CN112510196A - Preparation method of manganese-based metal oxide positive electrode - Google Patents
Preparation method of manganese-based metal oxide positive electrode Download PDFInfo
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- CN112510196A CN112510196A CN202011292541.8A CN202011292541A CN112510196A CN 112510196 A CN112510196 A CN 112510196A CN 202011292541 A CN202011292541 A CN 202011292541A CN 112510196 A CN112510196 A CN 112510196A
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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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- 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
- H01M4/485—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
- 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
- H01M4/52—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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- 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
Abstract
The invention discloses a preparation method of a manganese-based metal oxide anode, which comprises the following steps: s1, grinding and firing: grinding cobaltosic oxide, nickel oxide, manganese oxide and sodium carbonate in stoichiometric ratio in an agate mortar, fully grinding, then burning in a muffle furnace at 500 ℃ for 3 hours, and continuing heating to 850 ℃ for 12 hours; s2, cooling and isolating: cooling to room temperature, and storing the obtained solid powder in an argon-protected glove box to isolate air and moisture; s3, coating the positive electrode; s4, preparing materials; s5, stirring and mixing; s6, dropwise adding the slurry; and S7, vacuum drying. According to the preparation method of the manganese-based metal oxide anode, the coated material has the advantages of high specific capacity, strong circulation stability and good rate performance, the coated coating can effectively improve the circulation stability, prolong the circulation life, effectively relieve the structural stress of the active material caused by repeated sodium insertion/sodium removal, enhance the stability, reduce the contact area of the active material and electrolyte and reduce side reactions.
Description
Technical Field
The invention relates to the technical field of battery anode preparation, in particular to a preparation method of a manganese-based metal oxide anode.
Background
Over the past few decades, battery technologies have become increasingly powerful, making them a key component of our daily activities. Lithium ion batteries have become the primary power source for use in portable devices and electric vehicles due to their high energy density and environmentally friendly operation. These advantages have led to an explosive increase in global demand for lithium ion batteries. However, the high cost of cobalt and lithium as raw materials for lithium ion batteries is a serious problem. Therefore, it is important to develop new electrical energy storage systems that are low cost and environmentally sustainable. Because of abundant natural resources, wide availability and low sodium resource cost, sodium ion batteries are considered as one of the most promising substitute products of commercial lithium ion batteries, and the development of a positive electrode material with high specific capacity and excellent cycle life can effectively promote the commercialization process of the sodium ion batteries.
Therefore, we propose herein a method of making a manganese-based metal oxide positive electrode.
Disclosure of Invention
The invention provides a preparation method of a manganese-based metal oxide anode aiming at the defects in the background technology.
In order to solve the above phenomena, the present invention adopts the following technical scheme that the preparation method of the manganese-based metal oxide anode comprises the following steps: s1, grinding and firing: grinding cobaltosic oxide, nickel oxide, manganese oxide and sodium carbonate in stoichiometric ratio in an agate mortar, fully grinding, then burning in a muffle furnace at 500 ℃ for 3 hours, and continuing heating to 850 ℃ for 12 hours; s2, cooling and isolating: cooling to room temperature, and storing the obtained solid powder in an argon-protected glove box to isolate air and moisture; s3, positive electrode coating: the prepared anode material is directly coated with a layer of titanium dioxide (Na0.55Ni0.1Co0.1Mn0.8O2/TiO 2) with the thickness of about 5 nanometers by an Atomic Layer Deposition (ALD) technology; s4, preparing material: the active substances are the two manganese-based metal oxide positive electrode materials prepared in the above way, the solvent is N-methyl pyrrolidone (NMP), the conductive agent is acetylene black, the binder is polyvinylidene fluoride (PVDF and the solvent NMP are prepared into a 2.5wt% solution), and the current collector is a carbon-coated aluminum foil; s5, stirring and mixing: respectively dissolving Na0.55Ni0.1Co0.1Mn0.8O2 and Na0.55Ni0.1Co0.1Mn0.8O2/TiO2, acetylene black serving as a conductive agent and PVDF serving as a binder into NMP according to the mass ratio of 7: 2: 1, and uniformly stirring and mixing; s6, adding slurry dropwise: uniformly dripping the slurry on a pre-cut circular aluminum foil with the diameter of 12mm by using a liquid-transferring gun; s7, vacuum drying: and drying the aluminum foil coated with the slurry in a vacuum oven at 80 ℃ for 12 hours to obtain the required positive pole piece of the sodium-ion battery.
