CN114142022A - Micron-sized carbon-coated optimized mono-like anode material and application thereof - Google Patents
Micron-sized carbon-coated optimized mono-like anode material and application thereof Download PDFInfo
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- 239000010405 anode material Substances 0.000 title claims abstract description 68
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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Abstract
The invention belongs to the technical field related to lithium ion batteries, and particularly relates to a micron-sized carbon-based coating optimized mono-like cathode material for a lithium ion battery. The micron-sized carbon-based coated optimized mono-like anode material consists of a mono-like anode material and micron-sized graphene sheets; the micron-sized graphene sheet material is tightly coated on the surface of the positive electrode material with the single crystal-like appearance. According to the invention, the coating amount and thickness of the graphene sheet are controlled, the impedance of the battery material is reduced, and the cycle capacity retention rate at 45 ℃ and the high-rate discharge capacity retention rate are improved; the micron-sized carbon-coated optimized mono-like anode material has the advantages of good conductivity, high power density of the battery, high charging and discharging speed, small using amount of conductive materials, high tap density, capacity of preparing a large-capacity battery, prolonged service life of the battery and capability of meeting the requirement of large-scale production.
Description
Technical Field
The invention belongs to the technical field related to lithium ion batteries, and particularly relates to a micron-sized carbon-coated optimized mono-like anode material and application thereof.
Background
With the development of the preparation technology of the lithium ion battery and the related materials thereof in recent years, the lithium ion battery undoubtedly replaces the nickel-hydrogen battery, the lead-acid battery and the like to become a new generation power supply with high technological content and the most extensive application, has the advantages of environmental protection, high energy density, good cycle performance, good safety performance and the like, is called as the most promising chemical power supply, and has become one of the most rapid and active areas of the global lithium ion battery in China. The positive electrode material of the lithium ion battery is one of the key factors determining the performance of the battery, and therefore, under the current situation, the development of the positive electrode material of the lithium ion battery with good thermal safety performance and cycle stability performance is urgent.
The single-crystal-like positive electrode material has the characteristics of high energy density, high multiplying power and the like of the single-crystal-like positive electrode material and is widely used, but the multiplying power performance, the cycle performance and the like of the single-crystal-like positive electrode material have a great space for improvement. The carbon material has good performance and strong corrosion resistance, and is very suitable for being used as a coating material to carry out surface modification on the lithium ion anode material. The positive electrode material is at a high potential at the final stage of charging and has strong oxidizing property, so that a certain degree of oxygen loss reaction occurs in the positive electrode material, stable carbon substances such as graphene are coated on the surface of the positive electrode material, an effective means for reducing the oxygen loss reaction is provided, and meanwhile, the conductivity is improved, so that proper coating is required. According to the invention, graphene with the sheet diameter of micron order is used for coating the monocrystal-like positive electrode material, so that the performance of the monocrystal-like positive electrode material can be effectively optimized.
Disclosure of Invention
In order to solve the technical problems, the invention provides a micron-sized carbon-based coating optimized single-crystal-like cathode material, which consists of a single-crystal-like cathode material and nano-scale graphene sheets; the graphene sheet material is tightly coated on the surface of the positive electrode material with the single crystal-like appearance.
As a preferable technical scheme, the positive electrode material with the single crystal-like morphology is selected from LiCoO2、LiNixCoyMnzO2、LiNixCoyAlzO2One or more of; the LiNixCoyMnzO2Or LiNixCoyAlzO2Wherein x + y + z is 1, x is more than or equal to 0.2 and less than or equal to 0.95, y is more than or equal to 0.05 and less than or equal to 0.4, and z is more than or equal to 0.05 and less than or equal to 0.5; the crystal structure of the single crystal-like positive electrode material is a layered structure, the crystal structure belongs to an R-3m space group, and the positive electrode material particles are in a single crystal-like shape.
In a preferred embodiment, the graphene sheet has a sheet diameter of 1 to 20 μm.
As a preferred technical solution, the thickness of the graphene sheet is less than 10 nm.
As a preferred technical scheme, the difference between the average particle size of the micron-sized carbon-based coating optimized single-crystal-like cathode material and the average particle size of the single-crystal-like morphology cathode material is less than 1000 nm; preferably, the difference between the average particle size of the micron-sized graphene-coated single-crystal-like positive electrode material and the average particle size of the single-crystal-like positive electrode material is less than 700 nm; more preferably, the difference between the average particle size of the micron-sized carbon-based coating optimized single-crystal-like cathode material and the average particle size of the single-crystal-like morphology cathode material is less than 400 nm.
As a preferred technical scheme, in a laser raman spectrum, a D peak, a G peak, and a G 'peak of a coating region of the micron-sized carbon-based coating optimized single-crystal-like cathode material completely correspond to a D peak, a G peak, and a G' peak of a graphene sheet respectively.
