CN112234251A - Wide-temperature-range organic electrolyte applied to lithium battery and preparation method thereof - Google Patents

Wide-temperature-range organic electrolyte applied to lithium battery and preparation method thereof Download PDF

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CN112234251A
CN112234251A CN202011038452.0A CN202011038452A CN112234251A CN 112234251 A CN112234251 A CN 112234251A CN 202011038452 A CN202011038452 A CN 202011038452A CN 112234251 A CN112234251 A CN 112234251A
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temperature range
organic electrolyte
lithium battery
wide temperature
lithium
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陈昱霖
杨芳凝
苏晓倩
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CETC 18 Research Institute
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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
    • 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
    • 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
    • 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
    • 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
    • H01M10/0569—Liquid materials characterised by the solvents
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0025—Organic electrolyte
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    • 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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Abstract

The invention belongs to the technical field of lithium batteries, and particularly relates to a wide-temperature-range organic electrolyte applied to a lithium battery and a preparation method thereof, wherein the preparation method of the wide-temperature-range organic electrolyte applied to the lithium battery comprises the following steps: the method comprises the following steps: mixing and stirring fluorinated ethylene carbonate and fluorinated methyl ethyl carbonate; step two: adding lithium bistrifluoromethylenesulfonate imide into the mixed solution obtained in the step one, and stirring until the lithium bistrifluoromethylenesulfonate imide is completely dissolved; step three: adding 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether into the solution obtained in the second step, and stirring; step four: adding diethyl carbonate to the solution obtained in step three and stirring. The invention provides a wide temperature range organic electrolyte applied to a lithium battery and having the characteristics of wide temperature range working range, wide voltage window and nonflammability and a preparation method thereof.