As a further preferred mode of the invention, a pole piece was prepared as the positive electrode, metallic sodium (Sigma brand) as the negative electrode, Whatman GF/D glass fiber separator as the sodium ion battery separator, and sodium perchlorate electrolyte (NC-008, sovito chemical technologies ltd) was used.
In a further preferred embodiment of the present invention, the manganese-based metal oxide positive electrode has a composition of Na0.55Ni0.1Co0.1Mn0.8O2, and the material can provide an initial specific discharge capacity of 182mAh/g at a low current density of 20 mA/g.
In a further preferred embodiment of the present invention, in step S3, the apparatus is a plasma enhanced atomic layer deposition system (NMT-P-100-42) (the micro/nano technology ltd of china mehneider), and the deposition temperature is 85 ℃.
In a further preferred embodiment of the present invention, in step S3, the produced na0.55ni0.1co0.1mn0.8o2 is a bulk powder having an average size of about 3 μm, and the morphology of the material is not changed after coating with titanium dioxide.
According to the preparation method of the manganese-based metal oxide anode, the coated material has the advantages of high specific capacity, strong circulation stability and good rate performance, the coated coating can effectively improve the circulation stability, prolong the circulation life, effectively relieve the structural stress of the active material caused by repeated sodium insertion/sodium removal, enhance the stability, reduce the contact area of the active material and electrolyte and reduce the occurrence of side reactions.
Drawings
FIG. 1 is a schematic block diagram of the steps of a method for preparing a manganese-based metal oxide positive electrode according to the present invention;
FIG. 2 is a schematic view of a scanning electron microscope of Na0.55Ni0.1Co0.1Mn0.8O2 according to a method for preparing a manganese-based metal oxide positive electrode of the present invention;
FIG. 3 is a schematic view of a scanning electron microscope of Na0.55Ni0.1Co0.1Mn0.8O2/TiO2 according to a method for preparing a manganese-based metal oxide positive electrode of the present invention;
FIG. 4 is a schematic diagram of X-ray diffraction of Na0.55Ni0.1Co0.1Mn0.8O2 (NaNCMO) and Na0.55Ni0.1Co0.1Mn0.8O2/TiO2 (NaNCMO/TiO 2) according to the method for producing a manganese-based metal oxide positive electrode of the present invention;
FIG. 5 is a schematic view of a charge-discharge curve of Na0.55Ni0.1Co0.1Mn0.8O2 at current densities of 20mA/g and 500mA/g according to a method for preparing a manganese-based metal oxide positive electrode of the present invention;
FIG. 6 is a schematic diagram of the specific discharge capacity and coulombic efficiency of Na0.55Ni0.1Co0.1Mn0.8O2 of the manganese-based metal oxide positive electrode preparation method of the present invention for the first 100 turns at a current density of 100 mA/g;
FIG. 7 is a schematic view of a charge-discharge curve of Na0.55Ni0.1Co0.1Mn0.8O2/TiO2 at current densities of 20mA/g and 500mA/g according to a method for preparing a manganese-based metal oxide positive electrode of the present invention;
FIG. 8 is a schematic diagram of the specific discharge capacity and the coulombic efficiency of Na0.55Ni0.1Co0.1Mn0.8O2/TiO2 of the manganese-based metal oxide positive electrode of the invention for the first 100 turns at a current density of 100 mA/g.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: a preparation method of a manganese-based metal oxide positive electrode comprises the following steps:
s1, grinding and firing: grinding cobaltosic oxide, nickel oxide, manganese oxide and sodium carbonate in stoichiometric ratio in an agate mortar, fully grinding, then burning in a muffle furnace at 500 ℃ for 3 hours, and continuing heating to 850 ℃ for 12 hours;
