CN109205671B - From VS2Preparation method and application of graded-structure ball composed of nanosheets - Google Patents

From VS2Preparation method and application of graded-structure ball composed of nanosheets Download PDF

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CN109205671B
CN109205671B CN201811264825.9A CN201811264825A CN109205671B CN 109205671 B CN109205671 B CN 109205671B CN 201811264825 A CN201811264825 A CN 201811264825A CN 109205671 B CN109205671 B CN 109205671B
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structure ball
ball
graded
nanosheets
sodium
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CN109205671A (en
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魏明灯
王建标
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Fuzhou University
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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 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

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Abstract

The invention provides a Virtual Switch (VS)2Preparation of hierarchical structure ball composed of nanosheets and application of hierarchical structure ball as negative electrode material of sodium-ion battery, and VS is prepared by adopting simple one-step hydrothermal method2The nano-sheets form a grading sphere. Due to VS2The nano sheet has metal characteristics, and the ultra-thin nano sheet can effectively shorten the transmission path of ions. The electrochemical research result shows that the specific capacity of the material is maintained at 560 mAh/g after the material is cycled for 1000 circles under the current density of 2A/g, and the material has good cycling stability and rate capability.

Description

From VS2Preparation method and application of graded-structure ball composed of nanosheets
Technical Field
The invention belongs to the field of sodium ion batteries, and particularly relates to a composite negative voltage VS2Preparation of a hierarchical structure ball composed of nano sheets and application of the hierarchical structure ball as a negative electrode material of a sodium ion battery.
Background
So far, lithium ion batteries have been widely used, however, lithium resources are scarce, and in contrast, metallic sodium reserves are abundant and cheap. Therefore, the sodium ion battery becomes a potential novel battery for replacing a lithium battery. However, the radius of the sodium ions in the sodium ion battery is large, which causes problems of large volume expansion and low energy density. Therefore, the development of a suitable sodium ion negative electrode material has become a first task of researchers and an urgent need of modern society.
Currently unavailable VS2And (3) relevant patent reports of preparation of the hierarchical structure sphere composed of the nanosheets.
Disclosure of Invention
The invention aims to provide a method for switching between a Virtual Switch (VS)2Preparation of hierarchical structure ball composed of nanosheets and application of hierarchical structure ball as negative electrode material of sodium-ion battery, and VS is prepared by adopting simple one-step hydrothermal method2The nano-sheets form a grading sphere. Due to VS2The nano sheet has metal characteristics, and the ultra-thin nano sheet can effectively shorten the transmission path of ions. The electrochemical research result shows that the specific capacity is maintained at 560 mAh/g after 1000 cycles of circulation under the current density of 2A/g. Meanwhile, in the rate capability of FIG. 3, when the current returns to 0.2A/g, the capacity returns toThe previous capacity indicates that the electrochemical performance is stable.
In order to achieve the purpose, the invention adopts the following technical scheme:
from VS2VS composed of nanosheets2The preparation method of the graded structure ball comprises the following steps: 0.35g of VO (acac)2, 0.2gCH3CSNH2And 0.1g glucose was put into 35ml (CH)2OH)2Neutralized and stirred for 1 hour. Then the mixture is put into an oven with the temperature of 200 ℃ for reaction for 24 hours and then taken out, and the mixture is cooled to the room temperature. Centrifuging, washing with ethanol and deionized water for several times, and drying in a vacuum oven at 70 deg.C to obtain the final product. Thus obtaining the result of VS2VS composed of nanosheets2A hierarchically structured ball.
Assembling the sodium battery: according to the mass ratio: VS2Grading structure ball: acetylene black: uniformly mixing hydroxymethyl cellulose = 7:2:1, coating the mixture on a copper foil to form a negative electrode, wherein the reference electrode and the counter electrode are both sodium, and the electrolyte is 1M NaSO3CF3The diglyme solution, sodium battery assembly all operations were performed in a glove box.
