CN108777294A - A kind of porous spherical MoN that the carbon being made of nanometer sheet is supported and its application as negative material in lithium battery - Google Patents

A kind of porous spherical MoN that the carbon being made of nanometer sheet is supported and its application as negative material in lithium battery Download PDF

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Publication number
CN108777294A
CN108777294A CN201810519497.6A CN201810519497A CN108777294A CN 108777294 A CN108777294 A CN 108777294A CN 201810519497 A CN201810519497 A CN 201810519497A CN 108777294 A CN108777294 A CN 108777294A
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mon
carbon
supported
nanometer sheet
porous spherical
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CN201810519497.6A
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CN108777294B (en
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魏明灯
王建标
沈德立
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Fuzhou University
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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 present invention relates to a kind of porous spherical MoN lithium cell cathode materials that the carbon being made of nanometer sheet is supported.By 0.1g MoO2(acac)2, 0.2g CH4N2S and 0.1g glucose puts 20ml H into2In O and stir 1 hour, then it puts into 200 DEG C of baking ovens and is taken out after 12 hours, wait for that it is cooled to room temperature, product is centrifuged, ethyl alcohol and deionized water is used in combination to wash several times, puts 70 DEG C of baking oven drying into, obtain the presoma of MoN, then it is placed into tube furnace, is calcined 4 hours at 800 DEG C under ammonia atmosphere, obtain the porous spherical MoN materials that the carbon of nanometer sheet composition is supported.Prepared size has good cyclical stability and big high rate performance in the ball-type MoN nanometer sheets of 500nm as negative electrode of lithium ion battery, the specific capacity with 600 mAh/g after charge and discharge cycles 400 times when current density is 1A.

