CN107681147B - Preparation method and application of solid electrolyte coated modified lithium ion battery positive electrode material - Google Patents
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Abstract
The invention discloses a preparation method and application of a solid electrolyte coated modified lithium ion battery anode material, and belongs to the field of lithium ion battery electrode materials. The method comprises the following steps: (1) under certain conditions, dispersing an aluminum source and a lithium source in an organic solvent, and then dropwise adding a proper amount of a proper stabilizer to obtain aluminum metalithiate sol; (2) adding a proper amount of the positive electrode material into the sol, transferring the sol to the inner liner of a polytetrafluoroethylene reaction kettle, and directly using a solvothermal method to obtain a precursor of the solid electrolyte coated modified positive electrode material; (3) the prepared precursor of the solid electrolyte coated modified cathode material is calcined to obtain the compact, uniform and stable ultrathin solid electrolyte coated modified lithium ion battery cathode material which has good cycle stability, excellent rate capability and reliable safety, and the preparation method has the characteristics of low cost, simple operation, environmental friendliness and the like, and can be applied to industrial production on a large scale.
Description
Technical Field
The invention belongs to the technical field of energy storage and modification conversion, and mainly relates to application of a solid electrolyte coated modified lithium ion battery anode material and a preparation method thereof.
Background
The lithium ion battery is a novel chemical power source developed in recent years, is a hotspot for research and development of countries in the world, has the characteristics of small volume, light weight, high specific energy, no memory effect, long cycle life and the like, and is widely applied to the fields of mobile equipment, electric automobile energy sources and the like. In each component of a lithium ion battery, the electrode material is the core and key material of the lithium ion battery. The quality of the electrode material directly determines multiple key performances of the lithium ion battery, such as specific energy, cycle life, load resistance and the like. Therefore, the development of a lithium ion battery cathode material with high performance and long cycle life becomes a common target of researchers all over the world, and has great significance for improving the performance of the lithium ion battery, especially for developing a power lithium ion battery.
The coating modification is a protection method for forming a uniform coating layer on the surface of target material particles by adopting a material with excellent physical and chemical properties. Researchers coat the anode material with the solid electrolyte, and the results show that the anode material coated and modified by the solid electrolyte has higher capacity, good rate performance and excellent cycle performance.
The existing preparation method of the coating modified lithium ion battery anode material mainly comprises a high-energy ball milling method, a sol-gel method and the like, for example, Chinese patent CN101950803A, which has the problems of rough coating effect, difficult control of ultrathin coating and the like, and although the service life of the anode material is prolonged, the capacity and the rate capability of the anode material are limited. Therefore, the preparation method which has the advantages of effectiveness, simple operation, low cost and environmental friendliness is imperative to be found.
Disclosure of Invention
Aiming at the technical problems to be solved at present, the invention overcomes the defects of the anode material of the lithium ion battery at present and provides an ultrathin solid electrolyte LiAlO with uniform compactness and good stability2The method for coating the modified lithium ion battery anode material has the advantages of effect, simple operation, low cost and environmental protection, and is beneficial to industrial production.
The invention aims to provide an application of a solid electrolyte coated modified lithium ion battery anode material in a lithium ion battery, which can obtain the lithium ion battery with high capacity, high rate performance, long cycle life and high safety.
Preferably, the lithium source is LiCl or LiNO3、CH3OLi、 CH3COOLi、（CH3）2CHOLi at least one of them.
In a more preferred embodiment, the aluminum source is C12H27O3Al、C9H21O3At least one of Al.
Preferred embodiment, lithium source: the molar ratio of the aluminum source (the amount of the lithium atom substance: the amount of the aluminum atom substance) is 1 to 1.2.
In a more preferred embodiment, the amount of the lithium metaaluminate substance obtained by the stoichiometric ratio is 0.2 to 0.4% of the amount of the positive electrode material substance.
Preferably, the cathode material is: ternary LiNi with layered structure1-x-yCoxMny O2（0<x+y<1) A material.
The preferable scheme is a solvothermal method, and the reaction time is 6-15 h.
In the preferable scheme, the calcination time is 2-4 h.
