CN115504527A - Method for preparing ternary nano material by inducing nanofiber template, product and application - Google Patents

Method for preparing ternary nano material by inducing nanofiber template, product and application Download PDF

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CN115504527A
CN115504527A CN202211401243.7A CN202211401243A CN115504527A CN 115504527 A CN115504527 A CN 115504527A CN 202211401243 A CN202211401243 A CN 202211401243A CN 115504527 A CN115504527 A CN 115504527A
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manganese
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崔大祥
吴晓燕
林琳
陈超
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/40—Nickelates
    • C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
    • C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
    • C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
    • 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
    • H01M4/36—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
    • H01M4/36—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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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
    • H01M2004/028—Positive 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

Abstract

The invention provides a preparation method for preparing a ternary nano material by inducing a nano fiber template, and a product and application thereof, wherein polyvinylidene fluoride is dissolved in a mixed solvent of N, N-dimethylformamide and acetone, and is heated and dissolved; adding soluble manganese salt, continuously stirring until a uniform solution is formed, and preparing the PVDF/manganese salt nano fiber felt by adopting an electrostatic spinning method; and (3) carrying out low-temperature treatment on the PVDF/manganese salt nano fiber felt to obtain PVDF/manganese dioxide nano powder. Dissolving lithium salt, nickel salt, cobalt salt, PVDF/manganese dioxide and nitric acid in deionized water, and stirring to obtain a uniform and clear precursor solution; adding the mixed solution into a sodium hydroxide alkali solution, moving the mixed solution into a hydrothermal kettle, and carrying out hydrothermal reaction in an oven; and centrifuging a product after reaction, washing the precipitate obtained after centrifugation for many times by using deionized water and absolute ethyl alcohol, calcining the precipitate in a muffle furnace, and porphyrizing the calcined precipitate by using an agate mortar to obtain the ternary nano material.