Description

A kind of porous spherical MoN that the carbon that is made of nanometer sheet is supported and its as cathode material Expect the application in lithium battery
Technical field
The invention belongs to field of lithium ion battery, and in particular to a kind of porous spherical that the carbon being made of nanometer sheet is supported MoN and its application as negative material in lithium battery.
Background technology
So far, lithium ion battery has been obtained for being widely applied, however traditional commercialized negative material stone Ink cannot already meet the needs of modern electronic equipment since theoretical capacity only has 372 mAh/g, because the invention is alternatively held Measure high negative material be known as researcher top priority and modern society there is an urgent need to.
At present also not by the porous spherical MoN related patents report supported of the carbon that form of nanometer sheet.
Invention content
The purpose of the present invention is to provide a kind of porous spherical MoN that the carbon being made of nanometer sheet is supported and its as cathode Application of the material in lithium battery prepares what the carbon being made of nanometer sheet with large specific surface area was supported using two-step method Porous spherical MoN, the first step are prepared the precursor material of MoN using hydro-thermal reaction, are then forged at 800 DEG C under ammonia atmosphere Target product can be obtained by burning 4 hours.Since MoN materials either block or nanometer sheet all have metallic character, but receive The MoN of rice sheet is compared with its block with higher electric conductivity and the transmission for being more advantageous to electronics.It is 1 A/ in current density Under g, after 400 circle of cycle, specific capacity maintains 600 mA h/g.Meanwhile CV figures show that after first lap, image is basic It overlaps, shows the stable electrochemical property of MoN nanometer sheets.
To achieve the above object, the present invention adopts the following technical scheme that：
Compound preparation method：0.1g MoO2(acac)2, 0.2g CH4N2S and 0.1g glucose puts 20ml H into2In O And stir 1 hour, it then puts into 200 DEG C of baking ovens and is taken out after 12 hours, wait for that it is cooled to room temperature.Product is centrifuged, second is used in combination Alcohol and deionized water washing several times, put 70 DEG C of baking oven drying into, obtain the presoma of MoN, be then placed into tube furnace, It is calcined 4 hours at lower 800 DEG C of ammonia atmosphere, the porous spherical MoN materials that the carbon of nanometer sheet composition is supported can be obtained.
The assembling of lithium battery：In mass ratio：MoN nanometer sheets：Acetylene black：Kynoar=8:1:1 applies after mixing Cloth does cathode on copper foil, reference electrode and be lithium piece to electrode, and electrolyte is 1M LiClO4EC+DMC (EC/DMC= 1/1 v/v) solution, lithium battery assembling it is all operation carried out in glove box.
The present invention provides a kind of porous spherical MoN of the carbon support of nanometer sheet composition and its as negative material in energy storage Application in terms of material.
The remarkable advantage of the present invention is：Prepared size 500nm ball-type MoN nanometer sheets, as lithium-ion electric Pond cathode has good cyclical stability and big high rate performance, has after charge and discharge cycles 400 times when current density is 1A The specific capacity of 600 mAh/g.The nano material synthetic method is simple, favorable reproducibility, and storage lithium is had excellent performance.
Description of the drawings
Fig. 1 is the XRD diagram of MoN；
Fig. 2 is CV curve graphs；
Fig. 3 is the cycle performance figure of MoN；
Fig. 4 is the scanning electron microscope (SEM) photograph of MoN.
Specific implementation mode
The present invention is further illustrated the present invention with the following example, but protection scope of the present invention is not limited to following reality Apply example.
Embodiment 1
A kind of porous spherical MoN that the carbon being made of nanometer sheet is supported, preparation method includes the following steps：By 0.1g MoO2 (acac)2, 0.2g CH4N2S and 0.1g glucose puts 20ml H into2It in O and stirs 1 hour, then puts 200 DEG C of bakings into It is taken out after 12 hours in case, waits for that it is cooled to room temperature, product is centrifuged, be used in combination ethyl alcohol and deionized water to wash several times, put 70 into The drying of DEG C baking oven, obtains the presoma of MoN, is then placed into tube furnace, calcined 4 hours at 800 DEG C under ammonia atmosphere, Obtain the porous spherical MoN materials that the carbon of nanometer sheet composition is supported.
Applications of the MoN as negative material in lithium ion battery, the preparation method of the lithium battery：In mass ratio MoN nanometer sheets：Acetylene black：Kynoar=8:1:1 is coated on copper foil does cathode after mixing, reference electrode and to electricity Pole is lithium piece, and electrolyte is 1M LiClO4EC+DMC solution, wherein volume ratio EC/DMC=1/1, lithium battery assembling is all Operation carries out in glove box.
It is carried out at the same time electric performance test：Prepared size 500nm ball-type MoN nanometer sheets, as lithium ion battery Cathode has good cyclical stability and big high rate performance, has 600 after charge and discharge cycles 400 times when current density is 1A The specific capacity of mAh/g.Fig. 1 is the XRD diagram of MoN, and it is pure phase to show synthesized MoN.Fig. 2 is CV curve graphs, from second Circle starts, and figure almost overlaps the stable electrochemical property for showing MoN.Fig. 3 is the cycle performance figure of MoN, can be with from figure This electrode material is found out in the case where current density is 1 A/g, after 400 circle of cycle, remains to the capacity for keeping 600 mAh/g.Fig. 4 It is the scanning electron microscope (SEM) photograph of MoN, the spherical shape that as can be seen from the figure pattern of MoN is made of nanometer sheet, it can from damaged ball To find out that ball is hollow.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification should all belong to the covering scope of the present invention.

Claims (2)