s2, cooling and isolating: cooling to room temperature, and storing the obtained solid powder in an argon-protected glove box to isolate air and moisture;
s3, positive electrode coating: the prepared anode material is directly coated with a layer of titanium dioxide (Na0.55Ni0.1Co0.1Mn0.8O2/TiO 2) with the thickness of about 5 nanometers by an Atomic Layer Deposition (ALD) technology;
s4, preparing material: the active substances are the two manganese-based metal oxide positive electrode materials prepared in the above way, the solvent is N-methyl pyrrolidone (NMP), the conductive agent is acetylene black, the binder is polyvinylidene fluoride (PVDF and the solvent NMP are prepared into a 2.5wt% solution), and the current collector is a carbon-coated aluminum foil;
s5, stirring and mixing: respectively dissolving Na0.55Ni0.1Co0.1Mn0.8O2 and Na0.55Ni0.1Co0.1Mn0.8O2/TiO2, acetylene black serving as a conductive agent and PVDF serving as a binder into NMP according to the mass ratio of 7: 2: 1, and uniformly stirring and mixing;
s6, adding slurry dropwise: uniformly dripping the slurry on a pre-cut circular aluminum foil with the diameter of 12mm by using a liquid-transferring gun;
s7, vacuum drying: and drying the aluminum foil coated with the slurry in a vacuum oven at 80 ℃ for 12 hours to obtain the required positive pole piece of the sodium-ion battery.
Metallic sodium (Sigma brand) was used as the negative electrode, Whatman GF/D glass fiber separator was used as the sodium ion battery separator, and sodium perchlorate electrolyte (NC-008, duo chemical technologies ltd, su) was used. The electrolyte in the electrolyte is sodium perchlorate (NaClO 4), and the solvent is Ethylene Carbonate (EC), diethyl carbonate (DEC) and fluoroethylene carbonate (FEC); NaClO4, which had a composition of 1.0M in the electrolyte, was dissolved in Ethylene Carbonate (EC) + diethyl carbonate (DEC) + fluoroethylene carbonate (FEC) (volume ratio 19: 19: 2). Assembling a positive electrode, a negative electrode, a diaphragm and NC-008 electrolyte into a CR-2032 button cell, and assembling the cell in an argon-protected glove box; the assembled cells were performed under the newwe (Neware, shenzhen new wil electronics ltd) cell testing system.
The manganese-based metal oxide positive electrode is composed of Na0.55Ni0.1Co0.1Mn0.8O2, the material can provide initial specific discharge capacity of 182mAh/g under the low current density of 20mA/g, the material coated by titanium dioxide can still provide reversible specific discharge capacity of 109mAh/g even under the current density of 500mA/g, the reversible specific discharge capacity of 126mAh/g still exists after 100mA/g circulation and 100 circles, and the capacity retention rate is as high as 85.7%.
In step S3, the device is a plasma enhanced atomic layer deposition system (NMT-P-100-42, mfd. micro nano technology ltd., j. su) with a deposition temperature of 85 ℃.
In step S3, the prepared na0.55ni0.1co0.1mn0.8o2 was bulk powder having an average size of about 3 μm, and the morphology of the material was not changed after coating with titanium dioxide.
Wherein the manganese-based metal oxide positive electrode has the composition of Na0.55Ni0.1Co0.1Mn0.8O2, and the material can provide initial specific discharge capacity of 182mAh/g under the low current density of 20 mA/g.
The X-ray diffraction pattern of the prepared Na0.55Ni0.1Co0.1Mn0.8O2 shows that the material belongs to a P63/mmc space group (PDF # 54-0894), and the diffraction peak of titanium dioxide is not seen in the coated material, which is attributed to the ultrathin coating thickness of the metal oxide and the amorphous property of the ultrathin coating thickness.