As a preferred technical scheme, in an X-ray diffraction pattern, the diffraction peak positions and the relative intensity distribution orders of the micron-sized carbon-coated optimized single-crystal-like anode material and the single-crystal-like anode material are the same, and the integral deviation angle of the diffraction peaks is less than 3 degrees.
As a preferred technical scheme, a TEM image of the micron-sized carbon-based coated optimized single-crystal-like cathode material meets the requirement of figure 1; the SEM image satisfies that of FIG. 2; preferably, the included angle between the micron-sized graphene and the tangent line of the micron-sized graphene at the contact point of the mono-like morphology cathode material is less than 5 degrees; more preferably, the included angle between the micron-sized graphene and the tangent line of the micron-sized graphene at the contact point of the single crystal-like morphology cathode material is 0 °.
The invention provides a lithium ion battery electrode made of a micron-sized carbon-based coating optimized single-crystal-like anode material, and the preparation raw materials of the lithium ion battery electrode comprise the micron-sized carbon-based coating optimized single-crystal-like anode material, a conductive agent, a binder and a current collector.
Has the advantages that: the invention provides a micron-sized carbon-coated optimized mono-like positive electrode material, graphene sheets are uniformly dispersed and coated on the surface of the mono-like positive electrode material, so that on one hand, the conductivity of the material can be improved, the power density and the charging and discharging speed of a battery are improved, the using amount of a conductive material is reduced, on the other hand, the cyclic capacity retention rate of the battery can be improved, the service life of the battery is prolonged, and the capacity retention rate of a button battery corresponding to the micron-sized carbon-coated optimized mono-like positive electrode material is higher than 85% after the button battery is cycled for 200 times at 45 ℃; according to the invention, the micron-sized graphene is covered on the surface of the single-crystal-like positive electrode material, so that the prepared battery material has the advantages of smaller impedance, higher high-rate charge-discharge capacity retention rate and optimized comprehensive performance; the micron-sized carbon-coated optimized mono-like anode material has good conductivity and high tap density, can be used for preparing large-capacity batteries, and can meet the requirement of large-scale production.
Drawings
FIG. 1 is a TEM image of a micron-sized carbon-based coated optimized single-crystal-like cathode material;
FIG. 2 is an SEM image of the micron-sized carbon-based coated optimized mono-like cathode material at 20K magnification;
FIG. 3 is XRD spectra of micron-sized carbon-coated optimized mono-like anode material (I) and mono-like morphology anode material (II);
FIG. 4 is a particle size distribution diagram of a micron-sized carbon-based coating optimized mono-like anode material (a) and a mono-like morphology anode material (b);
fig. 5 is a raman image (a) of the micron-sized carbon-coated single-crystal-like cathode material and a raman spectrum (b) of the micron-sized carbon-coated single-crystal-like cathode material;
FIG. 6 is an electrochemical alternating current impedance spectrum of a mono-like morphology positive electrode material (I) and a micron-sized carbon-coated optimized mono-like positive electrode material (II);
FIG. 7 shows the 45 ℃ cycle capacity retention of the button cell described in example 1 (c) and comparative example 1 (c);
fig. 8 is the rate charge capacity retention of the button cell described in example 1 (c) and comparative example 1 (c);
fig. 9 is the rate discharge capacity retention of the button cell described in example 1 (c) and comparative example 1 (c);
FIG. 10 is a schematic structural diagram of a micron-sized carbon-based cladding optimized mono-like cathode material; wherein a is a schematic diagram that micron-sized graphene sheets are tightly coated on single-crystal-like anode material particles; b is a schematic diagram of graphene sheets attached to single-crystal-like anode material particles in a free or semi-free manner in the prior art; 1. 3 represents a graphene sheet; 2. and 4 represents the positive electrode material particles with the single-crystal-like morphology.
Detailed Description
Unless otherwise indicated, implied from the context, or customary in the art, all parts and percentages herein are by weight and the testing and characterization methods used are synchronized with the filing date of the present application. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
The technical features of the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, and the scope of protection is not limited thereto.
The words "preferred", "preferably", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention. The sources of components not mentioned in the present invention are all commercially available.
In order to solve the technical problems, the invention provides a micron-sized carbon-based coating optimized single-crystal-like cathode material, which consists of a single-crystal-like morphology cathode material and graphene sheets; the graphene sheet material is tightly coated on the surface of the positive electrode material with the single crystal-like appearance.