1. a kind of porous spherical MoN that the carbon being made of nanometer sheet is supported, which is characterized in that preparation method includes following step Suddenly：By 0.1g MoO2(acac)2, 0.2g CH4N2S and 0.1g glucose puts 20ml H into2In O and stir 1 hour, then It puts into 200 DEG C of baking ovens and is taken out after 12 hours, wait for that it is cooled to room temperature, product is centrifuged, ethyl alcohol and deionized water is used in combination to wash Several times, 70 DEG C of baking oven drying are put into, the presoma of MoN is obtained, is then placed into tube furnace, 800 DEG C under ammonia atmosphere Lower calcining 4 hours obtains the porous spherical MoN materials that the carbon of nanometer sheet composition is supported.
2. the application for the porous spherical MoN that a kind of carbon being made of nanometer sheet as described in claim 1 is supported, feature exist In, applications of the MoN as negative material in lithium ion battery, the preparation method of the lithium battery：MoN in mass ratio nanometers Piece：Acetylene black：Kynoar=8:1:1 is coated on copper foil does cathode after mixing, reference electrode and is to electrode Lithium piece, electrolyte are 1M LiClO4EC+DMC solution, wherein volume ratio EC/DMC=1/1, all operations of lithium battery assembling are equal It is carried out in 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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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109841815A (en) * 2019-02-20 2019-06-04 福州大学 A kind of Mo2N/MoO3/C complex lithium ion battery cathode material and preparation method thereof
CN109860535A (en) * 2018-12-18 2019-06-07 福州大学 Fabricated in situ MoS2The method and its application of@MoN hollow sphere
CN110265225A (en) * 2019-05-23 2019-09-20 天津大学 The method for preparing N doping three-dimensional porous carbosphere load molybdenum carbide/molybdenum nitride and iron nano-particle composite material
CN112599753A (en) * 2021-01-07 2021-04-02 福州大学 Preparation and application of SnS @ C graded ball with S defects
CN114156455A (en) * 2021-11-30 2022-03-08 电子科技大学 Heterostructure material for lithium metal battery lithium negative electrode protection, preparation and application
CN114551813A (en) * 2022-02-28 2022-05-27 华中科技大学 Metal lithium composite electrode, preparation method, application and battery

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CN101974714A (en) * 2010-09-13 2011-02-16 长沙伟晖高科技新材料有限公司 Molybdenum titanium carbonitride solid solution and preparation method thereof
CN102034985A (en) * 2010-11-15 2011-04-27 中国科学院青岛生物能源与过程研究所 Oxygen electrode of lithium air battery as well as preparation method and application thereof
CN103123961A (en) * 2011-11-18 2013-05-29 北汽福田汽车股份有限公司 Water-based lithium-air battery
CN103151541A (en) * 2013-03-01 2013-06-12 北京化工大学常州先进材料研究院 Novel air electrode for lithium-air battery and preparation method
CN105206427A (en) * 2015-09-24 2015-12-30 哈尔滨工程大学 Preparation methods for MoN nanometer material and counter electrode

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101974714A (en) * 2010-09-13 2011-02-16 长沙伟晖高科技新材料有限公司 Molybdenum titanium carbonitride solid solution and preparation method thereof
CN102034985A (en) * 2010-11-15 2011-04-27 中国科学院青岛生物能源与过程研究所 Oxygen electrode of lithium air battery as well as preparation method and application thereof
CN103123961A (en) * 2011-11-18 2013-05-29 北汽福田汽车股份有限公司 Water-based lithium-air battery
CN103151541A (en) * 2013-03-01 2013-06-12 北京化工大学常州先进材料研究院 Novel air electrode for lithium-air battery and preparation method
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109860535A (en) * 2018-12-18 2019-06-07 福州大学 Fabricated in situ MoS2The method and its application of@MoN hollow sphere
CN109841815A (en) * 2019-02-20 2019-06-04 福州大学 A kind of Mo2N/MoO3/C complex lithium ion battery cathode material and preparation method thereof
CN110265225A (en) * 2019-05-23 2019-09-20 天津大学 The method for preparing N doping three-dimensional porous carbosphere load molybdenum carbide/molybdenum nitride and iron nano-particle composite material
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
CN112599753A (en) * 2021-01-07 2021-04-02 福州大学 Preparation and application of SnS @ C graded ball with S defects
CN112599753B (en) * 2021-01-07 2021-11-02 福州大学 Preparation and application of SnS @ C graded ball with S defects
CN114156455A (en) * 2021-11-30 2022-03-08 电子科技大学 Heterostructure material for lithium metal battery lithium negative electrode protection, preparation and application
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
CN114551813A (en) * 2022-02-28 2022-05-27 华中科技大学 Metal lithium composite electrode, preparation method, application and battery
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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