CN105633464A - Trimethyl borate additive contained high-voltage functional electrolyte and preparation method and application therefor - Google Patents
Trimethyl borate additive contained high-voltage functional electrolyte and preparation method and application therefor 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
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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Abstract
The invention discloses a trimethyl borate additive contained high-voltage functional electrolyte and a preparation method and an application therefor. The electrolyte is obtained by adding a functional additive to a common electrolyte; the common electrolyte is formed by a cyclic carbonate solvent, a linear carbonate solvent and a conductive lithium salt; and the functional additive adopts trimethyl borate. According to the functional electrolyte, the trimethyl borate additive is taken as the high-voltage film-forming additive for the lithium ion electrolyte; the additive is relatively low in oxidization and reduction potential, so that a compact and stable SEI film layer can be formed on the surfaces of a positive electrode and a negative electrode in the first charge-discharge process; therefore, the films on the surfaces of the positive electrode and the negative electrode are optimized, the resistance between the positive electrode and the electrolyte is lowered, and the surface activity of the electrodes is restrained, so that the further contact between the electrolyte and the electrode active material is restrained consequently, and the oxidization and decomposition of the electrolyte main body solvent on the electrode surface is lowered; and the cycling performance and the rate capability of the electrolyte additive contained lithium ion battery under 3-4.5V can be improved.
Description
Technical field
The invention belongs to field of lithium ion battery, in particular to and the high voltage functionality electrolytic solution of a kind of boronic acid containing trimethyl additive and its preparation method and application.
Background technology
Lithium ion battery has that energy density is big, operating voltage height and the advantage that has extended cycle life etc. The positive electrode material of current business lithium ion battery has lithium manganate, cobalt acid lithium, iron lithium phosphate, ternary material, and these are several, charge cutoff voltage is generally all no more than 4.2V, along with the progress of science and technology and the development in market, the energy density promoting lithium cell seems important and urgent day by day. Except the improvement of current material and battery production technology, high-voltage (> 4.5V) positive electrode material compares one of popular research direction, mainly realizes the high-energy-density of battery by promoting the charging degree of depth of positive electrode active materials.
Along with the progress of science and technology, the requirement of energy storage device is improved by the fields such as electronic product, electromobile, medical facilities and space flight and aviation day by day, and energy density height, volume lithium ion battery little, that have extended cycle life is used widely. At present, it is several that the positive electrode material of business lithium ion battery mainly contains lithium manganate, cobalt acid lithium, ternary material, LiFePO 4, and its charge cutoff voltage is generally no more than 4.2V. Along with the progress of science and technology and the development in market, the energy density promoting lithium cell seems important and urgent day by day. Therefore the energy density promoting the use voltage of lithium ion battery thus improve battery is the emphasis of research at present.
But, while improving positive electrode material voltage, the electrical properties such as the charge and discharge cycles of battery are but in decline, and reason is that ternary material material structure is stable not on the one hand, are then the coupling problem of electrolytic solution on the other hand. Conventional commercial electrolyte liquid is under high voltages easily in battery positive electrode surface oxygenolysis, and the oxidative decomposition of electrolytic solution self also can impel the pernicious reactions such as positive electrode material shape looks change, structure is caved in simultaneously. Therefore must develop a kind of ability (> 4.5V) the electrolytic solution of high-voltage, and then realize the excellent performance of lithium battery performance, it is to increase lithium battery cycle life. It is the most economical method of most convenient improving performance of lithium ion battery by adding a small amount of electrolysis additive in the lithium-ion battery electrolytes of routine.
Summary of the invention
In order to overcome the shortcoming of prior art and deficiency, the primary and foremost purpose of the present invention is to provide the high voltage functionality electrolytic solution of a kind of boronic acid containing trimethyl additive. This electrolytic solution is by adding functional additive trimethyl borate (TB), when being applied to lithium ion battery, the surfactivity of positive electrode material can be reduced, suppress the oxygenolysis of electrolytic solution, it is possible to improve high-voltage lithium ion batteries cycle performance at normal temperatures and high rate performance. Cyclical stability when this electrolytic solution can significantly improve lithium ion battery high-voltage and high rate performance.
