CN111697265A - LNCM manganese ternary lithium ion battery electrolyte, lithium battery and preparation method thereof - Google Patents
LNCM manganese ternary lithium ion battery electrolyte, lithium battery and preparation method thereof 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
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- 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
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Abstract
The invention provides an LNCM manganese ternary lithium ion battery electrolyte, a lithium battery and a preparation method thereof. The electrolyte comprises the following preparation raw materials: the electrolyte additive comprises an electrolyte additive, lithium salt and a solvent, wherein the electrolyte additive accounts for 1-10 wt% of the electrolyte of the battery, and the electrolyte additive is a mixture of vinylene carbonate, fluoroethylene carbonate and trimethyl borate. In the electrolyte, EC with high dielectric constant and DEC and EMC with low viscosity are mixed for use, and the requirements of the electrolyte in various aspects such as working temperature range, conductivity and the like are met. The working temperature range of the electrolyte is widened by reducing the content of the high-melting point solvent EC (melting point 35-38 ℃) and increasing the content of the low-melting point cosolvent DEC (melting point-43 ℃) and EMC (melting point-55 ℃).
Description
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to an LNCM manganese ternary lithium ion battery electrolyte, a lithium battery and a preparation method thereof.
Background
The lithium ion battery has the advantages of high energy density, good cycle performance, long storage time, small self-discharge and the like, is widely applied to the fields of 3C electronic products, portable electronic equipment, electric automobiles and aerospace, and is expected to gradually replace traditional energy storage devices, such as lead-acid batteries, nickel-cadmium batteries and nickel-hydrogen batteries. The lithium ion battery mainly comprises a positive electrode material, a negative electrode material, electrolyte and a diaphragm. Currently, many positive electrode materials including manganese-based, nickel-based, cobalt-based, and vanadium-based materials are being studied.
For developing a new generation of high-performance lithium ion battery system, one of the effective approaches is to adopt a high-voltage positive electrode and a high-capacity negative electrode material and develop a high-voltage electrolyte and a high-performance diaphragm matched with the high-voltage positive electrode and the high-capacity negative electrode material, and the battery system is called as a high-voltage lithium ion battery for short.
For positive electrode materials, LiNi1/3Co1/3Mn1/3O2The material (LNCM for short) belongs to manganese ternary anode material, and has the advantages of low cost, low toxicity, high thermal stability and wide voltage range. In view of cost and existing battery preparation process, the liquid electrolyte composed of carbonate organic solvent and lithium hexafluorophosphate (LiPF 6) will be the first choice for power battery in recent years, but the conventional electrolyte is easy to be oxidized and separated under high voltageThe solution generates acid, and further, the dissolution of transition metal Mn, the cracking of material crystals and the phase change of the material can be caused, so that the LNCM positive electrode material has serious capacity attenuation, poor cycle performance and low conductivity and rate performance.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides an LNCM manganese series ternary lithium ion battery electrolyte, a lithium battery and a preparation method thereof.
According to the embodiment of the first aspect of the invention, the preparation raw materials of the electrolyte of the LNCM manganese ternary lithium ion battery comprise: the electrolyte additive comprises an electrolyte additive, lithium salt and a solvent, wherein the electrolyte additive accounts for 1-10 wt% of the electrolyte of the battery, and the electrolyte additive is a mixture of vinylene carbonate, fluoroethylene carbonate and trimethyl borate.
According to some embodiments of the present invention, in the electrolyte additive, a mass ratio of Vinylene Carbonate (VC), fluoroethylene carbonate (FEC) and Trimethyl Borate (TB) is (1 to 3): (1-3): 1.
according to some embodiments of the invention, in the electrolyte additive, the mass ratio of VC, FEC and TB is 1: 1: 1.
the structural formula of Trimethyl Borate (TB) is shown as the formula:
the Trimethyl Borate (TB) can form a stable electron-deficient bond due to the three valence atoms on the p orbital of the B atom, namely, the B atom presents Lewis acidity, can be combined with PF 6-in LiPF6, and improves the dissociation degree of LiPF6 in the electrolyte, namely, improves the dissociation degree of free Li+The concentration of the electrolyte solution is reduced, so that the conductivity of the electrolyte solution is improved, the LiPF6 is inhibited from being decomposed to generate HF, the side reaction between the LNCM manganese series ternary positive electrode material and the electrolyte solution is greatly reduced, and a battery system is stabilized.
