CN111276685A - Positive electrode material and preparation method thereof, positive electrode piece and lithium ion battery - Google Patents

Positive electrode material and preparation method thereof, positive electrode piece and lithium ion battery Download PDF

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CN111276685A
CN111276685A CN202010101266.0A CN202010101266A CN111276685A CN 111276685 A CN111276685 A CN 111276685A CN 202010101266 A CN202010101266 A CN 202010101266A CN 111276685 A CN111276685 A CN 111276685A
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positive electrode
electrode material
solution
lithium
lithium ion
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王刚
王凤英
王冲
李鑫
王万玺
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Qinghai Nationalities University
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
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  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a positive electrode material, a preparation method thereof, a positive electrode plate and a lithium ion battery. The positive electrode material includes: a base material; a graphene coating layer coating the base material; wherein the matrix material is a lithium-rich manganese-based material. The outer layer of the reduced graphene oxide layer can effectively inhibit side reactions on the interface of the anode and electrolyte, so that the first-turn coulombic efficiency and the cycling stability of the device are improved; and the reduced graphene oxide layer can effectively reduce the series resistance of the anode, and improve the modification of the material on the lithium ion anode material, so that the obtained composite material has higher lithium ion transmission rate and lower impedance.

Description

Positive electrode material and preparation method thereof, positive electrode piece and lithium ion battery
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a positive electrode material, a preparation method thereof, a positive electrode plate and a lithium ion battery.
Background
Today, the electronic industry is not limited to small electric products such as watches and notebooks, but develops towards the electric automobile industry with high capacity and high energy density. Therefore, the demand for it is naturally higher and higher. Recently, the layered lithium-rich manganese-based oxide can reach a specific capacity of more than 200mAh/g, and has the characteristics of voltage stability, good cycle life and the like, so that the layered lithium-rich manganese-based oxide can be expected to be a candidate for providing energy for hybrid electric vehicles and pure electric vehicles.
However, the layered lithium-rich manganese-based oxide positive electrode material has some disadvantages, such as severe pressure drop, discharge capacity degradation, and poor rate performance during electrochemical testing. In order to improve these problems, people modify the particles mainly by means of coating, doping, controlling the morphology of the particles and the like. In these modification methods, the surface coating can improve the problems existing in the layered lithium-rich manganese-based positive electrode material. The materials used for coating at present are generally oxides, fluorides, phosphates and the like, and the coating can improve the cycling stability of the materials, but the coating material on the surface has poor conductivity, so that the rate performance is poor.
Disclosure of Invention
The invention adopts a unique core-shell structure to coat the lithium-rich manganese-based positive electrode material with graphene. The core of the core-shell structure is a lithium-rich manganese-based positive electrode material, the shell layer is high-temperature reduced graphene oxide, and the outer layer of reduced graphene oxide can provide high enough electron conductivity for the modified positive electrode material.
The invention provides a positive electrode material, which comprises: the graphene oxide coated substrate comprises a substrate material and reduced graphene oxide, wherein the graphene oxide coated substrate material is formed by changing the charges on the surface of the substrate material and the electrostatic interaction of the graphene through positive and negative potentials, so that GO is attached to the surface of the LLO.
The invention provides a positive electrode material, which comprises: a base material; a graphene coating layer coating the base material; wherein the matrix material is a lithium-rich manganese-based material.
In the above cathode material, the cathode material is of a core-shell structure, the core is the matrix material, and the shell is the graphene coating layer.
In the above cathode material, the graphene coating layer includes high-temperature reduced graphene oxide.
In the positive electrode material, the matrix material and the graphene clad layer are bonded by electrostatic interaction.
The invention also provides a positive pole piece, comprising: a current collector; an active material layer disposed on the current collector; wherein the active material layer comprises the positive electrode material.
The invention also provides a lithium ion battery which comprises the positive pole piece.
The invention also provides a method for preparing the cathode material, which comprises the following steps: weighing a lithium-rich manganese-based material, dispersing the lithium-rich manganese-based material in a solution of a surfactant, and stirring to obtain a matrix solution; carrying out ultrasonic treatment on a graphene oxide solution under ultrasonic waves, and then dropwise adding the solution into the matrix solution to obtain a mixed solution; and transferring the mixed solution into a water bath kettle for water bath reaction, filtering, drying and annealing to obtain the cathode material.
In the above method, wherein the surfactant comprises C38H80BrN。
In the above method, wherein the annealing comprises annealing at 400 ℃ for 5 h.
In the above method, wherein the water bath reaction comprises a water bath reaction at 60 ℃ for 12 h.
The invention has the advantages that: the process method is simple, and large-scale preparation and production can be realized; the outer layer of the reduced graphene oxide layer can effectively inhibit side reactions on the interface of the anode and electrolyte, so that the first-turn coulombic efficiency and the cycling stability of the device are improved; and the reduced graphene oxide layer can effectively reduce the series resistance of the anode, and improve the modification of the material on the lithium ion anode material, so that the obtained composite material has higher lithium ion transmission rate and lower impedance.
Drawings
Fig. 1 is an X-ray diffraction analysis (XRD) pattern and a Scanning Electron Microscope (SEM) pattern of the lithium-rich manganese-based positive electrode material precursor prepared in example 1.