Description

Method for preparing ternary nano material by inducing nanofiber template, product and application
Technical Field
The invention relates to a preparation method of a lithium battery anode material, in particular to a method for preparing a ternary nano material by inducing a nano fiber template, and a product and application thereof.
Background
With the rapid development of smaller, lighter and higher performance electronic and communication devices, there is an increasing demand for the performance of batteries that provide power sources for these devices, particularly with respect to energy. However, the specific capacities of lithium ion batteries and MH/Ni batteries which are commercialized at present are difficult to be improved continuously. Therefore, the development of batteries with higher specific energy is urgently required. Lithium ion secondary batteries have been widely used as high specific energy chemical power sources in the fields of mobile communication, notebook computers, video cameras, portable instruments and meters, etc., and have rapidly developed into one of the most important secondary batteries at present. Lithium ion batteries, which are the latest generation of green high-energy storage batteries, have been rapidly developed in the early 90 s of the 20 th century, and are favored because of their advantages of high voltage, high energy density, long cycle life, little environmental pollution, and the like.
The ternary material is the first choice material of the lithium battery due to low price and stable performance. Since the ternary material LiNi1-x-yCoxMnyO2 (0 yarn-x yarn-1 and 0 yarn-y yarn-1) has the characteristics superior to those of lithium iron phosphate and lithium cobaltate, and the ternary electrode materials with different performances can be prepared by adjusting the proportion of nickel, cobalt and manganese. With the rise and development of new energy automobiles, ternary materials become a research hotspot.
The invention provides a preparation method for preparing a ternary nano material by inducing a nano fiber template, and the ternary nano material prepared by the method has smaller particles, larger specific surface area and important effect on improving the electrochemical performance of the material. The preparation process is relatively simple and easy to operate.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for preparing a ternary nano material by inducing a nano fiber template.
Still another object of the present invention is to: there is provided a product obtained by the above process.
Yet another object of the present invention is: provides an application of the product.
The invention aims to realize the following scheme, and the preparation method for preparing the ternary nano material by inducing the nano fiber template comprises the following specific steps:
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 1~4:1; heating the solution to 50-55 ℃ until polyvinylidene fluoride is completely dissolved;
(2) Adding soluble manganese salt into the solution, continuously stirring the solution until a uniform solution is formed, and preparing the PVDF/manganese salt nano fiber felt by adopting an electrostatic spinning method under the voltage of 10 to 15 KV; the distance between the receiving plate and the spinning end is 10 to 15 cm;
(3) And (3) carrying out low-temperature treatment on the PVDF/manganese salt nano fiber felt, and carrying out heat treatment at 140-180 ℃ for 12-24 h to obtain PVDF/manganese dioxide nano powder.
(4) Dissolving lithium salt, nickel salt, cobalt salt, PVDF/manganese dioxide and 1 mL nitric acid in deionized water to enable the molar weight ratio of the lithium salt, the nickel salt, the cobalt salt and the PVDF/manganese dioxide to be 1: 1-x-y: x: y, and stirring to obtain uniform and clear precursor liquid; adding the mixed solution into 15 mL sodium hydroxide alkali solution, moving the mixed solution into a 25 mL hydrothermal kettle, and carrying out hydrothermal reaction in an oven at 180-200 ℃ for 1-3 h; and centrifuging a product after reaction, washing precipitates obtained after centrifugation for many times by using deionized water and absolute ethyl alcohol, calcining the precipitates in a muffle furnace at 400-500 ℃ for 2-3 h, and grinding the calcined precipitates in an agate mortar to obtain the ternary nano material.
The manganese salt is one or the combination of manganese acetate and manganese formate.
The lithium salt is one or a combination of lithium acetate and lithium formate.
The nickel salt is one or the combination of nickel acetate and nickel formate.
The soluble cobalt salt is one or the combination of cobalt acetate and cobalt formate.
A method for preparing a ternary nano material by inducing a nanofiber template is prepared by any one of the methods.
An application of a ternary nano material prepared by inducing a nano fiber template in a lithium ion battery anode material.
Compared with the prior art, the invention has the following beneficial effects: the invention provides a preparation method for preparing a ternary nano material by inducing a nano fiber template, and the ternary nano material prepared by the method has smaller particles, larger specific surface area and important effect on improving the electrochemical performance of the material. The preparation process is relatively simple and easy to operate.
Drawings
FIG. 1 is a graph of the visible light catalytic degradation rate of the zinc sulfide/carbon nanotube fiber photocatalytic material of example 1.
Detailed Description