The preparation method of the high voltage functionality electrolytic solution of the boronic acid containing trimethyl additive described in offer is provided.
It is still another object of the present invention to provide the application of the high voltage functionality electrolytic solution of described boronic acid containing trimethyl additive.
The object of the present invention is achieved through the following technical solutions:
A high voltage functionality electrolytic solution for boronic acid containing trimethyl additive, this electrolytic solution adds functional additive in general electrolytic liquid and obtains; Described general electrolytic liquid is made up of cyclic carbonate ester solvent, linear carbonates solvent and electric conducting lithium salt; Described functional additive is trimethyl borate (TB);
Described high pressure refers to the high-voltage that charge cutoff voltage is greater than 4.2;
The interpolation of described functional additive optimizes positive pole/electrolyte interface, reduce the surfactivity of positive pole, suppressing the oxygenolysis of electrolytic solution, so the present invention can improve high-voltage (> 4.2V) ternary material is circulation and the high rate performance of the lithium cell of positive electrode material.
Described ternary material is nickle cobalt lithium manganate (LiNi1/3Co1/3Mn1/3O2), but it is not limited to this;
Described functional additive content is the 1��20% of general electrolytic liquid quality; It is preferably 2%��10%.
As preferably, shown in the solvent burden ratio of described general electrolytic liquid: the mass ratio of cyclic carbonate ester solvent and linear carbonates solvent is (1:3)��(3:2);
The final concentration of described electric conducting lithium salt in general electrolytic liquid is 0.8��1.2mol/L;
Described cyclic carbonate ester solvent is preferably NSC 11801 (EC) or propylene carbonate (PC);
Described linear carbonates solvent comprises methylcarbonate (DMC), Methyl ethyl carbonate (EMC), at least one in diethyl carbonate (DEC) and methyl propyl carbonate (MPC);
Described electric conducting lithium salt is selected from lithium hexafluoro phosphate (LiPF6), LiBF4 (LiBF4), dioxalic acid lithium tetraborate (LiBOB), difluorine oxalic acid boracic acid lithium (LiDFOB), trifluoromethyl sulfonic acid lithium (LiSO3CF3), lithium perchlorate (LiClO4), hexafluoroarsenate lithium (LiAsF6), bis trifluoromethyl sulfimide lithium (Li (CF3SO2)2And LiC (CF N)3SO2)3In at least one;
The preparation method of the high voltage functionality electrolytic solution of described boronic acid containing trimethyl additive, comprises the steps:
(1) cyclic carbonate ester solvent and linear carbonates solvent are mixed, clarification, except water;
At ambient temperature, (2) electric conducting lithium salt is added in the solvent that step (1) obtains, obtain general electrolytic liquid;
(3) the general electrolytic liquid obtained in step (2) adds functional additive, obtains the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive; Described functional additive is trimethyl borate;
Cyclic carbonate ester solvent described in step (1) and described linear carbonates solvent be (1:3)��(3:2) mixing in mass ratio preferably;
Described cyclic carbonate ester solvent is preferably NSC 11801 (EC) or propylene carbonate (PC);
Described linear carbonates solvent comprises methylcarbonate (DMC), Methyl ethyl carbonate (EMC), at least one in diethyl carbonate (DEC) and methyl propyl carbonate (MPC);
Clarification described in step (1), process preferably by any one or a few in molecular sieve, gac, hydrolith, lithium hydride, anhydrous calcium oxide, calcium chloride, Vanadium Pentoxide in FLAKES, basic metal or alkaline-earth metal except water;
Described molecular sieve can adoptType,Type orType, preferably selectsType orType.
The temperature of the room temperature described in step (2) is 25��40 DEG C;
The final concentration that the consumption of the electric conducting lithium salt described in step (2) is preferably in described general electrolytic liquid is 0.8��1.2mol/L;
Described electric conducting lithium salt is selected from lithium hexafluoro phosphate (LiPF6), LiBF4 (LiBF4), dioxalic acid lithium tetraborate (LiBOB), difluorine oxalic acid boracic acid lithium (LiDFOB), trifluoromethyl sulfonic acid lithium (LiSO3CF3), lithium perchlorate (LiClO4), hexafluoroarsenate lithium (LiAsF6), bis trifluoromethyl sulfimide lithium (Li (CF3SO2)2And LiC (CF N)3SO2)3In at least one;
The high voltage functionality electrolytic solution of described boronic acid containing trimethyl additive is applied to manufacture lithium ion battery, and the battery obtained has good charge-discharge performance.
