CN108777294B - Carbon-supported porous spherical MoN composed of nanosheets and application of carbon-supported porous spherical MoN as negative electrode material in lithium battery - Google Patents

Carbon-supported porous spherical MoN composed of nanosheets and application of carbon-supported porous spherical MoN as negative electrode material in lithium battery Download PDF

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CN108777294B
CN108777294B CN201810519497.6A CN201810519497A CN108777294B CN 108777294 B CN108777294 B CN 108777294B CN 201810519497 A CN201810519497 A CN 201810519497A CN 108777294 B CN108777294 B CN 108777294B
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mon
carbon
porous spherical
supported porous
mixture
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CN108777294A (en
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魏明灯
王建标
沈德立
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Fuzhou University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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 relates to a carbon-supported porous spherical MoN lithium battery negative electrode material composed of nanosheets. 0.1g of MoO2(acac)2，0.2g CH4N2S and 0.1g glucose in 20ml H2And O, stirring for 1 hour, then placing the mixture into a 200 ℃ oven for 12 hours, taking out the mixture, cooling the mixture to room temperature, centrifuging the product, washing the product for several times by using ethanol and deionized water, placing the product into a 70 ℃ oven for drying to obtain a precursor of the MoN, then placing the precursor of the MoN into a tubular furnace, and calcining the precursor for 4 hours at 800 ℃ in an ammonia atmosphere to obtain the carbon-supported porous spherical MoN material consisting of the nano sheets. The prepared spherical MoN nanosheet with the size of 500nm has good cycling stability and high rate capability when used as a lithium ion battery cathode, and has specific capacity of 600 mAh/g after being subjected to charge-discharge cycling for 400 times when the current density is 1A.

