CN111668445A - Shape-controllable nickel manganese oxide electrode material and preparation method and application thereof - Google Patents

Shape-controllable nickel manganese oxide electrode material and preparation method and application thereof Download PDF

Info

Publication number
CN111668445A
CN111668445A CN202010484518.2A CN202010484518A CN111668445A CN 111668445 A CN111668445 A CN 111668445A CN 202010484518 A CN202010484518 A CN 202010484518A CN 111668445 A CN111668445 A CN 111668445A
Authority
CN
China
Prior art keywords
mixed solution
electrode material
manganese oxide
oxide electrode
nickel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010484518.2A
Other languages
Chinese (zh)
Inventor
李俊鹏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangdong Industry Technical College
Original Assignee
Guangdong Industry Technical College
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangdong Industry Technical College filed Critical Guangdong Industry Technical College
Priority to CN202010484518.2A priority Critical patent/CN111668445A/en
Publication of CN111668445A publication Critical patent/CN111668445A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0416—Methods of deposition of the material involving impregnation with a solution, dispersion, paste or dry powder
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of 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
    • H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
    • 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
    • H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention belongs to the technical field of electrode materials, and discloses a nickel manganese oxide electrode material with controllable morphology as well as a preparation method and application thereof. The nickel manganese oxide electrode material is prepared by dissolving nickel nitrate and manganese nitrate in absolute ethyl alcohol, stirring and mixing to obtain a mixed solution A; dissolving glycerol in absolute ethyl alcohol, stirring and mixing to prepare a mixed solution B; dropwise adding the mixed solution B into the mixed solution A, and stirring to obtain a mixed solution C; then, dripping the urea aqueous solution into the mixed solution C, stirring, transferring to a high-pressure reaction kettle, reacting at 120-200 ℃, naturally cooling to room temperature, and precipitatingCentrifugally washing the starch, and drying in vacuum to obtain NiMnCO3A precursor; mixing NiMnCO3The precursor is calcined at 650-850 ℃ to obtain the catalyst. According to the invention, the crystal orientation growth in the reaction process is changed through the solvent proportion, so that the NiMnO electrode material has the advantage of controllable morphology, and the performance of the battery material is improved.