A lithium ion battery for high voltage functionality electrolytic solution containing above-mentioned boronic acid containing trimethyl additive, comprises positive plate and negative plate, electrolytic solution, barrier film; Described positive plate is made up of ternary material, and negative plate is made up of graphite material, and the barrier film being interval between positive plate and negative plate is made up of polyethylene film, and described electrolytic solution is the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive described above.
The functional additive that the present invention uses is in the discharge and recharge system of 3��4.5V; the lower stable film with protection function of a layer impedance is defined at positive electrode surface; inhibit the oxygenolysis of high-voltage electrolyte on the one hand; protect positive electrode material on the other hand, it is possible to improve cycle performance and the high rate performance of high-voltage lithium ion simultaneously.
The present invention, relative to prior art, has following advantage and effect:
The present invention uses trimethyl borate additive as the high pressure film for additive of lithium-ion electrolyte, there is lower oxidation and reduction potential due to such additive, first charge-discharge process can form one layer of densification, stable SEI film at positive pole and negative terminal surface, optimize positive and negative electrode surface film, reduce the resistance between positive pole and electrolytic solution, suppress the surfactivity of electrode, thus suppress electrolytic solution to contact with the further of electrode active material, reduce the oxygenolysis of electrolytic solution bulk solvent at electrode surface. The cycle performance of lithium ion battery containing this kind of electrolysis additive under 3��4.5V and high rate performance improve.
Accompanying drawing explanation
Fig. 1 is the lithium ion battery linear time base sweep comparison diagram of the electrolytic solution making that the embodiment of the present invention 1 is prepared with comparative example.
Fig. 2 is the discharge and recharge comparison diagrams of lithium ion battery circulation 200 circle of the electrolytic solution making that the embodiment of the present invention 1 is prepared with comparative example.
Fig. 3 is the lithium ion battery high rate performance comparison diagram of the electrolytic solution making that the embodiment of the present invention 1 is prepared with comparative example.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
(1) by cyclic carbonate ester solvent NSC 11801 (EC) and linear carbonates solvent Methyl ethyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, and adopt molecular sieve, hydrolith, lithium hydride clarification, except water;
At ambient temperature, (2) by electric conducting lithium salt LiPF6Being dissolved in the solvent that step (1) obtains, final concentration is 1.0mol/L, stirs evenly, obtains general electrolytic liquid;
(3) consumption adding trimethyl borate in the general electrolytic liquid prepared in step (2) is the 10% of general electrolytic liquid quality; Obtain the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive.
Embodiment 2
(1) by cyclic carbonate ester solvent NSC 11801 (EC) and linear carbonates solvent Methyl ethyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, and adopt molecular sieve, hydrolith, lithium hydride clarification, except water;
At ambient temperature, (2) by electric conducting lithium salt LiPF6Being dissolved in the solvent that step (1) obtains, final concentration is 1.0mol/L, stirs evenly, is made into general electrolytic liquid;
(3) consumption adding trimethyl borate in the general electrolytic liquid prepared in step (2) is the 2% of general electrolytic liquid quality; Obtain the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive.
Embodiment 3
(1) by cyclic carbonate ester solvent NSC 11801 (EC) and linear carbonates solvent Methyl ethyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, molecular sieve, hydrolith, lithium hydride clarification is adopted, except water;
At ambient temperature, (2) by electric conducting lithium salt LiPF6Being dissolved in the solvent that step (1) obtains, final concentration is 1.0mol/L, stirs evenly, is made into general electrolytic liquid;
(3) consumption adding trimethyl borate in the general electrolytic liquid prepared in step (2) is the 3% of general electrolytic liquid quality; Obtain the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive.