Single crystal-like positive electrode material
In some embodiments, the single crystal-like morphology cathode material is selected from LiCoO2、LiNixCoyMnzO2、LiNixCoyAlzO2One or more of; the LiNixCoyMnzO2Or LiNixCoyAlzO2Wherein x + y + z is 1, x is more than or equal to 0.2 and less than or equal to 0.95, y is more than or equal to 0.05 and less than or equal to 0.4, and z is more than or equal to 0.05 and less than or equal to 0.5; the crystal structure of the single crystal-like positive electrode material is a single crystal-like layered structure and belongs to an R-3m space group.
The LiNixCoyMnzO2Is nickel cobalt manganese oxide; the LiNixCoyAlzO2Is nickel cobalt aluminum oxide.
Graphene sheet
In some embodiments, the graphene sheets have a sheet diameter of 1 μm to 20 μm.
In some embodiments, the graphene sheets have a thickness of less than 10 nm.
In some embodiments, the difference between the average particle size of the micron-sized carbon-based coated optimized single crystal-like cathode material and the average particle size of the single crystal-like morphology cathode material is less than 1000 nm; preferably, the difference between the average particle size of the micron-sized carbon-based coating optimized single-crystal-like cathode material and the average particle size of the single-crystal-like morphology cathode material is less than 700 nm; more preferably, the difference between the average particle size of the micron-sized carbon-based coating optimized single-crystal-like cathode material and the average particle size of the single-crystal-like morphology cathode material is less than 400 nm.
The particle size is measured by a laser light scattering method, and is equivalent sphere volume distribution.
In some embodiments, the particle size distribution of the micron-sized carbon-based coated optimized single crystal-like cathode material is substantially the same as the particle size distribution of the single crystal-like morphology cathode material; preferably, the longest distance between the micron-sized graphene and the surface of the single crystal-like positive electrode material is less than 3 nm; more preferably, the longest distance between the micron-sized graphene and the surface of the positive electrode material with the single-crystal-like morphology is 0 nm.
The "particle size distribution is substantially the same" means that the particle size distribution of the micron-sized carbon-based coating optimized single-crystal-like cathode material is little or unchanged compared with the particle size distribution of the single-crystal-like morphology cathode material, wherein the "little" means that the absolute value of the difference of the volume densities corresponding to the same particle size is less than 1%. The grain surface of the micron-sized carbon-coated optimized mono-like anode material does not obviously increase the grain size, namely the grain size distribution results of the micron-sized carbon-coated optimized mono-like anode material and the mono-like anode material are basically consistent.
In some embodiments, in a laser raman spectrum, a D peak, a G peak, and a G 'peak of a coating region of the micron-sized carbon-based coating optimized mono-like cathode material completely correspond to a D peak, a G peak, and a G' peak of a graphene sheet respectively; the ratio of the D peak, the G peak and the G ' peak Intensity of the graphene is 0.01-10 (D)/Intensity (G), and 0.01-10 (D ')/Intensity (D '); preferably, the ratio of the D peak, the G peak and the G 'peak Intensity of the graphene is 0.01 ≦ Intensity (D)/Intensity (G) ≦ 5, 0.01 ≦ Intensity (D)/Intensity (D') ≦ 5; more preferably, the ratio of the D peak, the G peak, and the G 'peak Intensity of the graphene is 0.01. ltoreq. Intensity (D)/Intensity (G) ≦ 1, 0.01. ltoreq. Intensity (D)/Intensity (D'). ltoreq.1; the non-coating region of the micron-sized carbon-based coating optimized single-crystal-like cathode material is free of a D peak, a G peak and a G' peak.
In some embodiments, in an X-ray diffraction pattern, the positions and relative intensity distribution orders of diffraction peaks of the micron-sized carbon-based coating optimized single-crystal-like cathode material and the single-crystal-like morphology cathode material are the same, and the overall shift angle of the diffraction peaks is less than 3 °.
The invention discloses a method for improving the overall deviation of diffraction peaks, which is characterized in that when the spectrum of a micron-sized carbon-coated optimized single-crystal-like anode material is compared with the peak shape of the spectrum of the single-crystal-like anode material, the deviation phenomenon of a single peak does not exist. The micron-sized graphene is coated on the surface of the crystal grain of the single-crystal-like anode material, and the bulk structure in the crystal grain is not influenced, namely the X-ray test results of the micron-sized carbon-coated optimized single-crystal-like anode material and the single-crystal-like anode material are basically consistent.
In some embodiments, a TEM image of the micron-sized carbon-based coated optimized single crystal-like cathode material satisfies fig. 1; the SEM image of the micron-sized carbon-based coated optimized single-crystal-like cathode material meets the requirement of the attached figure 2.
In TEM and SEM images of the micron-sized carbon-based coating optimized single-crystal-like cathode material, that is, the micron-sized carbon-based coating optimized single-crystal-like cathode material shown in fig. 1 and 2, the micron-sized graphene is in a close-fitting coating state on the surface of the crystal grain of the single-crystal-like cathode material.
