CN111313090A - Lithium ion battery electrolyte and lithium ion secondary battery containing same - Google Patents
Lithium ion battery electrolyte and lithium ion secondary battery containing same Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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Abstract
The invention discloses a lithium ion battery electrolyte, which consists of an organic solvent, conductive lithium salt and an additive, wherein the additive is a sulfonyl fluoride or sulfate compound. Solves the problems that the electrolyte in the prior art causes the CEI film formed on the surface of the LCO electrode not to be compact enough and LI+The lithium ion battery can not be effectively protected, the service life of an electrode is shortened, the deintercalation reversibility of Li + in the anode LCO material is relatively poor, and the capacity retention rate is low; by adding sulfonyl fluoride or sulfate compounds as additives into the electrolyte,the formed CEI film can be prior to the CEI film formed by the carbonate electrolyte, and the formed CEI film is more compact, so that the cycle stability of the lithium cobaltate anode can be better improved, the safety and the energy density of the lithium ion battery can be improved, and the good practicability and the durability can be shown; the electrolyte has simple preparation process, easy operation and low raw material price, and is beneficial to industrial production.
Description
Technical Field
The invention relates to the technical field of lithium ion battery electrolyte, in particular to a lithium ion battery electrolyte and a lithium ion secondary battery containing the same.
Background
Since 1990, lithium ion batteries have been known to have the advantages of high energy density, long cycle life, low environmental pollution, no memory effect, etc., and have become one of the internationally recognized ideal secondary batteries, and have been widely used in electronic devices such as mobile communication, portable computers, electric bicycles, etc. With the development of the fields of hybrid electric vehicles and pure electric vehicles expanding day by day, lithium ion batteries as ideal power sources of power vehicles face higher challenges of improving the safety performance and energy density of the batteries. The energy density of the lithium ion battery can be greatly improved by improving the working voltage. However, the application of high voltage lithium ion batteries is limited by poor high voltage cycling stability, one of the main reasons being the continued oxidative decomposition of conventional carbonate electrolytes under high voltage (> 4.3V) conditions. The decomposition products of the electrolyte are continuously deposited on the surface of the electrode, the reaction resistance of the electrode is increased, and HF which is one of the decomposition products can accelerate the dissolution of the lithium-containing transition metal electrode material, and finally, the cycle of the battery is sharply reduced.
The electrolyte of the lithium ion battery is a key part for the battery to exert the best performance, the existing electrolyte causes the CEI film formed on the surface of the LCO electrode not to be compact enough, and LI+The electrode can not be effectively protected, and the service life of the electrode is shortened; meanwhile, the Li + in the anode LCO material has relatively poor de-intercalation reversibility; and the capacity retention rate is low.
Disclosure of Invention
Aiming at the problems mentioned in the background technology, the invention provides a lithium ion battery electrolyte and a lithium ion secondary battery containing the same, which solve the problems that the electrolyte in the prior art causes that a CEI film formed on the surface of an LCO electrode is not compact enough and LI is not compact enough+Can not be effectively protected, the service life of the electrode is shortened, and Li < + > is in the extraction reversible phase of the anode LCO materialPoor in compatibility and low in capacity retention rate.
In order to achieve the purpose, the invention provides a lithium ion battery electrolyte, which is composed of an organic solvent, a conductive lithium salt and an additive, wherein the additive is a sulfonyl fluoride or sulfate compound.
The technical principle is as follows: under the protection of argon, an organic solvent is mixed with conductive lithium salt in proportion, and a sulfonyl fluoride or sulfate compound film forming additive is added to obtain an electrolyte, wherein a CEI film formed by the sulfonyl fluoride or sulfate compound additive can be prior to a CEI film formed by a carbonate electrolyte, and the formed CEI film is more compact, so that the circulation stability of a lithium cobaltate anode can be better improved, the safety and the energy density of a lithium ion battery can be improved, and good practicability and durability are shown. In addition, the electrolyte disclosed by the invention is simple in preparation process, easy to operate, low in raw material price, wide in market and beneficial to industrial production.