Description

Carbon-supported porous spherical MoN composed of nanosheets and application of carbon-supported porous spherical MoN as negative electrode material in lithium battery
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a carbon-supported porous spherical MoN composed of nanosheets and application thereof as a negative electrode material in a lithium battery.
Background
So far, lithium ion batteries have been widely used, however, the conventional commercialized negative electrode material graphite can not meet the requirements of modern electronic equipment because the theoretical capacity is only 372 mAh/g, so that the invention of the alternative high-capacity negative electrode material is called as the first task of researchers and the urgent needs of modern society.
At present, no patent report related to carbon-supported porous spherical MoN consisting of nanosheets exists.
Disclosure of Invention
The invention aims to provide carbon-supported porous spherical MoN consisting of nanosheets and application of the carbon-supported porous spherical MoN as a negative electrode material in a lithium battery. Since the MoN material has metal characteristics in both bulk and nanosheet, nano-flake MoN has higher conductivity and is more favorable for electron transport than its bulk. Under the condition of the current density of 1A/g, after the circulation of 400 circles, the specific capacity of the lithium ion battery is maintained at 600 mA h/g. Meanwhile, the CV graph shows that after the first turn, the images are basically overlapped, indicating that the electrochemical performance of the MoN nanosheet is stable.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the compound comprises the following steps: 0.1g MoO2(acac)2, 0.2g CH4N2S and 0.1g glucose in 20ml H2And stirring for 1 hour, then putting the mixture into an oven at 200 ℃ for 12 hours, taking the mixture out, and cooling the mixture to room temperature. And centrifuging the product, washing the product for several times by using ethanol and deionized water, putting the product into a 70 ℃ oven for drying to obtain a precursor of the MoN, putting the precursor into a tubular furnace, and calcining the precursor for 4 hours at 800 ℃ in an ammonia atmosphere to obtain the carbon-supported porous spherical MoN material consisting of the nano sheets.
Assembling the lithium battery: according to the mass ratio: MoN nanosheet: acetylene black: uniformly mixing polyvinylidene fluoride = 8:1:1, coating the mixture on a copper foil to form a negative electrode, wherein the reference electrode and the counter electrode are both lithium sheets, and the electrolyte is 1M LiClO4EC + DMC (EC/DMC =1/1 v/v) solution, lithium battery assembly all operations were performed in a glove box.
The invention provides a carbon-supported porous spherical MoN composed of nanosheets and application of the carbon-supported porous spherical MoN as a negative electrode material in the aspect of energy storage materials.
The invention has the following remarkable advantages: the prepared spherical MoN nanosheet with the size of 500nm has good cycling stability and high rate capability when used as a lithium ion battery cathode, and has specific capacity of 600 mAh/g after being subjected to charge-discharge cycling for 400 times when the current density is 1A. The nano material has the advantages of simple synthesis method, good reproducibility and excellent lithium storage performance.
Drawings
FIG. 1 is an XRD pattern of MoN;
FIG. 2 is a CV diagram;
FIG. 3 is a graph of the cycle performance of MoN;
FIG. 4 is a scanning electron micrograph of MoN.
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
A carbon-supported porous spherical MoN composed of nanosheets, the preparation method of which comprises the following steps: 0.1g of MoO2(acac)2，0.2g CH4N2S and 0.1g glucose in 20ml H2And O, stirring for 1 hour, then placing the mixture into a 200 ℃ oven for 12 hours, taking out the mixture, cooling the mixture to room temperature, centrifuging the product, washing the product for several times by using ethanol and deionized water, placing the product into a 70 ℃ oven for drying to obtain a precursor of the MoN, then placing the precursor of the MoN into a tubular furnace, and calcining the precursor for 4 hours at 800 ℃ in an ammonia atmosphere to obtain the carbon-supported porous spherical MoN material consisting of the nano sheets.
The application of the MoN as a negative electrode material in a lithium ion battery comprises the following steps: MoN nanosheets in mass ratio: acetylene black: uniformly mixing polyvinylidene fluoride = 8:1:1, coating the mixture on a copper foil to form a negative electrode, wherein the reference electrode and the counter electrode are both lithium sheets, and the electrolyte is 1M LiClO4The EC + DMC solution of (1), wherein the volume ratio EC/DMC =1/1, all operations of lithium battery assembly were performed in a glove box.
And simultaneously carrying out electrical property test: the prepared spherical MoN nanosheet with the size of 500nm has good cycling stability and high rate capability when used as a lithium ion battery cathode, and has specific capacity of 600 mAh/g after being subjected to charge-discharge cycling for 400 times when the current density is 1A. Fig. 1 is an XRD pattern of MoN, indicating that the synthesized MoN is a pure phase. Fig. 2 is a CV graph, starting from the second circle, with nearly overlapping graphs indicating the stability of the electrochemical performance of MoN. FIG. 3 is a graph of the cycle performance of MoN, and it can be seen that the electrode material can still maintain a capacity of 600 mAh/g after 400 cycles at a current density of 1A/g. Fig. 4 is a scanning electron micrograph of MoN, from which it can be seen that the morphology of MoN is spherical composed of nanosheets, and from the broken spheres it can be seen that the spheres are hollow.
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. A carbon-supported porous spherical MoN composed of nanosheets is characterized in that the preparation method comprises the following steps: 0.1g of MoO2(acac)2，0.2g CH4N2S and 0.1g glucose in 20ml H2And O, stirring for 1 hour, then placing the mixture into a 200 ℃ oven for 12 hours, taking out the mixture, cooling the mixture to room temperature, centrifuging the product, washing the product for several times by using ethanol and deionized water, placing the product into a 70 ℃ oven for drying to obtain a precursor of the MoN, then placing the precursor of the MoN into a tubular furnace, and calcining the precursor for 4 hours at 800 ℃ in an ammonia atmosphere to obtain the carbon-supported porous spherical MoN material consisting of the nano sheets.
2. The application of the carbon-supported porous spherical MoN composed of nanosheets according to claim 1, wherein the MoN is applied as a negative electrode material in a lithium ion battery, and the preparation method of the lithium ion battery comprises the following steps: MoN nanosheets in mass ratio: acetylene black: uniformly mixing polyvinylidene fluoride = 8:1:1, coating the mixture on a copper foil to form a negative electrode, wherein the reference electrode and the counter electrode are both lithium sheets, and the electrolyte is 1M LiClO4The EC + DMC solution of (1), wherein the volume ratio EC/DMC =1/1, all operations of lithium battery assembly were performed in a glove box.
CN201810519497.6A 2018-05-28 2018-05-28 Carbon-supported porous spherical MoN composed of nanosheets and application of carbon-supported porous spherical MoN as negative electrode material in lithium battery Expired - Fee Related CN108777294B (en)

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CN109860535A (en) * 2018-12-18 2019-06-07 福州大学 Fabricated in situ MoS2The method and its application of@MoN hollow sphere
CN109841815B (en) * 2019-02-20 2021-06-22 福州大学 Mo2N/MoO3/C composite lithium ion battery cathode material and preparation method thereof
CN110265225B (en) * 2019-05-23 2021-03-16 天津大学 Method for preparing nitrogen-doped three-dimensional porous carbon microsphere loaded molybdenum carbide/molybdenum nitride and iron nanoparticle composite material
CN112599753B (en) * 2021-01-07 2021-11-02 福州大学 Preparation and application of SnS @ C graded ball with S defects
CN114156455B (en) * 2021-11-30 2023-04-07 电子科技大学 Heterostructure material for lithium metal battery lithium negative electrode protection, preparation and application
CN114551813B (en) * 2022-02-28 2024-02-02 华中科技大学 Metal lithium composite electrode, preparation method, application and battery

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