The micron-sized graphene is in a close-fit coating state on the surface of a crystal grain of a mono-like anode material, so that the included angle between the micron-sized graphene and a tangent line of the micron-sized graphene at a contact point of the micron-sized graphene and the mono-like anode material is less than 4 degrees; preferably, the included angle between the micron-sized graphene and the tangent line of the micron-sized graphene at the contact point of the single crystal-like morphology cathode material is 0 degree.
The micron-sized graphene is in a close-fit coating state on the surface of the crystal grain of the single crystal-like positive electrode material, and the longest distance between the micron-sized graphene and the surface of the single crystal-like positive electrode material is less than 2 nm; preferably, the longest distance between the micron-sized graphene and the surface of the single crystal-like positive electrode material is 0 nm.
As shown in fig. 10a, the micron-sized graphene can be tightly attached to the surface of the single crystal-like positive electrode material, the micron-sized graphene is tightly contacted with the single crystal-like positive electrode material particles without gaps, and the shortest distance between the micron-sized graphene and the surface of the single crystal-like positive electrode material is about 0; instead of the method shown in fig. 10b, in the conventional technology, the micron-sized graphene coats the surface of the single-crystal-like anode material, under the condition of the same area of the micron-sized graphene, the contact area or the coating area of the micron-sized graphene on the surface of the single-crystal-like anode material is smaller, a gap is formed between the micron-sized graphene and the surface of the single-crystal-like anode material, the longest distance between the micron-sized graphene and the surface of the single-crystal-like anode material is far greater than 3nm, the close attachment shown in fig. 10a is not achieved, and the range of the invention that the micron-sized graphene is in a coating state on the surface of a crystal grain of the single-crystal-like anode material is also out.
In one embodiment, the preparation method of the micron-sized carbon-based coating optimized single-crystal-like cathode material comprises the following steps:
(1) uniformly mixing N-methyl pyrrolidone, a graphene sheet and polyvinylidene fluoride to obtain a substance I;
(2) mixing the substance I obtained in the step (1), the monocrystal-like positive electrode material and N-methylpyrrolidone, and stirring for 3 hours at 40 ℃ to uniformly mix to obtain mixed slurry;
(3) drying the mixed slurry obtained in the step (2) to obtain a micron-sized carbon-coated optimized mono-like anode material;
the mass ratio of the graphene sheet material to the polyvinylidene fluoride to the single crystal-like positive electrode material is (0.001-0.05): (0.001-0.07): 1; preferably, the mass ratio of the graphene sheet material to the polyvinylidene fluoride to the single-crystal-like positive electrode material is (0.002-0.04): (0.003-0.05): 1; more preferably, the mass ratio of the graphene sheet material to the polyvinylidene fluoride to the mono-like morphology cathode material is 0.003: 0.004: 1;
the adding amount of the N-methyl pyrrolidone is determined according to the viscosity of the mixed slurry; the viscosity of the mixed slurry is 5000-; preferably, the viscosity of the mixed slurry is 6000-7000cp (25 ℃); more preferably, the viscosity of the mixed slurry is 6500cp (25 ℃);
the drying mode is spray drying; the temperature of the air inlet in the spray drying process is 420 ℃, and the temperature of the outlet is 215 ℃.
The invention provides a lithium ion battery electrode made of a micron-sized carbon-based coating optimized single-crystal-like anode material, and the preparation raw materials of the lithium ion battery electrode comprise the micron-sized carbon-based coating optimized single-crystal-like anode material, a conductive agent, a binder and a current collector.
In some embodiments, the weight ratio of the micron-sized carbon-based coating optimized single-crystal-like cathode material, the conductive agent and the binder is (90-98): (1-6): (1-6).
In some preferred embodiments, the weight ratio of the micron-sized carbon-based coating optimized single-crystal-like cathode material, the conductive agent and the binder is (92-96): (2-5): (2-5).
In a more preferred embodiment, the weight ratio of the micron-sized carbon-based coating optimized single-crystal-like cathode material, the conductive agent and the binder is 93: 3: 3.
conductive agent
In some embodiments, the conductive agent is selected from one or more of carbon black, micron graphite, acetylene black, graphene, activated carbon.
In some preferred embodiments, the conductive agent is carbon black, and the invention is not particularly limited by the brand and manufacturer of the carbon black.
Binder
In some embodiments, the binder is selected from one or more of fluororubber, polyvinylidene fluoride, polytetrafluoroethylene, fluorinated polyvinylidene fluoride, polytetrafluoroethylene-ethylene copolymer.
In some preferred embodiments, the binder is polyvinylidene fluoride, and the invention is not particularly limited to the grade and manufacturer of polyvinylidene fluoride.