Vinylene Carbonate (VC) is an organic film-forming additive and an overcharge protection additive, has good high-low temperature performance and an anti-ballooning function, and can improve the capacity and the cycle life of the battery. Fluoroethylene carbonate (FEC) is a commonly used film forming additive, and the molecules of fluoroethylene carbonate (FEC) have 1-F bond more than Ethylene Carbonate (EC), so that the fluoroethylene carbonate (FEC) has higher electronegativity and stronger electron-withdrawing capability, has stronger oxidation resistance, prevents the decomposition of electrolyte, further prevents the decomposition of trace water and HF, inhibits more gases, and improves the low-temperature performance and cycle life of the electrolyte. Trimethyl Borate (TB) can be preferentially oxidized based on the electrolyte, a stable thin low-impedance film is formed on the surface of the LNCM positive electrode material, the low-impedance film can inhibit the decomposition of the electrolyte and the dissolution of transition metal ions in the LNCM, and the cycle stability and the rate capability of the battery are improved. The combination and matching of Vinylene Carbonate (VC), fluoroethylene carbonate (FEC) and Trimethyl Borate (TB) realize the efficacy synergy.
According to some embodiments of the invention, the lithium salt is present in the battery electrolyte in an amount of 5 to 20 wt%.
According to some embodiments of the invention, the proportion of the lithium salt in the battery electrolyte is preferably 12 wt%.
According to some embodiments of the invention, the lithium salt is lithium hexafluorophosphate.
According to some embodiments of the invention, the solvent is 70 to 90 wt% in the battery electrolyte.
According to some embodiments of the invention, the solvent is preferably present in the battery electrolyte in a proportion of 85 wt%.
According to some embodiments of the invention, the solvent is a mixture of diethyl carbonate (DEC), Ethyl Methyl Carbonate (EMC) and Ethylene Carbonate (EC).
According to some embodiments of the invention, the mass ratio of diethyl carbonate (DEC), Ethyl Methyl Carbonate (EMC) and Ethylene Carbonate (EC) is 5:5: 7.
Ethylene Carbonate (EC) is a cyclic carbonate having a high dielectric constant, but also having a large viscosity; diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) are chain carbonates and have low viscosity, but also low dielectric constant. EC with high dielectric constant and DEC and EMC with low viscosity are mixed for use, and the requirements of the electrolyte in various aspects such as working temperature range, conductivity and the like can be met.
The working temperature range of the electrolyte can be widened by reducing the content of the high-melting point solvent EC (melting point 35-38 ℃) and increasing the content of the low-melting point cosolvent DEC (melting point-43 ℃) and EMC (melting point-55 ℃). Specifically, the working temperature range of the current commercially available electrolyte is-30-60 ℃, and the working temperature range of the electrolyte in the embodiment of the invention is-40-80 ℃.
The preparation method of the LNCM manganese series ternary lithium ion battery electrolyte according to the embodiment of the second aspect of the invention comprises the following steps:
s1: controlling the temperature and pressure, and adding the lithium salt into a solvent;
s2: and (4) sequentially adding vinylene carbonate, fluoroethylene carbonate and trimethyl borate into the product obtained in the step S1 to obtain the catalyst.
According to some embodiments of the invention, in step S1, the temperature is less than 2 ℃.
According to some embodiments of the present invention, a method for preparing an LNCM manganese-based ternary lithium ion battery electrolyte comprises the following steps:
(1) material melting: the melting points of different solvents are different, and the melting point of EC is 36-38 ℃, so that the melting point is higher, the melting material is needed to be firstly carried out during operation, and the melting material process comprises the following steps: melting EC at 60-70 deg.C for 5-7 h;
(2) material suction: the prepared raw materials are pumped into a raw material tank by pressure difference, at the moment, the pressure of a raw material barrel is in micro-positive pressure, the pressure of the raw material tank is-0.1 Mpa, and the raw materials are transferred into the raw material tank under the protection of nitrogen;
(3) material passing: adding the pressure of a raw material tank to 0.1-0.15 Mpa, controlling the opening degree of valves of all pipelines, slowly pumping the raw material from the raw material tank to the purification equipment, performing purification treatment, and pumping the raw material to the high-purity raw material tank, wherein the pressures of the purification equipment and the high-purity raw material tank are both 0.02 Mpa;
(4) preparing materials: according to the melting point of the raw materials, the feeding sequence is strictly controlled as follows: EMC, DEC and EC, during the batching, the pressure of a high-purity raw material tank is adjusted to 0.15 Mpa, the pressure of a metering kettle is 0.03 Mpa, and the mass of 3 solvents is accurately metered by an electronic scale;
(5) adding lithium salt: reducing the temperature of the stirring kettle to below 2 ℃ by using a refrigerator and a circulating pump, adjusting the pressure of the stirring kettle to 0.02Mpa, adjusting the pressure of the measuring kettle to 0.15 Mpa for transferring materials, adding proper LiPF6 by using a glove box, and controlling the temperature of the stirring kettle within 2 ℃ all the time in the process of adding;
(6) adding an additive: the added additives comprise Vinylene Carbonate (VC), fluoroethylene carbonate (FEC) and Trimethyl Borate (TB) with specific mass fractions;
(7) and (3) filtering and packaging: and transferring the qualified electrolyte to a finished product barrel through a filter, and adjusting the pressure of the stirring kettle to 0.5bar (0.05 MPa) and the pressure of a finished product tank to 0.02MPa when transferring materials.