Further, the sulfonyl fluoride compounds comprise compounds with the following general formulas I, II, III and IV;
wherein n is 0, 1, 2, 3 … …;
R1，R1’，R2，R2’，R3，R4，R5，R6，R7，R8，R9，R9’，R10，R10' is-Me (methyl) or-Et (ethyl) or-Ph (phenyl) or-iPr (isopropyl) or-H (hydrogen) or vinyl or-F, R1，R1’，R2，R2’，R3，R4，R5，R6，R7，R8，R9，R9’，R10，R10' may be the same or different;
x is O, S, Si, CH2，C(CF3)2，C(CH3)2O ═ S ═ O, C ═ O, and C (═ O) O.
In the general formula R1Can be independently O, S, CH2，C(CF3)2，C(CH3)2O ═ S ═ O, C (═ O) O; r2Can be independently F, CI, [ (CH)2)nCH3，n≥0]，C(CF3)2，C(CH3)2O ═ S ═ O, C (═ O) O; r3Can be independently H, CI, F, Br, OCH3，CF3，CH＝CH2And OPh.
When R is1The radicals being O, S, C (CH)3)2，C(CF3)2，SO2CO, when R2Is F, CH3，R3Is F, OCH3，CF3，CH＝CH2Molecular building blocks at OPh.
Some typical additive structures are shown in the following table:
further, the sulfate compounds comprise compounds with the following general formula V;
R11，R12，R13，R14is-Me (methyl) or-Et (ethyl) or-Ph (phenyl) or-iPr (isopropyl) or-H (hydrogen) or vinyl or-F; r11，R12，R13，R14May be the same or different.
Further, the additive also comprises-OSO2F or sulfate structure-OS (═ O)2Oligomers of O-。
Further, the organic solvent is one or more of ethylene carbonate, propylene carbonate, butylene carbonate, fluoroethylene carbonate, methyl ethylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, methyl propyl carbonate, 1, 4-butyrolactone, methyl propionate, methyl butyrate, ethyl butyrate or ethyl acetate.
Further, the lithium ion battery electrolyte sulfonyl fluoride or sulfate compound additive accounts for 0.01-15% of the organic solvent in mass fraction.
Further, the concentration of the lithium salt in the electrolyte is 0.5M-2M.
Further, a preparation method of the lithium ion battery electrolyte comprises the following steps: if a mixture of a plurality of organic solvents is used, uniformly mixing the same amount of organic solvents, adding lithium salt, adding an additive, and uniformly mixing to obtain an electrolyte; if a single organic solvent is used, a lithium salt is directly added to the organic solvent; then adding the additive and mixing uniformly to obtain the electrolyte.
Further, a lithium ion secondary battery includes: a positive electrode, a negative electrode, a separator, and the organic electrolytic solution.
In summary, compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, by adding sulfonyl fluoride or sulfate compounds as additives into the electrolyte, the formed CEI film can be prior to the CEI film formed by the carbonate electrolyte, and the formed CEI film is more compact, so that the cycle stability of the lithium cobaltate anode can be better improved, the safety and energy density of the lithium ion battery can be improved, and good practicability and durability can be shown;
(2) the electrolyte disclosed by the invention is simple in preparation process, easy to operate, low in raw material price, wide in market and beneficial to industrial production;
(3) the electrolyte of the invention ensures that a CEI film formed on the surface of an LCO electrode is compact enough, and LI+The electrode can be effectively protected, and the service life of the electrode is prolonged; meanwhile, the Li + in the anode LCO material has relatively high de-intercalation reversibility; and holdThe amount retention rate is high.
Drawings
FIG. 1 is a CV curve for five cycles prior to an LCO half cell, wherein (a) is the graph for example 1 and (b) is the graph for a comparative example of example 1;
fig. 2 is an SEM image of the LCO pole pieces after 5 cycles, where the images (a, b, c) are SEM images of comparative examples and (d, e, f) are SEM images of example 1.
Detailed Description
All features disclosed in this specification may be combined in any combination, except features and/or steps that are mutually exclusive.