Description

Shape-controllable nickel manganese oxide electrode material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a nickel manganese oxide electrode material with controllable morphology as well as a preparation method and application thereof.
Background
With the gradual exhaustion of fossil energy and the gradual protrusion of urban environment deterioration problems, the optimal scheme of urban traffic is the large-scale application of electric vehicles. The lithium ion battery is the optimal choice for the electric automobile due to high energy density, long cycle life and no memory effect. However, the current universal negative electrode material is graphite, the theoretical specific capacity of the graphite is very low (372mAh/g), and the requirement of a high-energy density battery cannot be met. The new generation of cathode material is required to be developed to meet the requirement of high-endurance electric vehicles. The theoretical specific capacity of the metal oxide negative electrode material is far greater than that of graphite, so the development of the metal oxide negative electrode material has great scientific significance.
The nickel element with rich earth content has strong ductility and corrosion resistance, and can obviously improve the stability and activity of the electrode material. The other transition metal element manganese with rich content is also an important electrode material raw material. The performance of the electrode material is closely related to the synthesis method. Conventional synthetic methods such as precipitation and wet impregnation have been gradually eliminated due to the inability to control the concentration gradient and dispersion of the metal particles. In recent years, a method in which a surfactant is combined with a conventional coprecipitation method has been proposed and widely used for the preparation of electrode materials. The surface tension and interfacial energy of water in the pores can be reduced by the hydroxyl proton exchange effect between the surfactant and the aqueous metal hydroxide gel. Therefore, synthesis of an oxide electrode material with a high specific surface area can be assisted. The surfactant has unique self-organizing ability in an interface or a solution, can change the interface property and enhance the compatibility between different material materials.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide a nickel manganese oxide electrode material with controllable morphology.
The invention also aims to provide a preparation method of the nickel manganese oxide electrode material with controllable morphology.
The invention further aims to provide application of the nickel manganese oxide electrode material with controllable morphology.
The purpose of the invention is realized by the following technical scheme:
a nickel manganese oxide electrode material with controllable appearance,the nickel manganese oxide electrode material is prepared by dissolving nickel nitrate and manganese nitrate in absolute ethyl alcohol, stirring and mixing to obtain a mixed solution A; dissolving glycerol in absolute ethyl alcohol, stirring and mixing to prepare a mixed solution B; dropwise adding the mixed solution B into the mixed solution A, and stirring to obtain a mixed solution C; then, dripping the urea aqueous solution into the mixed solution C, stirring, transferring to a high-pressure reaction kettle, reacting at 120-200 ℃, naturally cooling to room temperature, centrifugally washing the obtained precipitate, drying in vacuum, and obtaining the NiMnCO3The precursor is calcined at 650-850 ℃ to obtain the catalyst.
Preferably, the molar ratio of nickel ions to manganese ions in the mixed solution a is 1: (1-3).
Preferably, the mass ratio of the total mass of the nickel nitrate and the manganese nitrate to the absolute ethyl alcohol is (10-15): 1.
preferably, the volume ratio of the glycerol to the absolute ethyl alcohol is 1: (1-3).
Preferably, the volume ratio of the mixed solution B to the mixed solution A is 1: (1-3).
Preferably, the mass ratio of urea to water in the urea aqueous solution is 1: (100-500).
Preferably, the mass ratio of the urea aqueous solution to the mixed solution C is 1: (1-3).
Preferably, the reaction time at 120-200 ℃ is 5-12 h, the stirring time is 1-3 h, the vacuum drying time is 4-8 h, and the calcining time is 1-3 h.
The preparation method of the nickel manganese oxide electrode material with controllable morphology comprises the following specific steps:
s1, dissolving nickel nitrate and manganese nitrate in absolute ethyl alcohol, and stirring at room temperature to uniformly mix the solution to obtain a mixed solution A; dissolving glycerol in absolute ethyl alcohol, and stirring at room temperature to uniformly mix the glycerol and the absolute ethyl alcohol to obtain a mixed solution B; dropwise adding the mixed solution B into the mixed solution A, and continuously stirring to prepare a mixed solution C;
s2, dripping the urea aqueous solution into the mixed solution C, stirring at room temperature, transferring to a high-pressure reaction kettle, reacting at 120-200 ℃, naturally cooling to room temperature,centrifugally washing the obtained precipitate, and drying the precipitate in vacuum at the temperature of 80-120 ℃ to obtain NiMnCO3A precursor;
s3, mixing NiMnCO3And calcining the precursor at 650-850 ℃ to prepare the nickel-manganese oxide electrode material.
The nickel manganese oxide electrode material with controllable morphology is applied to the preparation of lithium ion batteries.
The invention successfully synthesizes the NiMnO electrode material by the surfactant-assisted solvothermal reaction. Urea is used as a precipitator, a surfactant glycerol is used as a morphology regulating agent, and the following ionic reactions occur in the solvothermal process: ni2++Mn2++CO3 2-→NiMnCO3. The following reaction occurs during the calcination at 650-850 ℃ (preferably 750 ℃): NiMnCO3→NiMnO+CO2. Different glycerol amounts lead to different morphologies of the electrode material. Glycerol can prevent NiMnCO3Aggregation and compression. While glycerol of greater mass represents more molecular chains, making it more likely that glycerol molecules will become entangled or helical with other glycerol molecules through hydrogen bonds. NiMnCO3Roasting at 650-850 deg.C (preferably 750 deg.C), and mixing with glycerol and CO2The volatilization of the alcohol can lead rich holes to appear in the NiMnO structure, and the electrode material added with the glycerol has a macroporous structure. With the addition of glycerol, flakes appear on the surface of the prepared NiMnO electrode material. Wherein, the addition amount of the glycerol is 6g, a good petal-shaped sheet is formed, the specific area is large, and the specific capacity of the battery is the highest.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the crystal orientation growth in the reaction process is changed through the solvent proportion, so that the NiMnO electrode material has the advantage of controllable morphology, and the performance of the battery material is improved.