Current collector
In the invention, the current collector refers to a structure or a part for collecting current, and mainly refers to metal foils such as copper foil and aluminum foil on the lithium ion battery; the function of the current collector is to collect the current generated by the active materials of the battery so as to form a larger current output, therefore, the current collector should be in full contact with the active materials, and the internal resistance should be as small as possible.
In some embodiments, the current collector is a copper foil and/or an aluminum foil.
In some preferred embodiments, the current collector is an aluminum foil, and the thickness, width and manufacturer of the aluminum foil are not particularly limited.
In one embodiment, the method for preparing the lithium ion battery electrode made of the micron-sized carbon-based coated optimized single-crystal-like cathode material comprises the following steps: and mixing the micron-sized carbon-coated optimized mono-like positive electrode material, a conductive agent and a binder, and coating the mixture on a current collector to prepare a positive electrode plate, thus obtaining the lithium ion battery electrode made of the micron-sized carbon-coated optimized mono-like positive electrode material.
The invention provides an application of the lithium ion battery electrode made of the micron-sized carbon-coated optimized single-crystal-like anode material, and the lithium ion battery electrode made of the micron-sized carbon-coated optimized single-crystal-like anode material is used for preparing a button cell.
The button cell is also called a button cell, and refers to a cell with the external dimension like a small button, generally speaking, the diameter is larger, and the thickness is thinner (compared with a columnar cell such as a cell with No. 5 AA in the market); the button cell is classified from the appearance, and the same corresponding cell is classified into a cylindrical cell, a square cell and a special-shaped cell.
In some embodiments, a button cell is assembled by using lithium metal or graphite as a negative electrode and using a lithium ion battery electrode made of the micron-sized carbon-based coating optimized single-crystal-like positive electrode material as a positive electrode.
In some preferred embodiments, metal lithium or graphite is used as a negative electrode, the lithium ion battery electrode coated with the optimized mono-like positive electrode material by the micron-sized carbon is used as a positive electrode, and the lithium ion battery electrode coated with the optimized mono-like positive electrode material by the micron-sized carbon is placed in a vacuum drying oven at 110 ℃ and dried for 4.5 hours for later use; rolling the pole piece on a rolling machine, and punching the rolled pole piece into a circular pole piece with a proper size; the cell assembly was carried out in a glove box filled with argon, the electrolyte of the electrolyte was 1M LiPF6, the solvent was EC: DEC: and (3) assembling the DMC as a button cell by a volume ratio of 1:1: 1.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
Examples
Example 1
the monocrystal-like positive electrode material is HYX6 type nickel cobalt lithium manganate, belongs to a ternary material, is in a monocrystal-like shape, has a D50 ═ 3.9 +/-1.0 mu m, and is purchased from Yao graphene energy storage materials science and technology ltd in Ningxia Han;
the graphene sheet is GRCP0130L type graphene, the thickness of the graphene is less than about 30 layers (namely less than about 10nm), the sheet diameter is 1-20 mu m, and the graphene sheet is purchased from Tianjin Ikekan graphene science and technology limited company;
the particle size distribution diagram of the micron-sized carbon-based coated optimized mono-like cathode material is shown in fig. 4-a; the particle size distribution diagram of the single crystal-like morphology cathode material is 4-b; the particle size distribution of the micron-sized carbon-coated optimized mono-like anode material is basically the same as that of the mono-like anode material; the difference value between the average particle size of the micron-sized carbon-coated optimized single-crystal-like anode material and the average particle size of the single-crystal-like anode material is almost 0 nm;
the laser Raman spectrum of the micron-sized carbon-coated optimized mono-like cathode material is shown in figure 5; the micron-sized graphene and the single-crystal-like positive electrode material can be distinguished by a laser Raman (Raman) testing technology, and a D peak, a G peak and a G 'peak of a coating area of the micron-sized carbon-based coating optimized single-crystal-like positive electrode material completely correspond to the D peak, the G peak and the G' peak of a graphene sheet respectively; the non-coating region of the micron-sized carbon-coated optimized mono-like cathode material is free of a D peak, a G peak and a G' peak;
the X-ray diffraction pattern of the micron-sized carbon-coated optimized mono-like anode material is shown in a figure 3-I; the X-ray diffraction pattern of the single-crystal-like positive electrode material is shown in a figure 3-II; the diffraction peak positions and relative intensities of the micron-sized carbon-coated optimized single-crystal-like anode material and the single-crystal-like anode material are the same, and the integral deviation angle of the diffraction peak is almost 0 degree;
a TEM image of the micron-sized carbon-based coated optimized single-crystal-like cathode material is shown in FIG. 1; the SEM image of the micron-sized carbon-based coating optimized single-crystal-like cathode material is shown in FIG. 2; the included angle between the micron-sized graphene and the tangent line of the micron-sized graphene at the contact point of the mono-like morphology cathode material is almost 0 degree; the longest distance between the micron-sized graphene and the surface of the single crystal-like positive electrode material is almost 0 nm;
the preparation method of the micron-sized carbon-coated optimized mono-like anode material comprises the following steps:
(1) uniformly mixing N-methyl pyrrolidone, a graphene sheet and polyvinylidene fluoride to obtain a substance I;
(2) mixing the substance I obtained in the step (1), the monocrystal-like positive electrode material and N-methylpyrrolidone, and stirring for 3 hours at 40 ℃ to uniformly mix to obtain mixed slurry;
(3) drying the mixed slurry obtained in the step (2) to obtain a micron-sized carbon-coated optimized mono-like anode material;
the mass ratio of the graphene sheet to the polyvinylidene fluoride is 0.003: 0.0045;
the polyvinylidene fluoride is available from battery grade PVDF 5130 from suwei corporation;
the adding amount of the N-methyl pyrrolidone is determined according to the viscosity of the mixed slurry; the viscosity of the mixed slurry was 6500cp (25 ℃);
the drying mode is spray drying; the temperature of the air inlet in the spray drying process is 420 ℃, and the temperature of the outlet is 215 ℃.