According to a third aspect of the embodiment of the invention, the lithium battery comprises the LNCM manganese-based ternary lithium ion battery electrolyte.
Detailed Description
The following are specific examples of the present invention, and the technical solutions of the present invention will be further described with reference to the examples, but the present invention is not limited to the examples.
Example 1
The embodiment provides an LNCM manganese ternary lithium ion battery electrolyte, which comprises the following preparation raw materials: the electrolyte additive comprises an electrolyte additive, lithium salt and a solvent, wherein the electrolyte additive accounts for 1-10 wt% of the electrolyte of the battery, and the electrolyte additive is a mixture of vinylene carbonate, fluoroethylene carbonate and trimethyl borate.
In the electrolyte additive, the mass ratio of Vinylene Carbonate (VC), fluoroethylene carbonate (FEC) and Trimethyl Borate (TB) is (1-3): (1-3): 1. preferably 1: 1: 1.
the proportion of the lithium salt in the battery electrolyte is 5-20 wt%, preferably 12 wt%. The lithium salt is lithium hexafluorophosphate.
The proportion of the solvent in the battery electrolyte is 70-90 wt%, preferably 85 wt%. The solvent is a mixture of diethyl carbonate (DEC), Ethyl Methyl Carbonate (EMC) and Ethylene Carbonate (EC), and the mass ratio of the diethyl carbonate (DEC), the Ethyl Methyl Carbonate (EMC) and the Ethylene Carbonate (EC) is 5:5: 7.
Example 2
The embodiment provides a preparation method of an LNCM manganese series ternary lithium ion battery electrolyte, which comprises the following steps:
s1: controlling the temperature and pressure, and adding the lithium salt into a solvent;
s2: and (4) sequentially adding vinylene carbonate, fluoroethylene carbonate and trimethyl borate into the product obtained in the step S1 to obtain the catalyst.
In step S1, the temperature is less than 2 ℃.
The preparation method specifically comprises the following steps:
(1) material melting: the melting points of different solvents are different, and the melting point of EC is 36-38 ℃, so that the melting point is higher, the melting material is needed to be firstly carried out during operation, and the melting material process comprises the following steps: melting EC at 60-70 deg.C for 5-7 h;
(2) material suction: the prepared raw materials are pumped into a raw material tank by pressure difference, at the moment, the pressure of a raw material barrel is in micro-positive pressure, the pressure of the raw material tank is-0.1 Mpa, and the raw materials are transferred into the raw material tank under the protection of nitrogen;
(3) material passing: adding the pressure of a raw material tank to 0.1-0.15 Mpa, controlling the opening degree of valves of all pipelines, slowly pumping the raw material from the raw material tank to the purification equipment, performing purification treatment, and pumping the raw material to the high-purity raw material tank, wherein the pressures of the purification equipment and the high-purity raw material tank are both 0.02 Mpa;
(4) preparing materials: according to the melting point of the raw materials, the feeding sequence is strictly controlled as follows: EMC, DEC and EC, during the batching, the pressure of a high-purity raw material tank is adjusted to 0.15 Mpa, the pressure of a metering kettle is 0.03 Mpa, and the mass of 3 solvents is accurately metered by an electronic scale;
(5) adding lithium salt: reducing the temperature of the stirring kettle to below 2 ℃ by using a refrigerator and a circulating pump, adjusting the pressure of the stirring kettle to 0.02Mpa, adjusting the pressure of the measuring kettle to 0.15 Mpa for transferring materials, adding proper LiPF6 by using a glove box, and controlling the temperature of the stirring kettle within 2 ℃ all the time in the process of adding;
(6) adding an additive: the added additives comprise Vinylene Carbonate (VC), fluoroethylene carbonate (FEC) and Trimethyl Borate (TB) with specific mass fractions;
(7) and (3) filtering and packaging: and transferring the qualified electrolyte to a finished product barrel through a filter, and adjusting the pressure of the stirring kettle to 0.5bar (0.05 MPa) and the pressure of a finished product tank to 0.02MPa when transferring materials.