2. The NiMnO electrode material is synthesized by adopting a glycerol-assisted solvothermal method, the preparation process is simple, the operation is convenient, and meanwhile, the large-scale production is easy, so that the requirements of modern chemistry and industrialization are completely met;
3. the pore structure and the electrochemical performance of the NiMnO electrode material can be controlled by changing the addition of the glycerol, so that a new idea is provided for the controllable synthesis of other surfactants in the electrode material;
4. the invention can improve the understanding of the special function of the surface active agent in the electrochemical reaction process by accurately exploring the action mechanism of the protective agent glycerol, and is favorable for guiding the accurate preparation of the novel electrode material.
5. The NiMnO electrode material with the surfactant glycerol added in an amount of 6g has abundant petal-shaped scales, large specific surface area, high reaction efficiency and best battery performance.
Drawings
FIG. 1 is an SEM photograph of the nickel manganese oxide material obtained in examples 1-3.
FIG. 2 is an XRD spectrum of the nickel manganese oxide material obtained in examples 1-3.
FIG. 3 shows the specific surface area and pore size distribution of the nickel manganese oxide material obtained in examples 1 to 3.
FIG. 4 is a second charge-discharge curve of the nickel manganese oxide material prepared in examples 1-3 at a current density of 100 mA/g.
FIG. 5 is a graph of the cycling performance of the nickel manganese oxide materials prepared in examples 1-3 at a current density of 100 mA/g.
FIG. 6 is a graph of rate capability of nickel manganese oxide materials prepared in examples 1-3.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
1. Weighing nickel nitrate (2.43g) and manganese nitrate (6.67g) to dissolve in 50mL of absolute ethanol, and stirring for 3 hours at room temperature by using a magnetic stirrer to form a uniform mixed solution;
2. dissolving 8g of urea in 10mL of deionized water, dropwise adding the solution into the mixed solution obtained in the step 1, stirring the solution at room temperature for 2 hours, transferring the solution to a high-pressure reaction kettle with a polyvinyl fluoride lining,sealing, reacting at 180 deg.C for 10h, naturally cooling to room temperature, centrifuging and washing the obtained precipitate, and drying at 80 deg.C for 6h in vacuum drying oven to obtain NiMnCO3A precursor of the compound (I) is prepared,
3. mixing NiMnCO3And calcining the precursor in a muffle furnace at 750 ℃ for 2h to obtain the NiMnO electrode material (marked as NMO).
Example 2
1. Weighing nickel nitrate (2.43g) and manganese nitrate (6.67g) to dissolve in 50mL of absolute ethanol, and stirring for 3 hours at room temperature by using a magnetic stirrer to form a uniform mixed solution;
2. dissolving 4g of surfactant glycerol in 1mL of absolute ethyl alcohol to form a uniform mixed solution, then dropwise adding the mixed solution into the mixed solution in which nickel salt and manganese salt are dissolved, and continuously stirring for 1 h; dissolving 8g of urea in 10mL of deionized water, dropwise adding the solution into the mixed solution obtained in the step 1, stirring the solution at room temperature for 2 hours, transferring the solution into a high-pressure reaction kettle with a polyvinyl fluoride lining, sealing the reaction kettle, reacting the solution at 180 ℃ for 10 hours, naturally cooling the reaction kettle to room temperature, centrifugally washing the obtained precipitate, drying the precipitate in a vacuum drying oven at 80 ℃ for 6 hours to obtain NiMnCO3And transferring the precursor to a muffle furnace, and calcining at 750 ℃ for 2h to obtain the NiMnO electrode material (marked as NMO-glycerol-4 g).
Example 3
1. Weighing nickel nitrate (2.43g) and manganese nitrate (6.67g) to dissolve in 50mL of absolute ethanol, and stirring for 3 hours at room temperature by using a magnetic stirrer to form a uniform mixed solution;
2. dissolving 6g of surfactant glycerol in 1mL of absolute ethyl alcohol to form a uniform mixed solution, then dropwise adding the mixed solution into the mixed solution in which nickel salt and manganese salt are dissolved, and continuously stirring for 1 h; dissolving 8g of urea in 10mL of deionized water, dropwise adding the solution into the mixed solution obtained in the step 1, stirring the solution at room temperature for 2 hours, transferring the solution to a high-pressure reaction kettle with a polyvinyl fluoride lining, sealing the reaction kettle, reacting the solution at 180 ℃ for 10 hours, naturally cooling the reaction kettle to room temperature, centrifugally washing the obtained precipitate, and drying the precipitate at 80 ℃ in a vacuum drying oven for 6 hours to obtain NiMnCO3A precursor;
3. mixing NiMnCO3Transferring the precursor to a muffle furnace, calcining at 750 ℃ for 2h to obtain a NiMnO electrode material (marked as NMO-glycerol)-6g)。
Uniformly mixing a NiMnO electrode material with Super-P and PVDF (the mass ratio is 7: 2: 1), stirring the mixture in N-methylpyrrolidone to form a uniform suspension, coating the suspension on a copper foil, and drying the copper foil in a drying oven at 60 ℃ for 10 hours to obtain a lithium ion battery negative plate; to obtain the lithium ion battery cathode plate, 1M LiPF6The electrolyte is dissolved in EC, DEC and DMC mixed solvent (volume ratio is 1: 1: 1), Celgard 2400 polypropylene membrane is used as a diaphragm, a lithium sheet is used as a counter electrode, and the diaphragm are assembled into a CR2032 button cell in a glove box filled with argon.