A lithium ion battery electrode made of a micron-sized graphene-coated single-crystal-like anode material comprises the micron-sized graphene-coated single-crystal-like anode material, a conductive agent, a binder and a current collector, wherein the raw materials for preparing the lithium ion battery electrode comprise the micron-sized graphene-coated single-crystal-like anode material, the conductive agent, the binder and the current collector;
the weight ratio of the micron-sized carbon-coated optimized mono-like cathode material to the conductive agent to the binder is 93: 3: 3;
the conductive agent is carbon black, which is purchased from SuperP of Imery company;
the binder is polyvinylidene fluoride, available from HSV900 of arkema;
the current collector was aluminum foil, available from the Yongjie company 1060-H18;
the preparation method of the lithium ion battery electrode made of the micron-sized carbon-coated optimized mono-like anode material comprises the following steps: and mixing the micron-sized carbon-coated optimized mono-like positive electrode material, a conductive agent and a binder, and coating the mixture on a current collector to prepare a positive electrode plate, thus obtaining the lithium ion battery electrode made of the micron-sized carbon-coated optimized mono-like positive electrode material.
A button cell of a lithium ion battery electrode made of a micron-sized carbon-coated optimized mono-like anode material takes metal lithium or graphite as a negative electrode, takes the lithium ion battery electrode made of the micron-sized carbon-coated optimized mono-like anode material as a positive electrode, and puts the lithium ion battery electrode made of the micron-sized carbon-coated optimized mono-like anode material in a vacuum drying oven at 110 ℃ for drying for 4.5 hours for later use; rolling the pole piece on a rolling machine, and punching the rolled pole piece into a circular pole piece with a proper size; the cell assembly was carried out in a glove box filled with argon, the electrolyte of the electrolyte was 1M LiPF6, the solvent was EC: DEC: and (3) assembling the DMC as a button cell by a volume ratio of 1:1: 1.
Comparative example 1
The comparative example 1 provides a lithium ion battery electrode made of a single-crystal-like anode material, and the preparation raw materials of the lithium ion battery electrode comprise a single-crystal-like anode material, a conductive agent, a binder and a current collector;
the monocrystal-like positive electrode material is HYX6 type nickel cobalt lithium manganate, belongs to a ternary material, is in a monocrystal-like shape, has a D50 ═ 3.9 +/-1.0 mu m, and is purchased from Yao graphene energy storage materials science and technology ltd in Ningxia Han;
the conductive agent is carbon black, which is purchased from SuperP of Imery company;
the binder is polyvinylidene fluoride, available from HSV900 of arkema;
the current collector was aluminum foil, available from Yongjie 1060-H18.
The preparation method of the lithium ion battery electrode made of the single-crystal-like anode material comprises the following steps:
(1) uniformly mixing N-methyl pyrrolidone and polyvinylidene fluoride to obtain a substance I;
(2) mixing the substance I obtained in the step (1), the quasi-single crystal anode material and N-methyl pyrrolidone, and stirring for 4 hours at 40 ℃ to uniformly mix to obtain mixed slurry;
(3) drying the mixed slurry obtained in the step (2); mixing the dried mixed slurry, a conductive agent and a binder, and coating the mixture on a current collector to prepare a positive pole piece, namely obtaining the lithium ion battery electrode of the monocrystal-like positive pole material;
the weight ratio of the polyvinylidene fluoride to the single crystal-like positive electrode material is 0.004: 1;
the polyvinylidene fluoride is available from battery grade PVDF 5130 from suwei corporation;
the adding amount of the N-methyl pyrrolidone is determined according to the viscosity of the mixed slurry; the viscosity of the mixed slurry was 6500cp (25 ℃);
the drying mode is spray drying; the temperature of the air inlet in the spray drying process is 420 ℃, and the temperature of the outlet is 215 ℃.
