CN112047380A - Hierarchical nanowire structure V2O5Preparation method and application of electrode material - Google Patents

Hierarchical nanowire structure V2O5Preparation method and application of electrode material Download PDF

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CN112047380A
CN112047380A CN202010509306.5A CN202010509306A CN112047380A CN 112047380 A CN112047380 A CN 112047380A CN 202010509306 A CN202010509306 A CN 202010509306A CN 112047380 A CN112047380 A CN 112047380A
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electrode material
nanowire structure
preparation
hierarchical
sol
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李延伟
季靖程
姚金环
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Guilin University of Technology
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Guilin University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • 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
    • 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
    • H01M4/36—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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • 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
    • 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 hierarchical nanowire structure V2O5A preparation method and application of the electrode material. Will V2O5Powder and H2O2Sequentially added into deionized water to prepare V2O5A solution; v to be sealed2O5Standing the solution at low temperature to prepare V2O5Gelling; to V2O5Adding a small amount of P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer) into the gel, diluting with deionized water, and dispersing to obtain V2O5Sol; will V2O5After freeze drying the sol, the sol is put in an air atmosphereIntermediate sintering to obtain the hierarchical nanowire structure V2O5An electrode material. The electrode material is applied to the preparation of lithium ion batteries, and shows excellent cycle performance and rate capability. The preparation method of the invention has the advantages of simplicity, low cost, high yield, easy control of preparation conditions and suitability for large-scale production.