Description

Wide-temperature-range organic electrolyte applied to lithium battery and preparation method thereof
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to a wide-temperature-range organic electrolyte applied to a lithium battery and a preparation method thereof.
Background
The prior art and the defects are as follows:
in recent decades, the number of electric vehicles has exponentially increased due to a large-scale decrease in the cost of lithium batteries, and more than 60% of the lithium batteries are applied to electric vehicles worldwide. The electric vehicle puts forward a strict requirement on the safety of the lithium battery in a wider temperature range, and has urgent requirements on the lithium battery capable of being applied in a wide temperature range in the fields of military industry and aerospace.
The vinyl carbonate-based electrolyte for commercial lithium batteries has a stable use temperature range of only-20 to +5 c and is highly combustible, and thus is easily burnt and exploded when used or damaged under extreme conditions. In order to broaden the temperature range of use of lithium batteries, the most successful methods include the addition of small amounts of additives to the electrolyte and the addition of heating and thermal insulation means outside the battery. However, these methods reduce the energy density and power density of lithium batteries.
In the latest research progress, a lithium battery adopting liquid carbon dioxide and fluorinated methane as electrolyte can release 60% of the capacity at normal temperature at-60 ℃, but the safety of the lithium battery at normal temperature is difficult to guarantee, because the pressure inside the battery at normal temperature is up to dozens of bars; the lithium battery can work under the condition of-70 ℃ by using the ethyl acetate-based electrolyte, but the working voltage of the lithium battery is only about 2V due to the chemical instability of ethyl acetate, so that the energy density and the power density of the lithium battery are greatly reduced. In a certain sense, the electrolyte with excellent electrochemical performance under a low temperature condition is easy to generate side reaction under a high temperature condition, so that the performance of the lithium battery is reduced, mainly because the electrolyte with excellent low temperature performance is often selected to be a solvent with a lower melting point, and the solvent with the lower melting point is often unstable under the high temperature condition. The narrow temperature range of lithium batteries is thus mainly due to the strong interaction of lithium ions and solvents in order to obtain a higher conductivity.
The difficulty and significance for solving the technical problems are as follows:
therefore, based on the problems, it is of great practical significance to provide a wide temperature range organic electrolyte applied to a lithium battery and having wide temperature range working range, wide voltage window and non-flammable characteristics, and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a wide temperature range organic electrolyte applied to a lithium battery and having wide temperature range working range, wide voltage window and non-flammable characteristic for solving the technical problems in the prior art and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems in the prior art is as follows:
a preparation method of wide temperature range organic electrolyte applied to a lithium battery comprises the following steps:
the method comprises the following steps: mixing fluorinated ethylene carbonate and fluorinated methyl ethyl carbonate according to the volume ratio of 1:2-1:4, and stirring until the two solvents are completely mutually soluble;
step two: adding lithium bistrifluoromethylenesulfonate imide into the mixed solution obtained in the step one, and stirring until the lithium bistrifluoromethylenesulfonate imide is completely dissolved and the concentration of the lithium salt is 3-4M;
step three: adding 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether into the solution obtained in the second step, wherein the volume ratio of the 1,1,2, 2-tetrafluoroethyl ether to the fluorinated ethylene carbonate is 1:7-1:8, and stirring until all components in the solution are completely mutually dissolved, so that the solution is clear and transparent;
step four: adding diethyl carbonate into the solution obtained in the third step, wherein the volume ratio of the diethyl carbonate to the fluorinated ethylene carbonate is 2:1-4:1, and stirring until the solution is clear and transparent.
The invention can also adopt the following technical scheme:
in the preparation method of the wide temperature range organic electrolyte applied to the lithium battery, further, in the first step, magnetons are adopted to stir for 1-1.5 hours at the rotating speed of 200-400 r/min until the two solvents are completely mutually soluble and no layering phenomenon is generated.
In the above preparation method of the wide temperature range organic electrolyte applied to the lithium battery, further, in the second step, the rotation speed of the magnetons is 300-.
In the above preparation method of the wide temperature range organic electrolyte applied to the lithium battery, further, in the third step, the 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether is in an ultra-dry grade, and the rotation speed of the magneton is 400-ion 600 r/min.
In the above method for preparing the wide temperature range organic electrolyte for a lithium battery, further, in the fourth step, the rotation speed of the magnetons is 200-400 r/min.
In the above method for preparing a wide temperature range organic electrolyte for a lithium battery, further, the first to fourth steps are all operated in a glove box, and both the oxygen concentration and the water concentration are less than 0.01 ppm.
In the above preparation method of the wide temperature range organic electrolyte applied to the lithium battery, further, in the second step, the rotation speed of the magnetons is 300-; in the third step, the 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether is in an ultra-dry grade, and the rotating speed of magnetons is 400-600 r/min; in the fourth step, the rotating speed of the magnetons is 200-400 r/min.
The wide-temperature-range organic electrolyte is prepared by any one of the preparation methods of the wide-temperature-range organic electrolyte applied to the lithium battery.
In conclusion, the invention has the following advantages and positive effects:
1. the invention uses a large amount of fluorine-containing carbonate solvent, the voltage stability window of the electrolyte is wider and is not flammable, and simultaneously, a large proportion of weak polar solvent is introduced; the lithium salt is selected from LiTFSI, so that the lithium salt has the advantage of good high-temperature stability; the electrolyte can be applied to a lithium metal battery; the invention has the characteristics of wide temperature range working range, wide voltage window and nonflammability.
2. The method has the advantages of simple operation steps, simple equipment and easy preparation.
3. The wide-temperature-range organic electrolyte effectively regulates and controls the interaction between lithium ions and solvent molecules and between solvent molecules and solvent molecules through a composite solvent system, so that the mutual dissolution of a strong-polarity solvent, a weak-polarity solvent and lithium salt is realized, and the wide-temperature-range working range and higher ionic conductivity of the electrolyte are realized; meanwhile, a large amount of fluorine-containing components in the electrolyte make the electrolyte not easy to burn and have a wider voltage window.
Drawings
FIG. 1 is a photograph of a wide temperature range electrolyte prepared in example one at 50 and-70 deg.C;
FIG. 2 is a schematic diagram of the molecular dynamics simulation of the wide temperature range electrolyte prepared in the first example;
FIG. 3a is a discharge curve of soft-packed metal oxide lithium battery (MOX-Li) injected with wide temperature range electrolyte at 50 ℃ in example one;
FIG. 3b is a discharge curve of soft-packed metal oxide lithium battery (MOX-Li) injected with wide temperature range electrolyte at-70 ℃ in example one;
FIG. 4 shows the wide temperature range electrolyte and 1MLiPF prepared in example one6Cycle and capacity curves for EC/DMC injection soft package metal oxide secondary battery (NCM-Li) at different temperature intervals. The discharge rate was 1C.
Detailed Description
The present invention will be described in detail with reference to fig. 1 to 4.