A lithium ion battery electrode button cell of single crystal-like anode material, regard metallic lithium or graphite as the negative pole, regard lithium ion battery electrode of the above-mentioned single crystal-like anode material as the positive pole, put the lithium ion battery electrode of the single crystal-like anode material in the vacuum drying oven of 110 duC and oven dry for 4.5 hours for subsequent use; rolling the pole piece on a rolling machine, and punching the rolled pole piece into a circular pole piece with a proper size; the cell assembly was carried out in a glove box filled with argon, the electrolyte of the electrolyte was 1M LiPF6, the solvent was EC: DEC: and (3) assembling the DMC as a button cell by a volume ratio of 1:1: 1.
Performance evaluation
1. Transmission electron microscopy images: the micron-sized graphene-coated single-crystal-like cathode material prepared in example 1 is subjected to TEM characterization, and the test result is shown in FIG. 1.
2. Scanning electron microscopy: the micron-sized carbon-based coated optimized mono-like cathode material in example 1 is magnified by 20k under a scanning electron microscope, and the test result is shown in fig. 2.
Fig. 2 is an SEM image (scanning electron microscope image) of the micro graphene coated single-crystal-like cathode material prepared by the present invention.
X-ray diffraction pattern: the micron-sized carbon-coated optimized mono-like positive electrode material (i) and the mono-like morphology positive electrode material (ii) in the embodiment 1 are subjected to an X-ray diffraction test, and the test result is shown in FIG. 3.
As can be seen from fig. 3, the micron graphene sheet is coated on the surface of the crystal grain of the single-crystal-like material, and the bulk phase structure in the crystal grain is not affected, that is, the X-ray test results of the micron graphene coated single-crystal-like cathode material and the single-crystal-like cathode material are substantially consistent.
4. The particle size distribution diagram is as follows: the micron-sized carbon-coated optimized single-crystal-like cathode material (a) and the single-crystal-like morphology cathode material (b) in example 1 were subjected to particle size distribution analysis, and the test results are shown in fig. 4.
As can be seen from fig. 4, the micron graphene sheet is coated on the surface of the crystal grain of the single-crystal-like material, and the particle size of the crystal grain is not significantly increased, that is, the particle size distribution results of the micron graphene coated single-crystal-like cathode material and the single-crystal-like cathode material are substantially consistent.
5. And (3) laser Raman testing: the micron-sized carbon-based coated optimized single-crystal-like cathode material described in example 1 was subjected to a laser raman test, and the test result is shown in fig. 5.
As can be seen from fig. 5, the positive electrode material portion and the coating material portion can be distinguished by a laser Raman (Raman) test technique, and the measured characteristic peaks of the coating material completely correspond to the characteristic peaks D, G, and G' of graphene; and the ratio of the D peak, the G peak and the G' peak Intensity of the graphene is not less than 0.01 and not more than Intensity (D)/not more than 1, and not less than 0.01 and not more than Intensity (D)/not more than 1.
6. Measuring alternating current impedance: the electrochemical alternating-current impedance of the mono-like anode material battery and the micro-scale carbon coated and optimized mono-like anode material battery are tested at room temperature of 25 ℃, and the experimental result is shown in figure 6.
As can be seen from fig. 6, the impedance of the micron-sized carbon-based coating optimized single-crystal-like cathode material battery is reduced to a certain extent compared with the impedance of the single-crystal-like cathode material battery before coating.
7. Battery capacity retention ratio: the micron-sized carbon-coated optimized mono-like positive electrode material battery II in the embodiment 1 and the mono-like positive electrode material battery I in the comparative example 1 are subjected to a button cell capacity retention rate test at 45 ℃, and the test result is shown in FIG. 7.
As can be seen from fig. 7, the storage rate of the button cell corresponding to the micron-sized carbon-coated optimized single-crystal-like anode material is higher than 85% after 200 cycles at 45 ℃, the retention rate of the capacity of the micron-sized carbon-coated optimized single-crystal-like anode material cell is higher than that of the single-crystal-like anode material cell at 45 ℃, and the micron-sized graphene is coated with a certain improvement effect.
8. Battery rate charge capacity retention ratio: the micron-sized carbon-coated optimized mono-like positive electrode material battery (II) in the embodiment 1 and the mono-like positive electrode material battery (I) in the comparative example 1 are subjected to a button cell rate charge capacity retention rate test, and the test result is shown in FIG. 8.