FIG. 1 is an SEM photograph of the nickel manganese oxide material obtained in examples 1-3. Wherein, (a) NMO, (b) NMO-glycerol-4 g, and (c) NMO-glycerol-6 g. As can be seen from FIG. 1, spherical NiMnO electrode materials of different sizes were prepared by the solvothermal method without adding a glycerol surfactant. Adding 4g of glycerol surfactant in the solvothermal reaction process to prepare the nickel-manganese oxide material with irregular flakes distributed on the structural surface. Figure 2 is an XRD pattern of nickel manganese oxide material. As can be seen from fig. 2, the material obtained in example 1 is nickel manganese metal oxide. The diffraction peaks of the nickel manganese oxide materials prepared in examples 2 and 3 after adding glycerol are consistent with those of the nickel manganese oxide materials without adding the surfactant, and the nickel manganese oxide materials are nickel manganese oxide. Fig. 3 is a plot of specific surface area and pore size distribution for nickel manganese oxide materials. Wherein, (a) is a low-temperature nitrogen adsorption and desorption curve, and (b) is a pore size distribution curve. As can be seen from FIG. 3, the NiMnO electrode material without glycerol (example 1) has only a few micropores and is in the form of spheres of 4 to 7 μm. The porosity of the nickel-manganese oxide material prepared by adding glycerol (embodiment 2) is obviously improved, and macropores are formed in the structure of the nickel-manganese oxide material prepared by adding 6g of glycerol (embodiment 3), so that the contact surface of the material and electrolyte can be improved, and the multiplying power performance of the material can be improved. FIG. 4 is a second charge-discharge curve of the nickel manganese oxide material prepared in examples 1-3 at a current density of 100 mA/g. FIG. 5 is a graph of the cycling performance of the nickel manganese oxide materials prepared in examples 1-3 at a current density of 100 mA/g. As can be seen from FIGS. 4 and 5, the specific discharge capacity of the second time is 842mAh/g and the capacity retention rate is 19% after 50 charge-discharge cycles according to the charge-discharge of 100mA/g current density; the specific capacity of the nickel-manganese oxide material prepared in the embodiment 2 reaches 972mAh/g in the second discharge under the current density of 100mA/g, the capacity retention rate is 30% after 50 cycles, the specific capacity of the nickel-manganese oxide material prepared in the embodiment 3 reaches 1046mAh/g in the second discharge under the current density of 100mA/g after glycerol is added, and the capacity retention rate is 60% after 50 cycles, which indicates that the cycle stability is obviously improved. FIG. 6 is a graph of rate capability of nickel manganese oxide materials prepared in examples 1-3. As can be seen from fig. 6, the large current discharge performance of the nickel-manganese oxide material prepared in examples 2 and 3 by adding glycerol is significantly improved. The specific discharge capacity of the nickel-manganese oxide material prepared in the example 3 is 278mA/g at the current density of 5000mA/g, which shows that the prepared nickel-manganese oxide material has excellent rate capability.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. The nickel manganese oxide electrode material is characterized in that nickel nitrate and manganese nitrate are dissolved in absolute ethyl alcohol and are stirred and mixed to prepare a mixed solution A; dissolving glycerol in absolute ethyl alcohol, stirring and mixing to prepare a mixed solution B; dropwise adding the mixed solution B into the mixed solution A, and stirring to obtain a mixed solution C; then, dripping the urea aqueous solution into the mixed solution C, stirring, transferring to a high-pressure reaction kettle, reacting at 120-200 ℃, naturally cooling to room temperature, centrifugally washing the obtained precipitate, drying in vacuum, and obtaining the NiMnCO3The precursor is calcined at 650-850 ℃ to obtain the catalyst.
2. The morphology-controllable nickel manganese oxide electrode material according to claim 1, wherein the molar ratio of nickel ions to manganese ions in the mixed solution A is 1: (1-3).
3. The morphology-controllable nickel manganese oxide electrode material according to claim 1, wherein the mass ratio of the total mass of nickel nitrate and manganese nitrate to absolute ethyl alcohol is (10-15): 1.
4. the topography controlled nickel manganese oxide electrode material according to claim 1, wherein the volume ratio of glycerol to absolute ethyl alcohol is 1: (1-3).
5. The morphology-controllable nickel manganese oxide electrode material according to claim 1, wherein the volume ratio of the mixed solution B to the mixed solution A is 1: (1-3).
6. The topography controllable nickel manganese oxide electrode material according to claim 1, wherein the mass ratio of urea to water in the urea aqueous solution is 1: (100-500).
7. The shape-controllable nickel manganese oxide electrode material as claimed in claim 1, wherein the mass ratio of the urea aqueous solution to the mixed solution C is 1: (1-3).
8. The shape-controllable nickel manganese oxide electrode material as claimed in claim 1, wherein the reaction time at 120-200 ℃ is 5-12 h, the stirring time is 1-3 h, the vacuum drying time is 4-8 h, and the calcination time is 1-3 h.
9. The preparation method of the morphology-controllable nickel manganese oxide electrode material according to any one of claims 1 to 8, characterized by comprising the following specific steps:
s1, dissolving nickel nitrate and manganese nitrate in absolute ethyl alcohol, and stirring at room temperature to uniformly mix the solution to obtain a mixed solution A; dissolving glycerol in absolute ethyl alcohol, and stirring at room temperature to uniformly mix the glycerol and the absolute ethyl alcohol to obtain a mixed solution B; dropwise adding the mixed solution B into the mixed solution A, and continuously stirring to prepare a mixed solution C;
s2, then dripping the urea aqueous solution into the mixed solution CStirring at room temperature, transferring the mixture to a high-pressure reaction kettle for reaction at 120-200 ℃, naturally cooling to room temperature, centrifugally washing the obtained precipitate, and vacuum drying at 80-120 ℃ to obtain NiMnCO3A precursor;
s3, mixing NiMnCO3And calcining the precursor at 650-850 ℃ to prepare the nickel-manganese oxide electrode material.
10. Use of the topographically controllable nickel manganese oxide electrode material of any one of claims 1 to 8 in the preparation of a lithium ion battery.
CN202010484518.2A 2020-06-01 2020-06-01 Shape-controllable nickel manganese oxide electrode material and preparation method and application thereof Pending CN111668445A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010484518.2A CN111668445A (en) 2020-06-01 2020-06-01 Shape-controllable nickel manganese oxide electrode material and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010484518.2A CN111668445A (en) 2020-06-01 2020-06-01 Shape-controllable nickel manganese oxide electrode material and preparation method and application thereof