The invention also provides application of the solid electrolyte coated modified lithium ion battery anode material, and the solid electrolyte coated modified lithium ion battery anode material is applied to a lithium ion battery.
The method for preparing the solid electrolyte coated modified lithium ion anode material comprises the following specific steps:
(1) preparing lithium metaaluminate sol: respectively dispersing a certain amount of aluminum source, a certain amount of lithium source and a certain amount of stabilizer in a certain amount of organic solvent, and stirring for 2-4 h at room temperature.
(2) Precursor of lithium metaaluminate coated lithium ion battery anode material: and (3) transferring a certain amount of the positive electrode material and the sol into a polytetrafluoroethylene reaction kettle, preserving the temperature for 6-15 hours at the temperature of 120-180 ℃, carrying out suction filtration on the obtained product, washing, putting the product into a blast drying oven, and drying for 2-4 hours at the temperature of 80 ℃ to obtain the precursor of the lithium metaaluminate coated lithium ion battery positive electrode material.
(3) And (3) placing the precursor prepared in the step (2) in a ceramic crucible, calcining for 2-4 h at the temperature of 400-500 ℃, and naturally cooling to room temperature to obtain the lithium metaaluminate coated lithium ion battery anode material.
The invention further discloses the application of the solid electrolyte coated modified lithium ion battery anode material in the preparation of lithium ionsApplication in batteries. The method comprises the following steps: grinding and fully mixing a solid electrolyte coated modified lithium ion positive electrode material, conductive carbon black (conductive agent), polyvinylidene fluoride (PVDF binder) and a small amount of N-methylpyrrolidone (NMP) to form uniform paste, coating the paste on an aluminum foil substrate to be used as a test electrode, wherein the electrolyte is 1M LiPF6EC: DMC (V: V =1: 1), and button cell was made with metallic lithium as the counter electrode. The experimental results show that: solid electrolyte LiAlO2Coated positive electrode material LiNi0.6Co0.2Mn0.2O2After 350 times of charge-discharge tests, the capacity can still reach 149 mA h/g
The technical scheme includes that a certain amount of aluminum source, a certain amount of lithium source and a certain amount of stabilizer are dispersed in a certain amount of organic solvent, stirring is carried out at room temperature for 2-4 hours to generate lithium metaaluminate sol, and the lithium metaaluminate sol is uniformly adsorbed on the surface of a positive electrode material through a solvothermal method to form a layer of ultrathin LiAl (OH)4Coating layer of LiAl (OH)4Further dehydrating at high temperature to produce LiAlO2。
The invention mainly researches the solid electrolyte LiAlO2Coating positive electrode material LiNi0.6Co0.2Mn0.2O2The preparation method and the application mainly solve the problems of short cycle life and poor rate capability of the existing lithium ion battery.
The coating layer in the lithium ion battery anode material coated by the fast ion conductor prepared by the technical scheme of the invention is compact and uniform, has good stability, can effectively prevent the corrosion of electrolyte to the anode material in the charge-discharge cycle process of the lithium ion battery, greatly prolongs the cycle life of the lithium ion battery, promotes the lithium ion transmission function, and improves the electrochemical performance of the lithium ion battery.
The method for preparing the solid electrolyte coated lithium ion battery anode material fully utilizes the reaction of an aluminum source and a lithium source in an organic solvent to generate the lithium metaaluminate sol, and the sol has better adsorption performance and can be decomposed at high temperature to generate LiAlO2The principle of (1). An ultrathin, compact, uniform and stable solid electrolyte coating layer is formed on the surface of the anode material and can be provided withEffectively prevents the direct contact of the anode active substance and the electrolyte solution, thereby inhibiting the side reaction of the electrode material and the electrolyte, reducing the dissolution loss of the anode active substance, greatly prolonging the cycle life of the battery, simultaneously greatly improving the electronic and lithium ion conductivity of the electrode and improving the electrochemical performance of the lithium ion battery.
The lithium ion battery anode material coated and modified by the solid electrolyte is prepared by sol-solvent heat-assisted synthesis and combining a high-temperature sintering method, and the method has the advantages of low raw material cost, simplicity in operation and environmental friendliness, and overcomes the defects of high raw material cost, rough coating effect, poor controllability and the like in the traditional solid electrolyte coating and modifying method.