The invention has the following remarkable advantages: due to VS2The nano sheet has metal characteristics, and the ultra-thin nano sheet can effectively shorten the transmission path of ions. The electrochemical research result shows that the specific capacity is maintained at 560 mA h/g after 1000 cycles of circulation under the current density of 2A/g. Meanwhile, in the rate performance of fig. 3, when the current returns to 0.2A/g again, the capacity returns to the previous capacity again, indicating that the electrochemical performance is stable. Due to VS2The graded structure ball is made of ultrathin nanometer sheet(s) ((<5 nm), the three-dimensional porous structure characteristic of the nano-sheet is beneficial to the diffusion of electrolyte and the inhibition of the agglomeration of the nano-sheet in the charge-discharge process, the stability of electrochemical performance is maintained, and the ultra-thin nano-sheet is also beneficial to the shortening of the transmission path of sodium ions.
Drawings
FIG. 1 is VS2Scanning electron micrographs of hierarchically structured spheres; as can be seen from FIG. 1, VS2Has a spherical morphology with a hierarchical structure.
FIG. 2 is VS2A long cycle performance diagram of the graded structure ball under the current density of 2A/g; as can be seen from FIG. 2, the specific capacity was maintained at 560 mA h/g after 1000 cycles at a current density of 2A/g.
FIG. 3 is VS2A magnification performance diagram of a graded structure ball; as can be seen from FIG. 3, when the current returns to 0.2A/g, the capacity returns to the previous capacity, indicating VS2The electrochemical performance of the graded structure ball is stable.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the present invention is not limited to the following examples.
Example 1
From VS2The preparation method of the graded-structure ball composed of the nano-sheets comprises the following steps:
0.35g of VO (acac)2, 0.2g CH3CSNH2And 0.1g glucose was put into 35ml (CH)2OH)2Neutralizing and stirring for 1 hour, then putting into a 200 ℃ oven for reaction for 24 hours, taking out, cooling to room temperature, centrifuging, washing with ethanol and deionized water for several times, putting into a 70 ℃ vacuum oven for drying to obtain the final product VS2VS composed of nanosheets2A hierarchically structured ball.
The VS2The application of the graded structure ball as a negative electrode material in a sodium ion battery is as follows: according to the mass ratio: VS2Grading structure ball: acetylene black: uniformly mixing hydroxymethyl cellulose = 7:2:1, coating the mixture on a copper foil to form a negative electrode, wherein the reference electrode and the counter electrode are both sodium, and the electrolyte is 1M NaSO3CF3The diglyme solution, sodium ion battery assembly all operations were performed in a glove box.
FIG. 1 is VS2Scanning electron micrographs of hierarchically structured spheres; as can be seen from FIG. 1, VS2Has a spherical morphology with a hierarchical structure. FIG. 2 is VS2A long cycle performance diagram of the graded structure ball under the current density of 2A/g; as can be seen from FIG. 2, the specific capacity was maintained at 560 mA h/g after 1000 cycles at a current density of 2A/g. FIG. 3Is VS2A magnification performance diagram of a graded structure ball; as can be seen from FIG. 3, when the current returns to 0.2A/g, the capacity returns to the previous capacity, indicating VS2The electrochemical performance of the graded structure ball is stable. FIGS. 2 and 3 exhibit VS2The graded structure ball has good circulation stability and rate capability.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (2)

1. From VS2The preparation method of the graded-structure ball composed of the nano-sheets is characterized by comprising the following steps:
0.35g of VO (acac)2, 0.2gCH3CSNH2And 0.1g glucose was put into 35ml (CH)2OH)2Neutralizing and stirring for 1 hour, then putting into a 200 ℃ oven for reaction for 24 hours, taking out, cooling to room temperature, centrifuging, washing with ethanol and deionized water for several times, putting into a 70 ℃ vacuum oven for drying to obtain the final product VS2VS composed of nanosheets2A hierarchically structured ball.
2. VS prepared by the process according to claim 12Use of a hierarchically structured ball, wherein said VS is2The application of the graded structure ball as a negative electrode material in a sodium ion battery is as follows: according to the mass ratio: VS2Grading structure ball: acetylene black: uniformly mixing hydroxymethyl cellulose = 7:2:1, coating the mixture on a copper foil to form a negative electrode, wherein the reference electrode and the counter electrode are both sodium, and the electrolyte is 1M NaSO3CF3The diglyme solution, sodium ion battery assembly all operations were performed in a glove box.
CN201811264825.9A 2018-10-29 2018-10-29 From VS2Preparation method and application of graded-structure ball composed of nanosheets Active CN109205671B (en)

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