Publications (1)

Publication Number Publication Date
CN111668445A true CN111668445A (en) 2020-09-15

Family

ID=72385502

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010484518.2A Pending CN111668445A (en) 2020-06-01 2020-06-01 Shape-controllable nickel manganese oxide electrode material and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN111668445A (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105742624A (en) * 2016-04-14 2016-07-06 河北工业大学 Preparation method of spherical lithium nickel manganese oxide material with hollow porous micro-nano level structure
CN106711443A (en) * 2016-12-16 2017-05-24 中南大学 Fusiform manganese cobalt oxide material and preparation and application thereof
CN107658451A (en) * 2017-09-18 2018-02-02 北京理工大学 A kind of 622NCM tertiary cathode materials and preparation method thereof
CN108493004A (en) * 2018-03-28 2018-09-04 江苏大学 A kind of preparation method and application of the ferric oxide nano-material of morphology controllable
CN110127767A (en) * 2019-06-11 2019-08-16 北京理工大学 A kind of preparation method of multi-level flower-like manganese base nano-sheet lithium ion battery positive electrode
US20190312265A1 (en) * 2018-04-08 2019-10-10 Microvast Power Systems Co., Ltd. Method for preparing cathode particles and cathode active materials having same
US20200131046A1 (en) * 2017-07-15 2020-04-30 Microvast Power Systems Co., Ltd. Method and apparatus for producing cathode particles