Fig. 2 is an XRD spectrum and an SEM spectrum of the graphene (rGO) -coated lithium ion cathode material prepared in example 2.
FIG. 3 is a TEM spectrum of the LLO @ rGO lithium ion cathode material prepared in example 3.
Fig. 4 is a first charge-discharge curve, a rate performance curve, a cycle curve and an electrochemical impedance spectrum of lithium ion batteries with different lithium ion cathode materials prepared in examples 1 and 2.
Detailed Description
The following examples are presented to enable those skilled in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The invention adopts the coating material graphene which has good conductivity and stable structure. Graphene is a material with excellent conductivity and super-strong mechanical properties, is an ideal conductive additive for mixed nanostructure electrodes, and is modified by graphene to certain metal or metal oxide cathode materials, so that the cycling stability and the rate performance of the cathode materials are improved.
The invention provides a surface coating modification method for a lithium-rich manganese-based lithium ion positive electrode material, and the whole preparation process is efficient, environment-friendly, economic, simple in process and suitable for large-scale production.
According to the invention, the lithium-rich manganese-based lithium ion positive electrode material is coated with graphene, and the lithium-rich manganese-based lithium ion positive electrode material and the reduced graphene oxide coating layer are sequentially arranged from inside to outside. Firstly, the surface potential of the positive electrode material is changed into a positive potential, and then the positive electrode material solution with positive charges and the graphene oxide solution with negative charges are mixed with each other. The graphene oxide is adsorbed on the surface of the positive electrode material through electrostatic action. In addition, after the graphene oxide layer is subjected to high-temperature treatment, a core-shell structure of the positive electrode material reduced graphene oxide is formed. The specific implementation process is as follows:
weighing quantitative lithium ion batteryThe electrode material is dispersed in a certain amount of surfactant solution (the surfactant may be C)38H80BrN, one of cationic surfactants) for 1-2 h. In addition, after a graphene oxide solution with a certain concentration (for example, 12mg/mL) is subjected to ultrasonic treatment for 1 hour, the solution is dropwise added into the mixed solution, the mixed solution is moved into a water bath, the water bath is carried out for 12 hours at the temperature of 60 ℃, solid particles are separated from the solution and dried, and annealing is carried out, so that the coated cathode material is obtained.
The following description is given in conjunction with specific examples to better understand the present invention.
Example 1: preparation of lithium-rich manganese-based positive electrode material
Will contain the required stoichiometric amount of MnSO4·H2O(5.07g)、NiSO4·6H2O (2.6286g) and CoSO4·7H2O (2.811g) in water was added to 50ml of water and stirred until the solution became clear, and 25ml of ethanol was added. After 1h, the precipitant NH4HCO3(4.1475g) the aqueous solution was added dropwise to the mixed solution. After 5h the precursor was separated using a centrifuge and washed three times and then dried at 60 ℃. Finally, the precursor is reacted with LiOH H2O (5% excess lithium) was mixed well and pre-treated in air at 400 deg.C-600 deg.C for 2h, calcined at 800 deg.C for 5 hours to give black powder (LLO). As shown in fig. 1 (a), the XRD pattern of the precursor of the sample is known as a typical carbonate structure.
Example 2: coating of graphene oxide layers
Three parts of lithium ion positive electrode material (0.15 g) dispersed in 0.003g of surfactant (C) were weighed out38H80BrN) solution for 0.5 h. In addition, after a graphene oxide solution of liquid Graphene Oxide (GO) (12mg/mL) with the mass ratio of 0.5 w%, 1 w% and 2 w% is subjected to ultrasonic treatment for 2 hours under microwave, the graphene oxide solution is dropwise added into the mixed solution, and the mixed solution is moved into a water bath kettle and is subjected to water bath at 60 ℃ for 12 hours. Finally, annealing for 5 hours at 400 ℃ in an atmosphere taking Ar gas as protective gas. Thus obtaining the LLO @ rGO with the core-shell structure. As shown in fig. 2 (a), all samples have similar diffraction peaks, with a set of smaller derivatives appearing between the regions of about 20 at 2 θPeak shooting, mainly due to Li contained in the bulk of the material2MnO3The structure is that Li and Mn in the transition metal layer are orderly arranged to form LiMn6、LiMn5The Ni type superlattice has space group of C2/m, and belongs to monoclinic system. This means that rGO coating does not cause transformations to the structure and crystal form of LLO. FIG. 2 (b) (LLO @ rGO) is an SEM image. FIG. 2 (C) is GO, LLO @ C38H80Zeta potential maps of three aqueous solutions of BrN and LLO. As can be seen from the figure, the graphene oxide aqueous solution is negatively charged. The zeta potential of the aqueous lithium-rich material (LLO) solution without surfactant modification is between 0 and 5mV, nearly neutral, and positively charged after treatment with surfactant. Therefore, when Graphene Oxide (GO) is added to the lithium-rich material aqueous solution, GO can be attached to the surface of LLO through the electrostatic action of positive and negative potentials. FIG. 3 is a TEM image of LLO @ rGO.
The uniform slurry was then cast onto aluminum foil by blade coating, which was then held in a vacuum oven at 80 ℃ for 12h, and the aluminum foil with active film was then punched into a circular disk (12 mm), the mass load of the positive electrode material being approximately the same as the mass load of the negative electrode material
Figure BDA0002386946030000051
cm-2. ) The cathode material of the above example is prepared into a lithium ion battery, and fig. 4 is a graph comparing electrochemical performances of the matrix material prepared in examples 1 and 2 and the modified material. As shown in fig. 4 (a), the obtained clad material has a high first-turn coulombic efficiency (73%), and in addition, as can be seen from fig. 4 (b), (c), and (d), the clad material has excellent voltage stability, cycle stability, and rate capability. (cycle and rate performance was measured on a Newware CT-4008 tester with charge and discharge voltages ranging from 2.0 to 4.8V.)
Those skilled in the art will appreciate that the above embodiments are merely exemplary embodiments and that various changes, substitutions, and alterations can be made without departing from the spirit and scope of the application.