Na0.55Ni0.1Co0.1Mn0.8O2 and Na0.55Ni0.1Co0.1Mn0.8O2/TiO2 both provided initial specific discharge capacity of 182mAh/g at a low current density of 20mA/g, and Na0.55Ni0.1Co0.1Mn0.8O2/TiO2 still provided reversible specific discharge capacity of 109mAh/g when the current density was increased to 500mA/g, whereas Na0.55Ni0.1Co0.1Mn0.8O2 had reduced specific discharge capacity to 87mAh/g at the same current density. The titanium dioxide coating coated by the ALD technology greatly enhances the rate capability of the material; at the same time, the capacity retention of the coated material after 100 cycles at 100mA/g increased from 73.8% to 85.7% of the uncoated material.
In conclusion, the preparation method of the manganese-based metal oxide positive electrode has the advantages that the coated material has high specific capacity, strong cycling stability and good rate performance, the coated coating can effectively improve the cycling stability, prolong the cycling life, effectively relieve the structural stress of the active material caused by repeated sodium insertion/sodium removal, enhance the stability, reduce the contact area of the active material and the electrolyte and reduce the occurrence of side reactions.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (5)
1. The preparation method of the manganese-based metal oxide positive electrode is characterized by comprising the following preparation steps of:
s1, grinding and firing: grinding cobaltosic oxide, nickel oxide, manganese oxide and sodium carbonate in stoichiometric ratio in an agate mortar, fully grinding, then burning in a muffle furnace at 500 ℃ for 3 hours, and continuing heating to 850 ℃ for 12 hours;
s2, cooling and isolating: cooling to room temperature, and storing the obtained solid powder in an argon-protected glove box to isolate air and moisture;
s3, positive electrode coating: the prepared anode material is directly coated with a layer of titanium dioxide (Na0.55Ni0.1Co0.1Mn0.8O2/TiO 2) with the thickness of about 5 nanometers by an Atomic Layer Deposition (ALD) technology;
s4, preparing material: the active substances are the two manganese-based metal oxide positive electrode materials prepared in the above way, the solvent is N-methyl pyrrolidone (NMP), the conductive agent is acetylene black, the binder is polyvinylidene fluoride (PVDF and the solvent NMP are prepared into a 2.5wt% solution), and the current collector is a carbon-coated aluminum foil;
s5, stirring and mixing: respectively dissolving Na0.55Ni0.1Co0.1Mn0.8O2 and Na0.55Ni0.1Co0.1Mn0.8O2/TiO2, acetylene black serving as a conductive agent and PVDF serving as a binder into NMP according to the mass ratio of 7: 2: 1, and uniformly stirring and mixing;
s6, adding slurry dropwise: uniformly dripping the slurry on a pre-cut circular aluminum foil with the diameter of 12mm by using a liquid-transferring gun;
s7, vacuum drying: and drying the aluminum foil coated with the slurry in a vacuum oven at 80 ℃ for 12 hours to obtain the required positive pole piece of the sodium-ion battery.
2. The method of claim 1, wherein the prepared sheet is used as a positive electrode, metallic sodium (Sigma brand) is used as a negative electrode, a Whatman GF/D glass fiber separator is used as a sodium ion battery separator, and a sodium perchlorate electrolyte (NC-008, Suzhou Dooduo chemical technology Co., Ltd.) is used.
3. The method of claim 1, wherein the positive electrode comprises Na0.55Ni0.1Co0.1Mn0.8O2, and the material provides an initial specific discharge capacity of 182mAh/g at a low current density of 20 mA/g.
4. The method of claim 1, wherein in step S3, the device is a plasma enhanced atomic layer deposition system (NMT-P-100-42) (micro nano technology ltd) with a deposition temperature of 85 ℃.
5. The method of claim 1, wherein in step S3, the produced na0.55ni0.1co0.1mn0.8o2 is a bulk powder having an average size of about 3 μm, and the titanium dioxide is coated without changing the morphology of the material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114447301A (en) * | 2022-01-21 | 2022-05-06 | 合肥国轩高科动力能源有限公司 | Ternary cathode material, preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114447301A (en) * | 2022-01-21 | 2022-05-06 | 合肥国轩高科动力能源有限公司 | Ternary cathode material, preparation method and application thereof |
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Application publication date: 20210316 |