The present invention is described in detail by the following specific examples, but the scope of the present invention is not limited to these examples.
Example 1
A ternary nano material prepared by inducing a nanofiber template is prepared by the following steps:
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 1:1; heating the solution to 50 ℃ until polyvinylidene fluoride is completely dissolved to obtain a PVDF solution;
(2) Adding soluble manganese acetate into the solution obtained in the step (1), continuously stirring until a uniform solution is formed, and preparing the PVDF/manganese acetate nano fiber felt by adopting an electrostatic spinning method under the voltage of 10 KV; and the distance between the receiving plate and the spinning end is 15 cm;
(3) Carrying out heat treatment on the PVDF/manganese acetate nano fiber felt at the temperature of 140-180 ℃ for 12-24h to obtain PVDF/manganese dioxide nano powder;
(4) Dissolving lithium acetate, nickel acetate, cobalt acetate, PVDF/manganese dioxide nano powder and 1 mL nitric acid in deionized water to ensure that the molar weight ratio of the lithium acetate, the nickel acetate, the cobalt acetate and the PVDF/manganese dioxide is 0.01mol to 0.0033mol to 0.0033mol, and stirring to obtain uniform and clear precursor solution; adding the precursor solution into 15 mL sodium hydroxide alkali solution, moving the solution to a 25 mL hydrothermal kettle, and carrying out hydrothermal reaction in an oven at 180 ℃ for 3 hours; and centrifuging the product after reaction, washing the precipitate obtained after centrifugation for many times by using deionized water and absolute ethyl alcohol, then calcining the precipitate in a muffle furnace at 400 ℃ for 3 hours, and grinding the calcined precipitate by using an agate mortar to obtain the ternary nano material.
The specific surface area of the ternary nano material is 21.2 m 2 /g。
FIG. 1 is a cycle life diagram of the ternary nano-material at a rate of 1C, the first specific discharge capacity of the ternary nano-material is 188.5 mAh/g, the specific discharge capacity of the ternary nano-material after 50 cycles is 178.3 mAh/g, and the specific capacity retention rate is 94.6%.
Example 2
A ternary nano material prepared by inducing a nanofiber template is prepared by the following steps:
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 3:1; heating the solution to 55 ℃ until the polyvinylidene fluoride is completely dissolved to obtain a PVDF solution;
(2) Adding soluble manganese formate into the solution obtained in the step (1), continuously stirring until a uniform solution is formed, and preparing the PVDF/manganese salt nano fiber felt by adopting an electrostatic spinning method under the voltage of 10 KV; and the distance between the receiving plate and the spinning end is 10cm;
(3) Performing heat treatment on the PVDF/manganese acetate nano-fiber felt at 180 ℃ for 12 hours to obtain PVDF/manganese dioxide nano-powder;
(4) Dissolving lithium formate, nickel formate, cobalt formate, PVDF/manganese dioxide nano powder and 1 mL nitric acid in deionized water, wherein the molar weight ratio of the lithium formate to the nickel formate to the cobalt formate to the PVDF/manganese dioxide is 0.01mol:0.005mol: 0.002mol, stirring to obtain uniform and clear precursor solution; adding the precursor solution into 15 mL sodium hydroxide alkali solution, moving the solution to a hydrothermal kettle of 25 mL, and carrying out hydrothermal reaction in an oven at 200 ℃ for 2 hours; and centrifuging the product after reaction, washing the precipitate obtained after centrifugation for many times by using deionized water and absolute ethyl alcohol, then placing the precipitate in a muffle furnace to calcine 3h at 450 ℃, and grinding the precipitate by using an agate mortar to obtain the ternary nano material.
The specific surface area of the ternary nano material is 20.8 m 2 /g。
Example 3
A ternary nano material is prepared by inducing a nano fiber template, and the method comprises the following steps:
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 2:1; heating the solution to 50-55 ℃ until polyvinylidene fluoride is completely dissolved to obtain a PVDF solution;
(2) Adding soluble manganese formate into the solution obtained in the step (1), continuously stirring until a uniform solution is formed, and preparing the PVDF/manganese formate nano fibrofelt by adopting an electrostatic spinning method under the voltage of 10 KV; and the distance between the receiving plate and the spinning end is 10cm;
(3) Performing low-temperature treatment on the PVDF/manganese formate nano fiber felt at 160 ℃ for 18 hours to obtain PVDF/manganese dioxide nano powder;
(4) Dissolving lithium formate, nickel formate, cobalt formate, PVDF/manganese dioxide nanopowder and 1 mL nitric acid in deionized water, so that the molar weight ratio of the lithium formate, the nickel formate, the cobalt formate and the PVDF/manganese dioxide is 0.018 mol; adding the precursor solution into 15 mL sodium hydroxide alkali solution, moving the solution into a 25 mL hydrothermal kettle, and carrying out hydrothermal reaction in a 200 ℃ drying oven for 2 hours; and centrifuging the product after reaction, washing the precipitate obtained after centrifugation with deionized water and absolute ethyl alcohol for multiple times, calcining the precipitate in a muffle furnace at 500 ℃ for 2 hours, and grinding the calcined precipitate in an agate mortar to obtain the ternary nano material.
The specific surface area of the ternary nano material is 20.6 m 2 /g。