In order to further understand the contents, features and effects of the present invention, the following embodiments are illustrated and described in detail with reference to the accompanying drawings:
example 1
Step 1, mixing fluorinated ethylene carbonate and fluorinated methyl ethyl carbonate according to the volume ratio of 1:2, and stirring for 1h by using magnetons at the rotating speed of 200r/min until the two solvents are completely mutually soluble and no layering phenomenon is generated.
And 2, adding lithium bistrifluoromethylenesulfonate imide into the mixed solution obtained in the step 1, and stirring with magnetons at the rotating speed of 300r/min until the lithium salt is completely dissolved, wherein the concentration range of the lithium salt is 3M.
And 3, adding 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether into the solution obtained in the step 2, wherein the volume ratio of the 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether to the fluorinated ethylene carbonate is 1:7, and stirring by using magnetons at the rotating speed of 400r/min until all components in the solution are completely mutually dissolved, so that the solution is clear and transparent.
And 4, adding diethyl carbonate into the solution obtained in the step 3, wherein the volume ratio of the diethyl carbonate to the vinyl fluoride carbonate is 2:1, and stirring by using magnetons at the rotating speed of 200r/min until the solution is clear and transparent.
And packaging the soft package battery under the vacuum degree of-0.9 MPa after liquid injection, and performing secondary packaging under the vacuum degree of-0.9 MPa after the soft package battery is subjected to subsidence for 24 hours at the temperature of 40 ℃.
The experimental results are as follows:
the wide temperature range electrolyte prepared in example 1 has a very low melting point and remains liquid at-70 ℃ (as shown in fig. 1).
Fig. 1 is an optical photograph of fluorine-doped graphene at-70 ℃ and 50 ℃, and it can be seen from the photograph that the electrolyte is in a liquid state at-70 ℃ and 50 ℃.
The various solvent molecules, lithium ions and anions of the wide temperature range electrolyte prepared in example 1 were uniformly distributed in the electrolyte system (as shown in fig. 2).
Fig. 2 is a molecular dynamics simulation diagram of the wide temperature range electrolyte, the area size is 65.1 × 65.1a3, the interaction between each solvent molecule and each ion is represented by a ball-stick model, it can be seen from the diagram that lithium ions and solvent molecules are uniformly distributed in a model interval and are also uniformly distributed in a smaller interval, which illustrates the good uniformity of the electrolyte system, and meanwhile, the ball-stick model shows that lithium ions are combined with less strongly polar solvent molecules and have smaller desolvation energy.
The wide temperature range electrolyte prepared in example 1 has excellent electrical properties at both-70 ℃ and 50 ℃ and can be discharged at a rate of 1C in a lithium metal oxide primary cell (as shown in fig. 3).
It can be seen from fig. 3 that the discharge capacity of the primary lithium battery injected with the wide temperature range electrolyte exceeds the normal temperature rated capacity at 50 ℃ and reaches 105% of the normal temperature capacity, mainly because the internal resistance of the battery is reduced along with the increase of the temperature; and 95% of the normal-temperature capacity is released at the temperature of-70 ℃, which indicates that the electrolyte shows excellent high-temperature and low-temperature performance in a lithium primary battery system.
The wide temperature range electrolyte prepared in example 1 has excellent electrical properties in different temperature ranges, and can be discharged at a rate of 1C in a lithium metal oxide secondary battery (as shown in fig. 4).
From fig. 4, it can be seen that the wide temperature range electrolyte exhibits good electrical properties, i.e. high capacity retention and good cycle performance, in the range from-85 ℃ to 70 ℃; the opposite 1MLiPF6EC/DMC electrolyte failed again at low temperature and high temperature.
Example 2
Step 1, mixing fluorinated ethylene carbonate and fluorinated methyl ethyl carbonate according to the volume ratio of 2:5, and stirring for 1.5 hours by using magnetons at the rotating speed of 250r/min until the two solvents are completely mutually soluble and no layering phenomenon is generated.
And 2, adding lithium bistrifluoromethylenesulfonate imide into the mixed solution obtained in the step 1, and stirring with magnetons at a rotating speed of 400r/min until the lithium salt is completely dissolved, wherein the concentration range of the lithium salt is 3M.
And 3, adding 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether into the solution obtained in the step 2, wherein the volume ratio of the 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether to the fluorinated ethylene carbonate is 1:8, and stirring by using magnetons at the rotating speed of 400r/min until all components in the solution are completely mutually dissolved, so that the solution is clear and transparent.
And 4, adding diethyl carbonate into the solution obtained in the step 3, wherein the volume ratio of the diethyl carbonate to the vinyl fluoride carbonate is 3:1, and stirring by using magnetons at the rotating speed of 300r/min until the solution is clear and transparent.
Example 3
Step 1, mixing fluorinated ethylene carbonate and fluorinated methyl ethyl carbonate according to the volume ratio of 1:3, and stirring for 1h by using magnetons at the rotating speed of 300r/min until the two solvents are completely mutually soluble and no layering phenomenon is generated.
And 2, adding lithium bistrifluoromethylenesulfonate imide into the mixed solution obtained in the step 1, and stirring with magnetons at the rotating speed of 400r/min until the lithium salt is completely dissolved, wherein the concentration range of the lithium salt is 4M.
And 3, adding 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether into the solution obtained in the step 2, wherein the volume ratio of the 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether to the fluorinated ethylene carbonate is 1:8, and stirring by using magnetons at the rotating speed of 400r/min until all components in the solution are completely mutually dissolved, so that the solution is clear and transparent.
And 4, adding diethyl carbonate into the solution obtained in the step 3, wherein the volume ratio of the diethyl carbonate to the vinyl fluoride carbonate is 3:1, and stirring by using magnetons at the rotating speed of 300r/min until the solution is clear and transparent.
Example 4
Step 1, mixing fluorinated ethylene carbonate and fluorinated methyl ethyl carbonate according to the volume ratio of 1:4, and stirring for 1.5 hours by using magnetons at the rotating speed of 400r/min until the two solvents are completely mutually soluble and no layering phenomenon is generated.
And 2, adding lithium bistrifluoromethylenesulfonate imide into the mixed solution obtained in the step 1, and stirring with magnetons at the rotating speed of 300r/min until the lithium salt is completely dissolved, wherein the concentration range of the lithium salt is 3M.
And 3, adding 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether into the solution obtained in the step 2, wherein the volume ratio of the 1,1,2, 2-tetrafluoroethyl ether to the fluorinated ethylene carbonate is 1:8, and stirring by using magnetons at the rotating speed of 600r/min until all components in the solution are completely mutually dissolved, so that the solution is clear and transparent.
And 4, adding diethyl carbonate into the solution obtained in the step 3, wherein the volume ratio of the diethyl carbonate to the vinyl fluoride carbonate is 4:1, and stirring by using magnetons at the rotating speed of 400r/min until the solution is clear and transparent.
The electrolyte with wide temperature range prepared in the second to fourth embodiments is consistent with the electrolyte obtained in the first embodiment in chemical composition, and the physical properties and the electrochemical performance are basically consistent.
In summary, the present invention provides a wide temperature range organic electrolyte for a lithium battery, which has a wide temperature range working range, a wide voltage window and a non-flammable characteristic, and a preparation method thereof.
The present invention has been described in detail with reference to the above examples, but the description is only for the preferred examples of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.