Example 3
The embodiment provides a lithium battery which comprises the LNCM manganese series ternary lithium ion battery electrolyte.
Example 4
In this example, three electrolytes, numbered a to C, were prepared according to the preparation method of example 2 and the formulation of example 1, and the specific formulation is shown in table 1.
TABLE 1 details of the three electrolyte compositions
Comparative example
In this example, referring to the mixture ratio of the electrolyte A in example 4, four comparative electrolytes, which are numbered A1-A4, were prepared, and the specific mixture ratio is shown in Table 2.
TABLE 2 details of the four comparative electrolyte formulations
Example of detection
The 2000 mAh 18650 battery system and the 5 Ah soft package battery system are adopted to test the charging and discharging and circulating performances of the electrolytes A to C and A1 to A4, and the capacity retention rates under different conditions are shown in tables 3 and 4.
TABLE 318650 Battery System Performance test results%
TABLE 4 Soft pouch cell System Performance test results%
The electrolyte A1 increases the content of cyclic carbonate EC, reduces the content of chain carbonate DEC and EMC, and increases the viscosity of the electrolyte, so that the conductivity of the electrolyte is reduced, and the rate capability is reduced.
The electrolyte a2 increased the DEC content and decreased the EC content, while EC having a high dielectric constant was able to form an SEI film on the negative electrode without additives, contributing to the improvement of the cycle performance of the battery, and thus the cycle performance of the battery was decreased in this comparative example.
Electrolyte A3 is not added with TB, which can protect the surface of the manganese ternary cathode material in the charge-discharge cycle process, and the rate capability and cycle performance of the battery are improved by improving the interface stability between the electrode and the electrolyte. Therefore, in this comparative example, the battery was greatly deteriorated in each performance.
The electrolyte A4 is not added with FEC, the FEC participates in film formation on the surface of the negative electrode, the decomposition of trace water and HF can be prevented, more gases are inhibited, the electrolyte is prevented from being further decomposed, meanwhile, the impedance is not increased, and the cycle life of the electrolyte is prolonged. This comparative example had no FEC added and the cell cycle performance was reduced.
Claims (10)
1. The electrolyte of the LNCM-series ternary lithium ion battery is characterized by comprising the following preparation raw materials: the electrolyte additive comprises an electrolyte additive, lithium salt and a solvent, wherein the electrolyte additive accounts for 1-10 wt% of the electrolyte of the battery, and the electrolyte additive is a mixture of vinylene carbonate, fluoroethylene carbonate and trimethyl borate.
2. An LNCM manganese ternary lithium ion battery electrolyte as claimed in claim 1, wherein in said electrolyte additive, the mass ratio of vinylene carbonate, fluoroethylene carbonate and trimethyl borate is (1-3): (1-3): 1.
3. an LNCM manganese ternary lithium ion battery electrolyte as claimed in claim 2, wherein the electrolyte additive is characterized in that the mass ratio of vinylene carbonate, fluoroethylene carbonate and trimethyl borate is 1: 1: 1.
4. an LNCM-based ternary lithium ion battery electrolyte according to claim 1, wherein the proportion of said lithium salt in the battery electrolyte is 5-20 wt%.
5. An LNCM manganese-based ternary lithium ion battery electrolyte according to claim 1 or 4, characterized in that said lithium salt is lithium hexafluorophosphate.
6. An LNCM manganese series ternary lithium ion battery electrolyte as claimed in claim 1, wherein the solvent is 70-90 wt% in the battery electrolyte.
7. An LNCM manganese ternary lithium ion battery electrolyte according to claim 1 or 6, characterized in that said solvent is a mixture of diethyl carbonate, ethyl methyl carbonate and ethylene carbonate.
8. The preparation method of the LNCM manganese series ternary lithium ion battery electrolyte as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
s1: controlling the temperature and pressure, and adding the lithium salt into a solvent;
s2: and (4) sequentially adding vinylene carbonate, fluoroethylene carbonate and trimethyl borate into the product obtained in the step S1 to obtain the catalyst.
9. The method of claim 8 wherein the temperature of step S1 is less than 2 ℃.
10. A lithium battery comprising the LNCM manganese-based ternary lithium ion battery electrolyte according to any one of claims 1 to 7.
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Application publication date: 20200922 |
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