Claims (10)

1. A positive electrode material comprising:
a base material;
a graphene coating layer coating the base material;
wherein the matrix material is a lithium-rich manganese-based material.
2. The positive electrode material according to claim 1, wherein the positive electrode material has a core-shell structure, a core is the matrix material, and a shell is the graphene clad layer.
3. The cathode material according to claim 1, wherein the graphene coating layer comprises high-temperature reduced graphene oxide.
4. The positive electrode material according to claim 1, wherein the matrix material and the graphene clad layer are bonded by electrostatic interaction.
5. A positive electrode sheet comprising:
a current collector;
an active material layer disposed on the current collector;
wherein the active material layer includes the positive electrode material according to any one of claims 1 to 4.
6. A lithium ion battery comprising the positive electrode sheet of claim 5.
7. A method of making a positive electrode material, comprising:
weighing a lithium-rich manganese-based material, dispersing the lithium-rich manganese-based material in a solution of a surfactant, and stirring to obtain a matrix solution;
carrying out ultrasonic treatment on a graphene oxide solution under ultrasonic waves, and then dropwise adding the solution into the matrix solution to obtain a mixed solution;
and transferring the mixed solution into a water bath kettle for water bath reaction, filtering, drying and annealing to obtain the cathode material.
8. The method of claim 7, wherein the surfactant comprises C38H80BrN。
9. The method of claim 7, wherein the annealing comprises annealing at 400 ℃ for 5 h.
10. The method of claim 7, wherein the water bath reaction comprises a water bath reaction at 60 ℃ for 12 hours.
CN202010101266.0A 2020-02-19 2020-02-19 Positive electrode material and preparation method thereof, positive electrode piece and lithium ion battery Pending CN111276685A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112331826A (en) * 2020-10-23 2021-02-05 华南师范大学 Modified lithium ion battery positive electrode material and preparation method and application thereof

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