Claims (10)

1. A method for preparing ternary nano material by inducing a nano fiber template is characterized by comprising the following steps,
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 1~4:1; heating the solution to 50-55 ℃ until polyvinylidene fluoride is completely dissolved to obtain a PVDF solution;
(2) Adding soluble manganese salt into the solution obtained in the step (1), continuously stirring until a uniform solution is formed, and preparing the PVDF/manganese salt nano fiber felt by adopting an electrostatic spinning method under the voltage of 10-15 KV; and the distance between the receiving plate and the spinning end is 10 to 15 cm;
(3) Treating the PVDF/manganese salt nano fiber felt at low temperature, and carrying out heat treatment at 140 to 180 ℃ for 12 to 24h to obtain PVDF/manganese dioxide nano powder;
(4) Dissolving lithium salt, nickel salt, cobalt salt, PVDF/manganese dioxide nano powder and 1 mL nitric acid in deionized water to enable the molar weight ratio of the lithium salt, the nickel salt, the cobalt salt and the PVDF/manganese dioxide to be 1: 1-x-y: x: y, and stirring to obtain uniform and clear precursor liquid; adding the precursor solution into 15 mL sodium hydroxide alkali solution, moving the solution into a 25 mL hydrothermal kettle, and carrying out hydrothermal reaction in an oven at 180-200 ℃ for 1-3h; and centrifuging the product after reaction, washing the precipitate obtained after centrifugation by using deionized water and absolute ethyl alcohol, calcining the precipitate in a muffle furnace at 400-500 ℃ for 2-3 h, and grinding the calcined product by using an agate mortar to obtain the ternary nano material.
2. The method of claim 1, wherein the manganese salt is one of manganese acetate or manganese formate or a combination thereof.
3. The method for preparing ternary nanomaterial by inducing nanofiber template according to claim 1, wherein the lithium salt is one or a combination of lithium acetate and lithium formate.
4. The method for preparing ternary nano-material by inducing nanofiber templates as claimed in claim 1, wherein the nickel salt is one or a combination of nickel acetate and nickel formate.
5. The method for preparing ternary nano-material by inducing nanofiber templates as claimed in claim 1, wherein the cobalt salt is one or a combination of cobalt acetate and cobalt formate.
6. The method for preparing the ternary nano-material by inducing the nano-fiber template according to any one of claims 1 to 5, wherein the method comprises the following steps:
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 1:1; heating the solution to 50 ℃ until the polyvinylidene fluoride is completely dissolved to obtain a PVDF solution;
(2) Adding soluble manganese acetate into the solution obtained in the step (1), continuously stirring the solution until a uniform solution is formed, and preparing the PVDF/manganese acetate nano fiber felt by adopting an electrostatic spinning method under the voltage of 10 KV; and the distance between the receiving plate and the spinning end is 15 cm;
(3) Carrying out heat treatment on the PVDF/manganese acetate nano fiber felt at the temperature of 140-180 ℃ for 12-24h to obtain PVDF/manganese dioxide nano powder;
(4) Dissolving lithium acetate, nickel acetate, cobalt acetate, PVDF/manganese dioxide nano powder and 1 mL nitric acid in deionized water to ensure that the molar weight ratio of the lithium acetate, the nickel acetate, the cobalt acetate and the PVDF/manganese dioxide is 0.01mol to 0.0033mol to 0.0033mol, and stirring to obtain uniform and clear precursor solution; adding the precursor solution into 15 mL sodium hydroxide alkali solution, moving the solution to a 25 mL hydrothermal kettle, and carrying out hydrothermal reaction in an oven at 180 ℃ for 3 hours; centrifuging the reaction product, washing the precipitate obtained after centrifugation with deionized water and absolute ethyl alcohol for multiple times, calcining the precipitate in a muffle furnace at 400 ℃ for 3 hours, and grinding the calcined precipitate in an agate mortar to obtain the precipitate with the specific surface area of 21.2 m 2 A ternary nanomaterial of/g.
7. The method for preparing the ternary nano-material by inducing the nanofiber template as claimed in any one of claims 1 to 5, wherein the method comprises the following steps:
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 3:1; heating the solution to 55 ℃ until polyvinylidene fluoride is completely dissolved to obtain a PVDF solution;
(2) Adding soluble manganese formate into the solution obtained in the step (1), continuously stirring until a uniform solution is formed, and preparing the PVDF/manganese salt nano fiber felt by adopting an electrostatic spinning method under the voltage of 10 KV; and the distance between the receiving plate and the spinning end is 10cm;
(3) Performing heat treatment on the PVDF/manganese acetate nano-fiber felt at 180 ℃ for 12 hours to obtain PVDF/manganese dioxide nano-powder;
(4) Dissolving lithium formate, nickel formate, cobalt formate, PVDF/manganese dioxide nano powder and 1 mL nitric acid in deionized water, wherein the molar weight ratio of the lithium formate to the nickel formate to the cobalt formate to the PVDF/manganese dioxide is 0.01mol:0.005mol: 0.002mol, stirring to obtain uniform and clear precursor solution; adding the precursor solution into 15 mL sodium hydroxide alkali solution, moving the solution into a hydrothermal kettle of 25 mL, and carrying out hydrothermal reaction in an oven at 200 ℃ for 2 hours; centrifuging the product after reaction, washing the precipitate obtained after centrifugation for many times by using deionized water and absolute ethyl alcohol, then placing the precipitate in a muffle furnace to calcine 3h at 450 ℃, and grinding the precipitate by using an agate mortar to obtain the product with the specific surface area of 20.8 m 2 A ternary nanomaterial of/g.
8. The method for preparing the ternary nano-material by inducing the nanofiber template as claimed in any one of claims 1 to 5, wherein the method comprises the following steps:
(1) Dissolving polyvinylidene fluoride in a mixed solvent of N, N-dimethylformamide and acetone, wherein the volume ratio of the N, N-dimethylformamide to the acetone is 2:1; heating the solution to 50-55 ℃ until polyvinylidene fluoride is completely dissolved to obtain a PVDF solution;
(2) Adding soluble manganese formate into the solution obtained in the step (1), continuously stirring until a uniform solution is formed, and preparing the PVDF/manganese formate nano fibrofelt by adopting an electrostatic spinning method under the voltage of 10 KV; and the distance between the receiving plate and the spinning end is 10cm;
(3) Performing low-temperature treatment on the PVDF/manganese formate nano fiber felt at 160 ℃ for 18 hours to obtain PVDF/manganese dioxide nano powder;
(4) Dissolving lithium formate, nickel formate, cobalt formate, PVDF/manganese dioxide nanopowder and 1 mL nitric acid in deionized water, so that the molar ratio of the lithium formate, the nickel formate, the cobalt formate and the PVDF/manganese dioxide is 0.018 mol; adding the precursor solution into 15 mL sodium hydroxide alkali solution, moving the solution to a 25 mL hydrothermal kettle, and carrying out hydrothermal reaction in a 200 ℃ oven for 2 hours; centrifuging the product after reaction, washing the precipitate obtained after centrifugation for many times by deionized water and absolute ethyl alcohol, then calcining the precipitate in a muffle furnace at 500 ℃ for 2 hours, and grinding the calcined precipitate by an agate mortar to obtain the product with the specific surface area of 20.6 m 2 A ternary nanomaterial of/g.
9. A ternary nanomaterial prepared by induction of a nanofiber template, characterized by being prepared according to the method of any one of claims 1 to 8.
10. The application of the ternary nano material prepared by inducing the nanofiber template as claimed in claim 9 in a lithium ion battery cathode material.
CN202211401243.7A 2022-11-09 2022-11-09 Method for preparing ternary nano material by inducing nanofiber template, product and application Pending CN115504527A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009127170A2 (en) * 2008-04-15 2009-10-22 Elmarco S.R.O. Method for production of nanofibres from fluorated copolymers and terpolymers through electrostatic spinning, nanofibres and fabrics
CN108666553A (en) * 2018-05-11 2018-10-16 深圳大学 A kind of cobalt sulfide/carbon fiber composite and the preparation method and application thereof
JP6572416B1 (en) * 2018-03-26 2019-09-11 大豊精機株式会社 Conductive nanofiber member, fuel cell member, fuel cell, and method of manufacturing conductive nanofiber member
WO2022016554A1 (en) * 2020-07-24 2022-01-27 苏州大学 Metal carbide catalyst, preparation method therefor, and use thereof in lithium oxygen battery
CN114551907A (en) * 2022-01-13 2022-05-27 河北大学 Carbon fiber loaded nickel-manganese oxide composite material and preparation method and application thereof
CN114883567A (en) * 2022-06-30 2022-08-09 河南科隆新能源股份有限公司 Lithium ion battery cathode material with hollow tubular structure and preparation method and application thereof
CN115231622A (en) * 2022-07-06 2022-10-25 上海纳米技术及应用国家工程研究中心有限公司 Method for preparing manganese cobalt oxygen by inducing low-temperature heat treatment of nanofiber template