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to fig. 1-2 and specific examples.
Example 1
In a glove box filled with argon, Ethylene Carbonate (EC), diethyl carbonate (DEC) and dimethyl carbonate (DMC) were mixed in a volume ratio of EC: DEC: DMC of 1: 1, lithium hexafluorophosphate was used as a lithium salt at a concentration of 1M, and 5 wt.% of a film forming additive HT812-06 was added thereto and mixed uniformly to obtain an electrolyte of example 1.
Molecular structure of HT 812-06:
comparative example
Reference example 1 was made with the exception that no film-forming additive was added. In a glove box filled with argon, Ethylene Carbonate (EC), diethyl carbonate (DEC) and dimethyl carbonate (DMC) were mixed in a volume ratio of EC: DEC: DMC of 1: 1, and lithium hexafluorophosphate was used as a lithium salt at a concentration of 1M to obtain an electrolyte of a comparative example.
Example 2
Referring to example 1, the electrolyte solution preparation method is different in that 10 wt.% of film forming additive HT812-06 is added to the electrolyte solution, and the electrolyte solution of example 2 is obtained after uniform mixing.
Molecular structure of HT 812-06:
example 3
Referring to example 1, except that 5 wt.% of film forming additive HT812-07 was added to the electrolyte, and the mixture was mixed uniformly to obtain the electrolyte of example 3.
Molecular Structure of HT 812-07:
example 4
Electrolyte preparation method refer to example 1, except that 5 wt.% of film forming additive XNY-2 is added to the electrolyte, and the electrolysis of example 4 is obtained after uniform mixing.
XNY-2, molecular structure:
example 5
Referring to example 1, except that 5 wt.% of film forming additive XNY-3 was added to the electrolyte, and the mixture was mixed uniformly to obtain the electrolyte of example 5.
XNY-3, molecular structure:
the result of the detection
Table 1 shows the results of electrochemical performance tests of the electrolytes of examples 1 to 5 and comparative example.
TABLE 1
| Lithium salt | Solvent(s) | Additive agent | Capacity retention ratio/%) | |
| Example 1 | 1MLiPF6 | EC∶DEC∶DMC＝1∶1∶1 | 5％HT812-06 | 98.2 |
| Comparative example | 1MLiPF6 | EC∶DEC∶DMC＝1∶1∶1 | Is free of | 94.3 |
| Example 2 | 1MLiPF6 | EC∶DEC∶DMC＝1∶1∶1 | 10％HT812-06 | 96.1 |
| Example 3 | 1MLiPF6 | EC∶DEC∶DMC＝1∶1∶1 | 5％HT812-07 | 96.8 |
| Example 4 | 1MLiPF6 | EC∶DEC∶DMC＝1∶1∶1 | 5％XNY-2 | 97.3 |
| Example 5 | 1MLiPF6 | EC∶DEC∶DMC＝1∶1∶1 | 5％XNY-3 | 97.5 |
According to the data detected in the table, the capacity retention rate of the electrolyte in each embodiment of the application is obviously improved compared with the prior art; meanwhile, as can be seen from the CV graph of the LCO half-cell in fig. 1, the second oxidation peak a is only present in the first cycle of example 1, and disappears in the latter 4 cycles, indicating that a possible CEI film has been formed during the first cycle, thereby effectively protecting the positive electrode material. Along with the increase of the cycle number, the cycle curve coincidence is relatively good, the change of the peak current value of the main oxidation reduction peak corresponding to 4.0V and 3.8V is relatively small, and the symmetry of the oxidation peak and the reduction peak is relatively good, which indicates that the deintercalation reversibility of Li + in the anode LCO material is relatively good. In the comparative example, the superposition of the electrolyte circulation curves without the additive is not consistent, and the symmetry of the oxidation peak and the reduction peak is not good, which indicates that the deintercalation reversibility of Li + at the anode LCO is not good. From the SEM image of the LCO pole pieces after 5 weeks of cycling in FIG. 2, it can be seen that LI was not present before cycling in example 1+The LCO electrode has rough particles, more and irregular pores and uneven whole surface, after circulation, the LCO electrode has smoother surface, increased density and more uniform and fine surface particles, which shows that a CEI film formed on the surface of the LCO electrode is more compact and LI is formed on the surface of the LCO electrode+Can be effectively protected, can effectively prolong the service life of the electrode, andratio, white particles formed on the surface after the circulation, and the surface was not flat and had many depressions, indicating LI+The surface is not effectively protected, thereby greatly shortening the service life.