Claims (8)

1. A preparation method of wide temperature range organic electrolyte applied to a lithium battery is characterized by comprising the following steps: the preparation method of the wide temperature range organic electrolyte applied to the lithium battery comprises the following steps:
the method comprises the following steps: mixing fluorinated ethylene carbonate and fluorinated methyl ethyl carbonate according to the volume ratio of 1:2-1:4, and stirring until the two solvents are completely mutually soluble;
step two: adding lithium bistrifluoromethylenesulfonate imide into the mixed solution obtained in the step one, and stirring until the lithium bistrifluoromethylenesulfonate imide is completely dissolved and the concentration of the lithium salt is 3-4M;
step three: adding 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether into the solution obtained in the second step, wherein the volume ratio of the 1,1,2, 2-tetrafluoroethyl ether to the fluorinated ethylene carbonate is 1:7-1:8, and stirring until all components in the solution are completely mutually dissolved, so that the solution is clear and transparent;
step four: adding diethyl carbonate into the solution obtained in the third step, wherein the volume ratio of the diethyl carbonate to the fluorinated ethylene carbonate is 2:1-4:1, and stirring until the solution is clear and transparent.
2. The method for preparing a wide temperature range organic electrolyte for a lithium battery according to claim 1, wherein: in the first step, magnetons are adopted to stir for 1-1.5h at the rotating speed of 200-400 r/min until the two solvents are completely mutually soluble and no layering phenomenon is generated.
3. The method for preparing a wide temperature range organic electrolyte for a lithium battery according to claim 1, wherein: in the second step, the rotation speed of the magnetons is 300-400 r/min.
4. The method for preparing a wide temperature range organic electrolyte for a lithium battery according to claim 1, wherein: in the third step, the 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether is in an ultra-dry grade, and the rotating speed of magnetons is 400-600 r/min.
5. The method for preparing a wide temperature range organic electrolyte for a lithium battery according to claim 1, wherein: in the fourth step, the rotating speed of the magnetons is 200-400 r/min.
6. The method for preparing a wide temperature range organic electrolyte for a lithium battery according to claim 1, wherein: and the first step to the fourth step are all operated in a glove box, and the oxygen concentration and the water concentration are both less than 0.01 ppm.
7. The method of preparing a wide temperature range organic electrolyte for a lithium battery according to claim 2, wherein: in the second step, the rotation speed of the magnetons is 300-400 r/min; in the third step, the 1,1,2, 2-tetrafluoroethyl-2, 2, 2-trifluoroethyl ether is in an ultra-dry grade, and the rotating speed of magnetons is 400-600 r/min; in the fourth step, the rotating speed of the magnetons is 200-400 r/min.
8. A wide temperature range organic electrolyte is characterized in that: the wide temperature range organic electrolyte is prepared by the method for preparing the wide temperature range organic electrolyte for a lithium battery according to any one of claims 1 to 7.
CN202011038452.0A 2020-09-28 2020-09-28 Wide-temperature-range organic electrolyte applied to lithium battery and preparation method thereof Pending CN112234251A (en)

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