As can be seen from fig. 8, the rate of retention of high rate charge capacity of the micron-sized carbon-coated optimized mono-like cathode material battery is higher than that of the mono-like cathode material battery, and the rate of retention of rate charge of the micron-sized carbon-coated mono-like cathode material battery is significantly improved.
9. Battery rate discharge capacity retention rate: the rate discharge capacity retention rate of the button cell was measured by using the micron-sized carbon-coated optimized mono-like positive electrode material battery in example 1 (c) and the mono-like positive electrode material battery in comparative example 1 (c), and the measurement results are shown in fig. 9.
As can be seen from fig. 9, the rate of retention of high-rate discharge capacity of the micron-sized carbon-coated optimized single-crystal-like positive electrode material battery is higher than that of the single-crystal-like positive electrode material battery, and the rate of retention of discharge capacity of the micron-sized carbon-coated optimized single-crystal-like positive electrode material battery is remarkably improved.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (9)
1. The micron-sized carbon-coated optimized mono-like cathode material is characterized by consisting of a mono-like morphology cathode material and micron-sized graphene sheets; the graphene sheet material is tightly coated on the surface of the positive electrode material with the single crystal-like appearance.
2. The micron-sized carbon-based coated optimized single-crystal-like cathode material according to claim 1, wherein a TEM image of the micron-sized carbon-based coated optimized single-crystal-like cathode material satisfies fig. 1; the SEM image satisfies that of FIG. 2; preferably, the included angle between the micron-sized graphene and the tangent line of the micron-sized graphene at the contact point of the mono-like morphology cathode material is less than 5 degrees; more preferably, the included angle between the micron-sized graphene and the tangent line of the micron-sized graphene at the contact point of the single crystal-like morphology cathode material is 0 °.
3. The micron-sized carbon-based coated optimized mono-like cathode material according to claim 1, wherein the mono-like morphology cathode material is selected from LiCoO2、LiNixCoyMnzO2、LiNixCoyAlzO2One or more of; the LiNixCoyMnzO2Or LiNixCoyAlzO2Wherein x + y + z is 1, x is more than or equal to 0.2 and less than or equal to 0.95, y is more than or equal to 0.05 and less than or equal to 0.4, and z is more than or equal to 0.05 and less than or equal to 0.5; the crystal structure of the single crystal-like positive electrode material is a layered structure, the crystal structure belongs to an R-3m space group, and the positive electrode material particles are in a single crystal-like shape.
4. The micron-sized carbon-based coated optimized mono-like cathode material according to claim 1, wherein the graphene sheet has a sheet diameter of 1-20 μm.
5. The micron-sized carbon-based coated optimized mono-like cathode material according to claim 1, wherein the graphene sheet has a thickness of less than 10 nm.
6. The micron-sized carbon-based coated optimized single-crystal-like cathode material according to any one of claims 1 to 5, wherein the difference between the average particle size of the micron-sized carbon-based coated optimized single-crystal-like cathode material and the average particle size of the single-crystal-like anode material is less than 1000 nm; preferably, the difference between the average particle size of the micron-sized carbon-based coating optimized single-crystal-like cathode material and the average particle size of the single-crystal-like morphology cathode material is less than 700 nm; more preferably, the difference between the average particle size of the micron-sized carbon-based coating optimized single-crystal-like cathode material and the average particle size of the single-crystal-like morphology cathode material is less than 400 nm.
7. The micron-sized carbon-based coated optimized single-crystal-like cathode material according to any one of claims 1 to 5, wherein in a laser Raman spectrum, a D peak, a G peak and a G 'peak of a coating region of the micron-sized carbon-based coated optimized single-crystal-like cathode material completely correspond to a D peak, a G peak and a G' peak of a graphene sheet respectively.
8. The micron-sized carbon-based coated optimized single-crystal-like cathode material according to any one of claims 1 to 5, wherein in an X-ray diffraction pattern, the positions and the relative intensity distribution orders of diffraction peaks of the micron-sized carbon-based coated optimized single-crystal-like cathode material and the single-crystal-like anode material are the same, and the integral deviation angle of the diffraction peaks is less than 3 degrees.
9. A lithium ion battery electrode made of micron-sized carbon-coated optimized mono-like cathode materials is characterized in that raw materials for preparing the lithium ion battery electrode comprise the micron-sized carbon-coated optimized mono-like cathode materials, a conductive agent, a binder and a current collector according to any one of claims 1 to 8.
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| CN107565121A (en) * | 2017-07-17 | 2018-01-09 | 江西南氏锂电新材料有限公司 | A kind of preparation method of lithium battery modified anode material |
| CN110364713A (en) * | 2019-07-16 | 2019-10-22 | 湖南长远锂科股份有限公司 | A kind of preparation method of combined conductive agent cladding class monocrystalline lithium-rich manganese-based anode material |
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