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105742624A (en) * 2016-04-14 2016-07-06 河北工业大学 Preparation method of spherical lithium nickel manganese oxide material with hollow porous micro-nano level structure
CN106711443A (en) * 2016-12-16 2017-05-24 中南大学 Fusiform manganese cobalt oxide material and preparation and application thereof
US20200131046A1 (en) * 2017-07-15 2020-04-30 Microvast Power Systems Co., Ltd. Method and apparatus for producing cathode particles
CN107658451A (en) * 2017-09-18 2018-02-02 北京理工大学 A kind of 622NCM tertiary cathode materials and preparation method thereof
CN108493004A (en) * 2018-03-28 2018-09-04 江苏大学 A kind of preparation method and application of the ferric oxide nano-material of morphology controllable
US20190312265A1 (en) * 2018-04-08 2019-10-10 Microvast Power Systems Co., Ltd. Method for preparing cathode particles and cathode active materials having same
CN110127767A (en) * 2019-06-11 2019-08-16 北京理工大学 A kind of preparation method of multi-level flower-like manganese base nano-sheet lithium ion battery positive electrode

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈亚杰: "《纳米TiO2及其复合体的控制合成与性能研究》", 30 June 2014 *

Similar Documents

Publication Publication Date Title
CN109167056B (en) Tungsten ion doped high-nickel layered oxide lithium battery positive electrode material and preparation method thereof
CN108878818A (en) Core-shell structure nickel-cobalt-manganternary ternary anode material presoma and preparation method thereof
CN115498177A (en) Positive electrode active material, preparation method thereof, positive electrode plate and sodium ion battery
WO2015039490A1 (en) Lithium-rich anode material and preparation method thereof
CN108899531A (en) A kind of preparation method of Phosphate coating nickel cobalt aluminium tertiary cathode material
CN110429268A (en) A kind of modified boron doping lithium-rich manganese-based anode material and the preparation method and application thereof
CN110323432A (en) A kind of miscellaneous modification lithium-ion battery anode material of cation-anion co-doping and preparation method thereof
CN108767216A (en) Anode material for lithium-ion batteries and its synthetic method with the full concentration gradient of variable slope
CN107732235A (en) A kind of ternary cathode material of lithium ion battery NCA preparation method
CN111525119B (en) Lithium-sulfur battery positive electrode material and preparation method thereof
CN110233261B (en) Preparation method of single crystal ternary lithium battery positive electrode material and lithium ion battery
CN113659141A (en) SiO @ Mg/C composite material and preparation method and application thereof
CN111490241A (en) Lithium phosphate in-situ coated lithium-rich manganese-based positive electrode material and preparation method thereof
CN109860536A (en) A kind of lithium-rich manganese base material and its preparation method and application
CN110085854B (en) Lithium vanadium phosphate cathode material and preparation method thereof
CN111211320A (en) Lithium nickel cobalt oxide positive electrode material, preparation method thereof and lithium ion battery
CN110197902B (en) Porous structure open walnut shell-shaped sodium ion battery positive electrode material and preparation method thereof
CN114933292B (en) Preparation method and application of lithium iron phosphate
CN114715956B (en) Modified porous nickel-rich positive electrode material and preparation method thereof
CN111640923B (en) Lithium nickel manganese oxide positive electrode material and preparation method thereof
CN112436135B (en) Cathode material and preparation method and application thereof
CN115172704A (en) Preparation method for preparing porous carbon lithium iron phosphate cathode material by using metal organic framework
CN108695501A (en) A kind of ultrasonic atomizatio preparation method of nickel, cobalt and manganese oxide negative material
CN114864932A (en) Preparation method of sodium ion battery positive electrode material
CN111668445A (en) Shape-controllable nickel manganese oxide electrode material and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200915