battery when the mixture is mixed according to the molar ratio of 1:0.8 and ethyl trifluoroacetate and fluoroethylene carbonate are added into a solvent, the discharge specific capacity at 25 ℃ is 143 mAh.g-1(ii) a The specific discharge capacity of the material is 139 mAh.g when the material is cooled to-10 DEG C-1(ii) a Discharge at a temperature of-22 deg.CSpecific capacity of 138mAh g-1(ii) a The specific discharge capacity is 135mAh g when the temperature is reduced to-32 DEG C-1(ii) a The specific discharge capacity of the material is 130mAh g when the material is cooled to-48 DEG C-1(ii) a The discharge specific capacity returned to 25 ℃ is 143mAh g-1(ii) a The specific discharge capacity of the lithium ion battery is 144mAh g when the temperature is raised to 55 DEG C-1(ii) a The specific discharge capacity is 146mAh g when the temperature is raised to 70 DEG C-1Therefore, the battery has excellent specific capacity retention rate at low temperature, the electrolyte does not have obvious change in a high-temperature environment, and the high-temperature stability is good.
FIG. 3 shows that at different temperatures, when the lithium salt is LiPF6When the solvent is methyl ethyl carbonate or ethylene carbonate, the specific discharge capacity of the battery is influenced, and the specific discharge capacity at 25 ℃ is 135 mAh.g-1(ii) a The specific discharge capacity of the material is 125 mAh.g when the material is cooled to-10 DEG C-1(ii) a The specific discharge capacity of the material is 100 mAh.g when the material is cooled to-22 DEG C-1(ii) a The specific discharge capacity is 50mAh g when the temperature is reduced to-32 DEG C-1(ii) a The specific discharge capacity is reduced to 10 mAh.g when the temperature is reduced to-48 DEG C-1The following; the discharge specific capacity returned to 25 ℃ is 135mAh g-1(ii) a The specific discharge capacity is increased to 55 ℃ and is from 137 mAh.g-1Reduced to 115.3mAh g-1(ii) a The specific discharge capacity is 100mAh g when the temperature is raised to 70 DEG C-1Quickly reduces to 51mAh g-1Therefore, the battery can not be normally charged and discharged at low temperature and high temperature, the capacity retention rate is very low, and the specific capacity of the battery is rapidly attenuated along with the increase of the cycle number.
Claims (9)
1. The wide-temperature electrolyte for the lithium iron phosphate battery is characterized by comprising the following components: lithium salt 10-20 wt%, organic solvent 80-85 wt% and additive 0.5-5 wt%, and the organic solvent includes cyclic carbonate and chain carbonate.
2. The wide-temperature electrolyte for the lithium iron phosphate battery as claimed in claim 1, wherein the mass fractions of the lithium salt, the organic solvent and the additive are respectively as follows: 14.3 percent of lithium salt, 81.2 percent of organic solvent and 4.5 percent of additive.
3. The wide temperature range type electrolyte for lithium iron phosphate battery as claimed in claim 1, wherein the cyclic carbonate is fluoroethylene carbonate (FEC), and the chain carbonate is composed of Ethyl Trifluoroacetate (ETFA), Ethyl Methyl Carbonate (EMC) and dimethyl carbonate (DMC).
4. The wide-temperature electrolyte for the lithium iron phosphate battery as claimed in claim 3, wherein the mass ratio of ethyl methyl carbonate, dimethyl carbonate, ethyl trifluoroacetate to fluoroethylene carbonate is 3-5: 3-5: 13-21: 7-11, and mixing.
5. The wide-temperature electrolyte for the lithium iron phosphate battery as claimed in claim 4, wherein the mass ratio of ethyl methyl carbonate, dimethyl carbonate, ethyl trifluoroacetate and fluoroethylene carbonate is 4: 4: 15: 7.
6. the wide temperature range type electrolyte for lithium iron phosphate battery as claimed in claim 1, wherein the concentration of lithium salt is 0.5-1.2 mol/L.
7. The wide temperature range type electrolyte for lithium iron phosphate battery according to claim 1, wherein the lithium salt is a high temperature lithium salt and a low temperature lithium salt at a molar concentration ratio of 1: 0.5 to 1.0.
8. The wide temperature range electrolyte for lithium iron phosphate battery as claimed in claim 7, wherein the high temperature lithium salt is LiSiF3(CF3CF3)3、LiSiF4SO4One or more of; the low temperature lithium salt is LiSiF4C2O4。
9. The wide temperature range type electrolyte for lithium iron phosphate battery as claimed in claim 1, wherein the additive is 2,2, 2-trifluoroethyl n-butyl ester (TFENB).
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