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009127170A2 (en) * 2008-04-15 2009-10-22 Elmarco S.R.O. Method for production of nanofibres from fluorated copolymers and terpolymers through electrostatic spinning, nanofibres and fabrics
JP6572416B1 (en) * 2018-03-26 2019-09-11 大豊精機株式会社 Conductive nanofiber member, fuel cell member, fuel cell, and method of manufacturing conductive nanofiber member
CN108666553A (en) * 2018-05-11 2018-10-16 深圳大学 A kind of cobalt sulfide/carbon fiber composite and the preparation method and application thereof
WO2022016554A1 (en) * 2020-07-24 2022-01-27 苏州大学 Metal carbide catalyst, preparation method therefor, and use thereof in lithium oxygen battery
CN114551907A (en) * 2022-01-13 2022-05-27 河北大学 Carbon fiber loaded nickel-manganese oxide composite material and preparation method and application thereof
CN114883567A (en) * 2022-06-30 2022-08-09 河南科隆新能源股份有限公司 Lithium ion battery cathode material with hollow tubular structure and preparation method and application thereof
CN115231622A (en) * 2022-07-06 2022-10-25 上海纳米技术及应用国家工程研究中心有限公司 Method for preparing manganese cobalt oxygen by inducing low-temperature heat treatment of nanofiber template

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
欧繁爱;钟洪彬;曾媚媚;赖玲;余文亚;张平;: "碳纳米管包覆LiNi_(0.8)Co_(0.1)Mn_(0.1)O_2纳米纤维制备及其电化学性能研究", 广东化工, no. 15 *

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