Description

Hierarchical nanowire structure V2O5Preparation method and application of electrode material
Technical Field
The invention belongs to the technical field of lithium ion battery anode materials, and particularly relates to a hierarchical nanowire structure V2O5A preparation method and application of the electrode material.
Background
V2O5Has rich oxidation state (from V)2+To V5+) The lithium ion battery anode material has the advantages of high theoretical specific capacity (300 mAh/g, corresponding to two lithium ion intercalation/deintercalation reactions), rich reserve, relatively low price and the like, and is considered to be a very competitive lithium ion battery anode material. However, as a positive electrode material for lithium ion batteries, V2O5Poor cycle performance and poor rate performance in the process of repeatedly inserting/extracting lithium. The nano-crystallization can effectively improve the specific surface of the material and greatly shorten the diffusion path of lithium ions, thereby improving V2O5An efficient method for electrochemical performance of lithium storage materials. Among a plurality of nano structures, the one-dimensional nano wire can provide a continuous path for the rapid charge transfer in the axial direction, is very favorable for the rapid insertion and extraction of lithium ions in the radial direction, and is very favorable for improving the cycle performance and the rate capability of the material, so the one-dimensional nano wire is widely concerned by domestic and foreign researchers. Preparation of V at present2O5The methods of the nanowire mainly include a template method, a hydrothermal method, an electrospinning method, a vapor deposition method and the like, but the methods have the problems of high cost, harsh synthesis conditions, complex process steps and the like, and are not beneficial to industrial production. Thus, the development of V is simple, convenient, easy, efficient and low-cost2O5A method of nanowires is very necessary. Therefore, the invention provides a preparation method of the hierarchical nanowire structure V, which is simple in process and low in cost2O5A novel method for preparing electrode material.
Disclosure of Invention
The invention aims to provide a hierarchical nanowire structure V2O5A preparation method and application of the electrode material.
Preparation of hierarchical nanowire structures V2O5The electrode material comprises the following specific steps:
(1) will V2O5Powder and 30% H2O2Sequentially adding the materials into deionized water according to the mol ratio of 1:8, stirring and reacting for 15 minutes to obtain an aqueous solution V2O5The concentration is 0.056 mol/L.
(2) Sealing the aqueous solution obtained in the step (1), and placing the sealed aqueous solution in an oven at 70 ℃ for 12 hours to form V2O5And (4) gelling.
(3) To V obtained in step (2)2O5Adding P123 into the gel, wherein the P123 and V in the gel2O5Is 2 percent, then deionized water is added, stirred, dispersed and diluted to form V2O5Sol with the concentration of 0.02 mol/L.
(4) V obtained in the step (3)2O5Freezing the sol in liquid nitrogen, freeze drying in a freeze drier to constant weight to obtain V2O5And (3) precursor.
(5) V obtained in the step (4)2O5The precursor is put in a muffle furnace and heated from room temperature to 450 ℃ under the air atmosphere, the heating speed is 10 ℃/min, the temperature is kept for 1 hour, and then the precursor is cooled along with the furnace and taken out, thus obtaining the hierarchical nanowire structure V2O5An electrode material.
And the P123 is a triblock copolymer surfactant of polyethylene oxide-polypropylene oxide-polyethylene oxide.
Hierarchical nanowire Structure V of the invention2O5The electrode material is applied to the preparation of lithium ion batteries.
The invention is realized by the reaction at V2O5A small amount of P123 is added into the gel to assist in simply and conveniently preparing the hierarchical nanowire structure V2O5The electrode material is applied to the anode material of the lithium ion battery, shows excellent electrochemical performance, has simple method, low cost, high yield and easily controlled preparation conditions, and is suitable for large-scale production.
Drawings
FIG. 1 is a hierarchical nanowire structure V prepared in accordance with an embodiment of the present invention2O5XRD pattern of electrode material.
FIG. 2 shows a hierarchical nanowire structure V prepared according to an embodiment of the present invention2O5SEM image of electrode material.
FIG. 3 shows a hierarchical nanowire structure V prepared according to an embodiment of the present invention2O5Electrode material inCycling performance curve at 4C (1C =150 mA/g) current density.
FIG. 4 shows a hierarchical nanowire structure V prepared according to an embodiment of the present invention2O5Rate performance curves of the electrode materials at different current densities 0.5C, 2C, 4C, 10C, 16C, 25C, 40C and 60C (1C =150 mA/g).
Detailed Description
The present invention is further described with reference to the following specific examples, which are intended to provide those skilled in the art with a better understanding of the present invention, and are not intended to limit the scope of the present invention, which is to be construed as limited thereby.
Example (b):
(1) 0.2547 g V will be mixed2O5Powder and 1.15 mL of H with the mass percentage concentration of 30%2O2Sequentially adding the mixture into 23.85 mL of deionized water, stirring and reacting for 15 minutes, wherein the V in the aqueous solution2O5The concentration is 0.056 mol/L.
(2) Sealing the aqueous solution obtained in the step (1), and placing the sealed aqueous solution in an oven at 70 ℃ for 12 hours to form V2O5And (4) gelling.
(3) To V obtained in step (2)2O50.0051 g P123 is added into the gel, and then 45 mL deionized water is added to stir, disperse and dilute to form V2O5Sol with the concentration of 0.02 mol/L.
(4) V obtained in the step (3)2O5Freezing the sol in liquid nitrogen, freeze drying in a freeze drier to constant weight to obtain V2O5And (3) precursor.
(5) V obtained in the step (4)2O5The precursor is put in a muffle furnace and heated from room temperature to 450 ℃ under the air atmosphere, the heating speed is 10 ℃/min, the temperature is kept for 1 hour, and then the precursor is cooled along with the furnace and taken out, thus obtaining the hierarchical nanowire structure V2O5An electrode material.
And the P123 is a triblock copolymer surfactant of polyethylene oxide-polypropylene oxide-polyethylene oxide.
Application example: hierarchical nanowire Structure V prepared in the examples2O5Mixing and dispersing an electrode material (active substance), Super P carbon black (conductive agent) and polyvinylidene fluoride (PVDF, binder) into a proper amount of N-methyl-2-pyrrolidone (NMP, solvent) according to a mass ratio of 7:2:1, uniformly mixing to form slurry, uniformly coating the slurry on an aluminum foil, drying the coated aluminum foil at 80 ℃ in vacuum for 12 hours, and blanking to obtain the electrode plate. Taking the electrode slice obtained after blanking as a working electrode, a metal lithium slice as a counter electrode, a polyolefin microporous membrane (Celgard 2400) as a diaphragm and 1.0 mol/L LiPF6The mixed solution of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) (V (EC): V (DMC) =1: 1) is used as electrolyte, and assembled into CR2016 type button lithium ion battery in a glove box filled with argon. The constant-current charging and discharging and multiplying power performance of the battery is tested by adopting an LAND battery testing system, and the charging and discharging voltage range is 2.0-4.0V (vs. Li)+/Li) where the current density for the cycling performance test was 4C (1C =150 mA/g) and the current density for the rate performance test was 0.5C, 2C, 4C, 10C, 16C, 25C, 40C and 60C (1C =150 mA/g), respectively. The V's obtained in the examples are shown in Table 12O5And testing the lithium storage performance of the electrode material.
Table 1 hierarchical nanowire structure V made in the example2O5Test result of lithium storage performance of electrode material
Figure DEST_PATH_IMAGE002
As can be seen from FIG. 1, the example prepared hierarchical nanowire structure V2O5The electrode material being in quadrature-phase V2O5。
As can be seen from FIG. 2, the example prepared hierarchical nanowire structure V2O5The electrode material is of a hierarchical nanowire structure, the nanowire is formed by connecting secondary single crystal nanoparticles, and the structure is very beneficial to the rapid insertion and extraction of lithium ions in the electrode material.
It can be seen from fig. 3 and 4Example prepared hierarchical nanowire Structure V2O5The electrode material has excellent cycle performance and rate capability.