The above-mentioned embodiments only express the specific embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for those skilled in the art, without departing from the technical idea of the present application, several changes and modifications can be made, which are all within the protection scope of the present application.
Claims (10)
1. The lithium ion battery electrolyte is characterized by comprising an organic solvent, conductive lithium salt and an additive, wherein the additive is a sulfonyl fluoride or sulfate compound.
2. The lithium ion battery electrolyte of claim 1, wherein the sulfonyl fluoride compound comprises a compound having the following general formula I, II, III, IV;
wherein n is 0, 1, 2, 3 … …;
R1，R1’，R2，R2’，R3，R4，R5，R6，R7，R8，R9，R9’，R10，R10' is-Me (methyl) or-Et (ethyl) or-Ph (phenyl) or-iPr (isopropyl) or-H (hydrogen) or vinyl or-F, R1，R1’，R2，R2’，R3，R4，R5，R6，R7，R8，R9，R9’，R10，R10' may be the same or different;
x is0，S，Si，CH2，C(CF3)2，C(CH3)2O ═ S ═ O, C ═ O, and C (═ 0) 0.
3. The lithium ion battery electrolyte of claim 1, wherein the sulfate compound comprises a compound having the following general formula V;
wherein R is11，R12，R13，R14is-Me (methyl) or-Et (ethyl) or-Ph (phenyl) or-iPr (isopropyl) or-H (hydrogen) or vinyl or-F; r11，R12，R13，R14May be the same or different.
4. The lithium ion battery electrolyte of claim 1, wherein the additive further comprises a compound comprising-OSO2F or sulfate structure-OS (═ O)2An oligomer of O-.
5. The lithium ion battery electrolyte according to claim 1, wherein the organic solvent is one or more of ethylene carbonate, propylene carbonate, butylene carbonate, fluoroethylene carbonate, methyl ethylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, methyl propyl carbonate, 1, 4-butyrolactone, methyl propionate, methyl butyrate, ethyl butyrate or ethyl acetate.
6. The lithium ion battery electrolyte of claim 1, wherein the lithium salt comprises one or more of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium perchlorate, lithium hexafluoroarsenate, lithium bistrifluoromethylsulfonimide, lithium trifluoromethanesulfonate, lithium difluorooxalato borate, and lithium bisoxalato borate.
7. The lithium ion battery electrolyte of claim 1, wherein the lithium ion battery electrolyte sulfonyl fluoride or sulfate compound additive accounts for 0.01-15% of the organic solvent by mass fraction.
8. The lithium ion battery electrolyte of claim 1, wherein the concentration of the lithium salt in the electrolyte is 0.5M to 2M.
9. The method for preparing the electrolyte of the lithium ion battery according to any one of claims 1 to 8, wherein if a mixture of a plurality of organic solvents is used, the same amount of each organic solvent is taken and mixed uniformly, then lithium salt is added, and then an additive is added and mixed uniformly to obtain the electrolyte; if a single organic solvent is used, a lithium salt is directly added to the organic solvent; then adding the additive and mixing uniformly to obtain the electrolyte.
10. A lithium-ion secondary battery characterized by comprising: a positive electrode, a negative electrode, a separator and the organic electrolytic solution according to any one of claims 1 to 8.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111934011A (en) * | 2020-08-14 | 2020-11-13 | 莱西市寰球新能源技术中心 | Lithium ion battery electrolyte and lithium ion battery |
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| CN111934011A (en) * | 2020-08-14 | 2020-11-13 | 莱西市寰球新能源技术中心 | Lithium ion battery electrolyte and lithium ion battery |
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Application publication date: 20200619 |
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