The method for coating the modified lithium ion battery anode material with the solid electrolyte provided by the invention has the advantages that the coating raw material is activated more fully by a solvent thermal-assisted method, the utilization rate of the raw material is improved, the process is simplified, and the conditions are mild.
The ultrathin solid electrolyte coating modified lithium ion battery cathode material prepared by the invention is applied to a lithium ion battery, has higher capacity, good rate performance and excellent cycle performance, and greatly prolongs the cycle life of the lithium ion battery.
Drawings
FIG. 1 is LiAlO in the examples2LiNi before and after coating modification0.6Co0.2Mn0.2O2Scanning electron microscope images of the anode material;
FIG. 2 is LiAlO in the examples2LiNi before and after coating modification0.6Co0.2Mn0.2O2XPS full spectrum of positive pole material;
FIG. 3 is LiAlO in the examples2Coating modified LiNi0.6Co0.2Mn0.2O2A high-resolution scanning transmission electron microscope image of the anode material;
FIG. 4 is a LiNi which has not been modified by coating0.6Co0.2Mn0.2O2Positive electrode material and coating-modified LiNi prepared in examples0.6Co0.2Mn0.2O2And (3) a curve diagram of the sub-cycle performance of the anode material.
Detailed Description
The invention is described below by means of specific embodiments. Unless otherwise specified, the technical means used in the present invention are well known to those skilled in the art. In addition, the embodiments should be considered illustrative, and not restrictive, of the scope of the invention, which is defined solely by the claims. It will be apparent to those skilled in the art that various changes or modifications in the components and amounts of the materials used in these embodiments can be made without departing from the spirit and scope of the invention. The raw materials and reagents used in the present invention are commercially available.
Example 1
(1) C is to be9H21O3Al and CH3OLi is dispersed in ethanol, then proper amount of proper stabilizer (the volume ratio of the stabilizer to the ethanol is 3: 2000) is dripped, and lithium metaaluminate sol is obtained after stirring for 1 hour;
(2) 0.3 g of LiNi serving as a positive electrode material was taken0.6Co0.2Mn0.2O2Adding the sol, transferring to the inner liner of a polytetrafluoroethylene reaction kettle, stirring for 1-2 h, and directly preserving the heat for 15h at 120-180 ℃ by using a solvothermal method to obtain a precursor of the solid electrolyte coated modified cathode material;
(3) filtering the product obtained in the step (2), washing the product for 3 times by using absolute ethyl alcohol, and then keeping the temperature of a filter cake in a forced air drying box at 80 ℃ for 3 hours to obtain LiAlO2Coating the precursor of the anode material;
(4) calcining the prepared precursor of the solid electrolyte coated modified positive electrode material at the temperature of 500 ℃ for 4h to obtain the solid electrolyte coated modified positive electrode material of the lithium ion battery;
(5) 0.68g of LiAlO obtained as described above was weighed2Coating-modified LiNi0.6Co0.2Mn0.2O2Adding 0.08g of conductive carbon black as a conductive agent and 0.08g of PVDF as a binder into the positive electrode material, dropwise adding a small amount of NMP, grinding and uniformly mixing to form uniform paste, coating the paste on an aluminum foil to be used as a test electrode, and using 1M LiPF6EC: DMC (V: V =1: 1), and charging and discharging performance (current density of 50 mAh/g) was tested;
the coating-modified LiNi prepared in this example was used0.6Co0.2Mn0.2O2The material characteristics and electrochemical properties of the cathode material are shown in the following chart:
FIG. 1 is a scanning electron micrograph from which it can be seen that LiNi has not been subjected to coating modification0.6Co0.2Mn0.2O2The anode material has a sphere-like structure consisting of primary particles with the size of 500-800nm, and the surface is smooth. Passing through a solid electrolyte (LiAlO)2) Coating modified LiNi0.6Co0.2Mn0.2O2The surface of the anode material particle is provided with a coating layer which is uniformly distributed, and the surface is rough.
FIG. 2 is an XPS survey, from which LiNi can be seen0.6Co0.2Mn0.2O2The anode material passes through a solid electrolyte (LiAlO)2) After coating modification, the surface is well coated by the solid electrolyte.