Embodiment 4
(1) by cyclic carbonate ester solvent NSC 11801 (EC) and linear carbonates solvent Methyl ethyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, molecular sieve, hydrolith, lithium hydride clarification is adopted, except water;
At ambient temperature, (2) by electric conducting lithium salt LiPF6Being dissolved in the solvent that step (1) obtains, final concentration is 1.0mol/L, stirs evenly, is made into general electrolytic liquid;
(3) consumption adding trimethyl borate in the general electrolytic liquid prepared in step (2) is the 4% of general electrolytic liquid quality; Obtain the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive.
Embodiment 5
(1) by cyclic carbonate ester solvent NSC 11801 (EC) and linear carbonates solvent Methyl ethyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, molecular sieve, hydrolith, lithium hydride clarification is adopted, except water;
At ambient temperature, (2) by electric conducting lithium salt LiAsF6Being dissolved in the solvent that step (1) obtains, final concentration is 1mol/L, stirs evenly, is made into general electrolytic liquid;
(3) consumption adding trimethyl borate in the general electrolytic liquid prepared in step (2) is the 3% of general electrolytic liquid quality; Obtain the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive.
Embodiment 6
(1) by cyclic carbonate ester solvent NSC 11801 (EC) and linear carbonates solvent Methyl ethyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, molecular sieve, hydrolith, lithium hydride clarification is adopted, except water;
At ambient temperature, (2) by electric conducting lithium salt Li (CF3SO2)2N is dissolved in the solvent that step (1) obtains, and final concentration is 1.0mol/L, stirs evenly, is made into general electrolytic liquid;
(3) consumption adding trimethyl borate in the general electrolytic liquid prepared in step (2) is the 3% of general electrolytic liquid quality; Obtain the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive.
Embodiment 7
(1) by cyclic carbonate ester solvent NSC 11801 (EC) and linear carbonates solvent Methyl ethyl carbonate (EMC) and diethyl carbonate (DEC) EC: EMC: DEC=3: 5: 2 mixing in mass ratio, molecular sieve, hydrolith, lithium hydride clarification is adopted, except water;
At ambient temperature, (2) by electric conducting lithium salt LiC (CF3SO2)3Being dissolved in the solvent that step (1) obtains, final concentration is 1.0mol/L, stirs evenly, is made into general electrolytic liquid;
(3) consumption adding trimethyl borate in the general electrolytic liquid prepared in step (2) is the 3% of general electrolytic liquid quality; Obtain the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive.
Comparative example
(1) by cyclic carbonate ester solvent NSC 11801 (EC) and linear carbonates solvent Methyl ethyl carbonate (EMC) and diethyl carbonate (DEC) EC:EMC:DEC=3:5:2 mixing in mass ratio, molecular sieve, lithium hydride clarification is adopted, except water;
At ambient temperature, (2) by electric conducting lithium salt LiPF6Being dissolved in the solvent that step (1) obtains, final concentration is 1.0mol/L, stirs evenly, is made into general electrolytic liquid.
Effectiveness comparison:
High voltage functionality electrolytic solution (being also namely 10%TB) and contrast general electrolytic liquid (being also namely STD) of boronic acid containing trimethyl additive embodiment 1 prepared compare:
(1) Fig. 1 is the linear time base sweep comparison diagram of the lithium ion battery of the electrolytic solution making that embodiment 1 is prepared with comparative example. Testing method is: work electrode with nickel manganese cobalt acid lithium, lithium sheet does electrode, the each 30 micro-liters of general electrolytic liquid prepared by the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive prepared by interpolation embodiment 1 and comparative example, carry out linear time base sweep electro-chemical test at Solartron-1470 (Britain) multi-channel analyzer after then becoming battery according to the assembled in sequence of negative cover, spring piece, pad, lithium sheet, positive pole, positive cover. Sweep velocity is 0.1mV/s; 6.0V is swept to from 3.0V; Fig. 1 shows that the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive prepared by embodiment 1 has lower oxidizing potential; illustrate that trimethyl borate can at positive electrode surface preferential oxidation; form layer protecting film, thus suppress the further oxygenolysis of carbonate solvent.