Claims (2)

1. Hierarchical nanowire structure V2O5The preparation method of the electrode material is characterized by comprising the following specific steps:
(1) will V2O5Powder and 30% H2O2Sequentially adding the materials into deionized water according to the mol ratio of 1:8, stirring and reacting for 15 minutes to obtain an aqueous solution V2O5The concentration is 0.056 mol/L;
(2) sealing the aqueous solution obtained in the step (1), and placing the sealed aqueous solution in an oven at 70 ℃ for 12 hours to form V2O5Gelling;
(3) to V obtained in step (2)2O5Adding P123 into the gel, wherein the P123 and V in the gel2O5Is 2 percent, then deionized water is added, stirred, dispersed and diluted to form V2O5Sol with the concentration of 0.02 mol/L;
(4) v obtained in the step (3)2O5Freezing the sol in liquid nitrogen, freeze drying in a freeze drier to constant weight to obtain V2O5A precursor;
(5) v obtained in the step (4)2O5The precursor is put in a muffle furnace and heated from room temperature to 450 ℃ under the air atmosphere, the heating speed is 10 ℃/min, the temperature is kept for 1 hour, and then the precursor is cooled along with the furnace and taken out, thus obtaining the hierarchical nanowire structure V2O5An electrode material;
and the P123 is a triblock copolymer surfactant of polyethylene oxide-polypropylene oxide-polyethylene oxide.
2. A hierarchical nanowire structure V prepared by the preparation method of claim 12O5Use of an electrode material, characterized in that the hierarchical nanowire structure V2O5The electrode material is applied to the preparation of lithium ion batteries.
CN202010509306.5A 2020-06-07 2020-06-07 Hierarchical nanowire structure V2O5Preparation method and application of electrode material Pending CN112047380A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102795666A (en) * 2012-07-27 2012-11-28 中南大学 Method for preparing vanadium pentoxide cathode nano-material of lithium-ion battery
CN107611410A (en) * 2017-09-30 2018-01-19 湖南国盛石墨科技有限公司 V2o5/ graphene composite materials preparation method and anode
CN109638245A (en) * 2018-12-07 2019-04-16 桂林理工大学 A method of sodium performance is stored up by the pre- embedding raising vanadic anhydride electrode material of copper ion
CN109659521A (en) * 2018-12-07 2019-04-19 桂林理工大学 A kind of preparation method of high-performance sodium-ion battery vanadic anhydride/grapheme composite positive electrode material
CN111244435A (en) * 2020-02-11 2020-06-05 桂林理工大学 Preparation method and application of nano linear vanadium pentoxide electrode material
CN111244462A (en) * 2020-02-11 2020-06-05 桂林理工大学 Preparation method and application of polypyrrole composite vanadium pentoxide electrode material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102795666A (en) * 2012-07-27 2012-11-28 中南大学 Method for preparing vanadium pentoxide cathode nano-material of lithium-ion battery
CN107611410A (en) * 2017-09-30 2018-01-19 湖南国盛石墨科技有限公司 V2o5/ graphene composite materials preparation method and anode
CN109638245A (en) * 2018-12-07 2019-04-16 桂林理工大学 A method of sodium performance is stored up by the pre- embedding raising vanadic anhydride electrode material of copper ion
CN109659521A (en) * 2018-12-07 2019-04-19 桂林理工大学 A kind of preparation method of high-performance sodium-ion battery vanadic anhydride/grapheme composite positive electrode material
CN111244435A (en) * 2020-02-11 2020-06-05 桂林理工大学 Preparation method and application of nano linear vanadium pentoxide electrode material
CN111244462A (en) * 2020-02-11 2020-06-05 桂林理工大学 Preparation method and application of polypyrrole composite vanadium pentoxide electrode material

Non-Patent Citations (1)

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Title
谢志平等: "0/1/2维混合纳米形貌V2O5的制备与储锂性能", 《高等学校化学学报》 *

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Application publication date: 20201208