FIG. 3 is a solid electrolyte (LiAlO)2) Coated and modified LiNi0.6Co0.2Mn0.2O2High resolution transmission electron microscopy of positive electrode material indicating solid state electrolyte (LiAlO)2) The surface of the anode material is coated with the anode material in an ultrathin, compact and uniform manner.
FIG. 4 is LiNi before coating modification0.6Co0.2Mn0.2O2Positive electrode material and coating-modified LiNi0.6Co0.2Mn0.2O2Long cycle performance plot of the positive electrode material, indicating the use of solid state electrolyte (LiAlO)2) Coating modified LiNi0.6Co0.2Mn0.2O2The electrode made of the anode material has the specific capacity of 149 mA h/g after circulating for 350 times and shows good circulating performance when discharging at constant current under the current density of 50mAh/g and the voltage of 4.5V at room temperature.
Example 2
(1) C is to be12H27O3Al and CH3OLi is dispersed in ethanol, then proper amount of proper stabilizer (the volume ratio of the stabilizer to the ethanol is 3: 2000) is dripped, and lithium metaaluminate sol is obtained after stirring for 1 hour;
(2) 0.3 g of LiNi serving as a positive electrode material was taken0.5Co0.2Mn0.3O2Adding the sol, transferring to the inner liner of a polytetrafluoroethylene reaction kettle, stirring for 1-2 h, and directly preserving the heat for 15h at 120-180 ℃ by using a solvothermal method to obtain a precursor of the solid electrolyte coated modified cathode material;
(3) filtering the product obtained in the step (2), washing the product for 3 times by using absolute ethyl alcohol, and then keeping the temperature of a filter cake in a forced air drying oven at 80 ℃ for 4 hours to obtain LiAlO2Coating the precursor of the anode material;
(4) calcining the prepared precursor of the solid electrolyte coated modified positive electrode material at the temperature of 500 ℃ for 4h to obtain the solid electrolyte coated modified positive electrode material of the lithium ion battery;
(5) 0.68g of LiAlO obtained as described above was weighed2Coating-modified LiNi0.5Co0.2Mn0.3O2Adding 0.08g of conductive carbon black as a conductive agent and 0.08g of PVDF as a binder into a positive electrode material, dropwise adding a small amount of NMP, grinding and uniformly mixing to form uniform paste, coating the paste on an aluminum foil to be used as a test electrode, and using 1M LiPF6EC: DMC (V: V =1: 1), and charging and discharging performance (current density of 50 mAh/g) was tested;
LiAlO prepared by the present example2Coating modified LiNi0.5Co0.2Mn0.3O2The positive electrode material is used for preparing an electrode and is assembled with a metal lithium sheet into a button cell, when the button cell is subjected to constant current discharge at room temperature, the specific capacity can still be kept at 175 mA h/g after the button cell is cycled for 100 times, the voltage is kept at 4.5V, and good cycle performance is shown.
Example 3
(1) C is to be9H21O3Al and (CH)3）2CHOLi is dispersed in ethanol, then proper amount of proper stabilizer (the volume ratio of the stabilizer to the ethanol is 3: 2000) is added dropwise, and lithium metaaluminate sol is obtained after stirring for 1 h;
(2) get0.3 g of LiNi, a positive electrode material0.33Co0.33Mn0.33O2Adding the sol, transferring to the inner liner of a polytetrafluoroethylene reaction kettle, stirring for 1-2 h, and directly preserving the heat for 15h at 120-180 ℃ by using a solvothermal method to obtain a precursor of the solid electrolyte coated modified cathode material;
(3) filtering the product obtained in the step (2), washing the product for 3 times by using absolute ethyl alcohol, and then keeping the temperature of a filter cake in a forced air drying oven at 80 ℃ for 2-4 h to obtain LiAlO2Coating the precursor of the anode material;
(4) calcining the prepared precursor of the solid electrolyte coated modified positive electrode material at the temperature of 500 ℃ for 4h to obtain the solid electrolyte coated modified positive electrode material of the lithium ion battery;
(5) 0.68g of LiAlO obtained as described above was weighed2Coating-modified LiNi0.33Co0.33Mn0.33O2Adding 0.08g of conductive carbon black as a conductive agent and 0.08g of PVDF as a binder into a positive electrode material, dropwise adding a small amount of NMP, grinding and uniformly mixing to form uniform paste, coating the paste on an aluminum foil to be used as a test electrode, and using 1M LiPF6EC: DMC (V: V =1: 1), and charging and discharging performance (current density of 50 mAh/g) was tested;
LiAlO prepared by the present example2Coating modified LiNi0.33Co0.33Mn0.33O2The positive electrode material is used for preparing an electrode and is assembled with a metal lithium sheet into a button cell, when the button cell is subjected to constant current discharge at room temperature, the specific capacity can still be kept at 147 mA h/g after the button cell is cycled for 100 times, the voltage is kept at 4.5V, and good cycle performance is shown.