(2) Fig. 2 is the discharge and recharge comparison diagrams of lithium ion battery circulation 200 circle of the electrolytic solution making that the embodiment of the present invention 1 is prepared with comparative example. As can be seen from the results, electrolytic solution add the used for electrolyte of trimethyl borate and can improve its cycle performance under high voltages in lithium ion battery.
(3) Fig. 3 is the lithium ion battery high rate performance test comparison figure of the electrolytic solution making that the embodiment of the present invention 1 is prepared with comparative example. As can be seen from the results, after adding trimethyl borate in electrolytic solution, the high rate performance of lithium ion battery significantly improves, and illustrates that this additive can reduce, the interface resistance between electrolytic solution/electrode.
Above-described embodiment is that the present invention preferably implements mode; but embodiments of the present invention are not restricted to the described embodiments; the change done under the spirit of other any the present invention of not deviating from and principle, modification, replacement, combination, simplification; all should be the substitute mode of equivalence, it is included within protection scope of the present invention.
Claims (10)
1. the high voltage functionality electrolytic solution of a boronic acid containing trimethyl additive, it is characterised in that: this electrolytic solution adds functional additive in general electrolytic liquid and obtains; Described general electrolytic liquid is made up of cyclic carbonate ester solvent, linear carbonates solvent and electric conducting lithium salt; Described functional additive is trimethyl borate.
2. the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive according to claim 1, it is characterised in that: described functional additive content is the 1��20% of general electrolytic liquid quality.
3. the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive according to claim 1, it is characterised in that: described cyclic carbonate ester solvent and the mass ratio of linear carbonates solvent are (1:3)��(3:2);
The final concentration of described electric conducting lithium salt in general electrolytic liquid is 0.8��1.2mol/L.
4. the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive according to claim 1, it is characterised in that: described cyclic carbonate ester solvent is NSC 11801 or propylene carbonate;
Described linear carbonates solvent comprises methylcarbonate, Methyl ethyl carbonate, at least one in diethyl carbonate and methyl propyl carbonate.
5. the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive according to claim 1, it is characterised in that: described electric conducting lithium salt is selected from LiPF6��LiBF4��LiBOB��LiDFOB��LiSO3CF3��LiClO4��LiAsF6��Li(CF3SO2)2N and LiC (CF3SO2)3In at least one.
6. the preparation method of the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive described in the arbitrary item of Claims 1 to 5, it is characterised in that comprise the steps:
(1) cyclic carbonate ester solvent and linear carbonates solvent are mixed, clarification, except water;
At ambient temperature, (2) electric conducting lithium salt is added in the solvent that step (1) obtains, obtain general electrolytic liquid;
(3) the general electrolytic liquid obtained in step (2) adds functional additive, obtains the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive.
7. the preparation method of the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive according to claim 6, it is characterised in that: the clarification described in step (1), processed by any one or a few in molecular sieve, gac, hydrolith, lithium hydride, anhydrous calcium oxide, calcium chloride, Vanadium Pentoxide in FLAKES, basic metal or alkaline-earth metal except water.
8. the preparation method of the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive according to claim 7, it is characterised in that: described molecular sieve adoptsType,Type orType.
9. the high voltage functionality electrolytic solution of boronic acid containing trimethyl additive described in the arbitrary item of Claims 1 to 5 is in the application manufactured in lithium ion battery.
10. one kind contains the lithium ion battery of the high voltage functionality electrolytic solution of the boronic acid containing trimethyl additive described in the arbitrary item of Claims 1 to 5, it is characterised in that comprise positive plate and negative plate, electrolytic solution, barrier film; Described positive plate is made up of ternary material, negative plate is made up of graphite material, the barrier film being interval between positive plate and negative plate is made up of polyethylene film, and described electrolytic solution is the high voltage functionality electrolytic solution of the boronic acid containing trimethyl additive described in the arbitrary item of Claims 1 to 5.
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| CN112909339A (en) * | 2021-03-23 | 2021-06-04 | 深圳赛骄阳能源科技股份有限公司 | Propylene carbonate-based electrolyte and lithium ion battery containing same |
| CN114142092A (en) * | 2021-11-26 | 2022-03-04 | 常州赛得能源科技有限公司 | Electrolyte, electrochemical device and method for stabilizing positive electrode material |
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