Claims (7)
1. A preparation method of a solid electrolyte coated modified lithium ion battery anode material is characterized by comprising the following steps:
(1) dispersing an aluminum source and a lithium source in an organic solvent, then dropwise adding a proper amount of a proper stabilizer, and stirring for 1-2 h to obtain a lithium metaaluminate sol;
(2) adding 0.3-2 g of the positive electrode material into the sol, transferring the sol to the inner liner of a polytetrafluoroethylene reaction kettle, stirring for 1-2 hours, and directly preserving heat for 6-15 hours at 120-180 ℃ by using a solvothermal method to obtain a first precursor of the solid electrolyte coated modified positive electrode material;
(3) filtering the product obtained in the step (2), washing the product for 3 times by using absolute ethyl alcohol, and then keeping the temperature of a filter cake in a forced air drying oven at 80 ℃ for 2-4 h to obtain a second precursor of the solid electrolyte coated modified cathode material;
(4) calcining the prepared second precursor of the solid electrolyte coated modified cathode material for 4 hours at the temperature of 400-500 ℃ to obtain the solid electrolyte coated modified lithium ion battery cathode material, wherein the thickness of the lithium metaaluminate coating layer is 0.5-2 nanometers;
the stabilizer refers to ethyl acetoacetate;
an aluminum source: the molar ratio of the lithium source is 1: 1; a stabilizer: the volume ratio of the organic solvent is 3: 2000;
the anode material is as follows: ternary LiNi with layered structure1-x-yCoxMny O2，0<x+y<1 material.
2. The method of claim 1, wherein: the thickness of the lithium metaaluminate coating layer is 0.5-2 nanometers, and the amount of the lithium metaaluminate substance is 0.20-0.40% of that of the anode material substance; the organic solvent is selected from one of ethanol and glycol.
3. The method of claim 1, wherein: the lithium source is LiCl or LiNO3、CH3OLi、 CH3COOLi or (CH)3）2CHOLi。
4. The method of claim 1, wherein: the aluminum source is C12H27O3Al or C9H21O3Al。
5. The method of claim 1, wherein: the reaction time of the solvothermal method is 6-15 h.
6. The method of claim 1, wherein: the calcination time is 2-4 h.
7. The application of the solid electrolyte coated modified lithium ion battery cathode material prepared by the method of claim 1 in preparing a lithium ion battery.
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| CN110137470A (en) * | 2019-05-15 | 2019-08-16 | 华南理工大学 | A kind of method of fluorine-based ionic liquid surface modification ternary cathode material of lithium ion battery |
| CN110581272B (en) * | 2019-09-30 | 2022-05-10 | 昆明云大新能源有限公司 | High-performance ternary cathode material for lithium ion battery and preparation method of ternary cathode material |
| CN110668507A (en) * | 2019-09-30 | 2020-01-10 | 湖北万润新能源科技发展有限公司 | Preparation method of ternary cathode material of lithium-rich manganese-based coating layer |
| CN112054194B (en) * | 2020-08-07 | 2021-12-17 | 西安理工大学 | Phosphorus-modified lithium ion battery positive electrode material and preparation method and application thereof |
| CN115425214B (en) * | 2022-09-29 | 2024-04-19 | 合肥国轩高科动力能源有限公司 | Coating modified high-nickel ternary positive electrode material, preparation method and application thereof |
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