CN106938852A - A kind of preparation method of lithium ion battery negative material nanometer CuO - Google Patents

A kind of preparation method of lithium ion battery negative material nanometer CuO Download PDF

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Publication number
CN106938852A
CN106938852A CN201710039267.5A CN201710039267A CN106938852A CN 106938852 A CN106938852 A CN 106938852A CN 201710039267 A CN201710039267 A CN 201710039267A CN 106938852 A CN106938852 A CN 106938852A
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CN
China
Prior art keywords
lithium ion
ion battery
negative material
battery negative
preparation
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Pending
Application number
CN201710039267.5A
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Chinese (zh)
Inventor
黄技军
李海
周鹏伟
戴涛
赵东辉
李冰蟾
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Fujian Xfh Battery Material Co Ltd
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Fujian Xfh Battery Material Co Ltd
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Priority to CN201710039267.5A priority Critical patent/CN106938852A/en
Publication of CN106938852A publication Critical patent/CN106938852A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00Compounds of copper
    • C01G3/02Oxides; Hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses a kind of preparation method of lithium ion battery negative material nanometer CuO, specific preparation method is that a water acetic acid copper is put into the Muffle furnace with heating schedule, open Muffle furnace, 500 800 DEG C of predetermined temperature is raised to from room temperature, programming rate is 35 °/min, and in predetermined temperature, 500 800 DEG C are incubated 2 10 hours, then take out, room temperature is cooled to, lithium ion battery negative material nanometer CuO is obtained.Preparing CuO has excellent electrochemical cycle stability, and the preparation method of the lithium ion battery negative material nanometer CuO is simple, and reaction condition is easily reached, and is adapted to be prepared on a large scale.

Description

A kind of preparation method of lithium ion battery negative material nanometer CuO
Technical field
The present invention relates to the preparation method of lithium ion battery negative material, specifically a kind of lithium ion battery negative material is used The preparation method of nanometer CuO, belongs to field of electrochemical power source.
Background technology
With the fast development of emerging economies, global energy consumption sharp increase.Lithium ion battery is with its high voltage, height Energy density, have extended cycle life, have a safety feature, it is with low cost the advantages of in portable electrics such as computer, camera and mobile phones Have been obtained for being widely applied in sub- equipment.In recent years, countries in the world all actively develop lithium ion battery apply to mixing Power electric automobile(HEV), pure electric automobile(PEV)Deng research, but lithium ion battery is used as the main of vehicle mounted dynamic battery Bottleneck is the performance of lithium ion battery negative material.
Graphite is current most widely used lithium ion battery negative material, however, the theoretical capacity of graphite only has 372 MAh/g, it is impossible to meet the demand of the height ratio capacity of power source, transition metal oxide is with its outstanding electrochemical lithium storage performance Receive much concern.As the CuO of Typical Representative due to higher theoretical capacity(672mAh/g), extensive resource reserve, valency The appropriateness of lattice and it is environmentally friendly the advantages of attract attention.But, CuO electrodes can influence electric charge due to its low electric conductivity Transmission in the electrodes, and then influence electrochemical lithium storage performance.In addition, CuO electrode materials are due to will be through in charge and discharge process By obvious structural failure efflorescence is caused than larger volumetric expansion, then cause the rapid decrease of circulation volume.
The content of the invention
There is provided a kind of preparation side of lithium ion battery negative material nanometer CuO for existing technical problem by the present invention Method, the nanometer CuO negative material with excellent electrochemical performance is prepared by simple efficient fused salt combustion synthesis method.
To achieve the above object, the present invention provides following technical scheme:A kind of lithium ion battery negative material nanometer CuO Preparation method, it is characterised in that it comprises the following steps:
(1)One water acetic acid copper is put into the Muffle furnace with heating schedule, Muffle furnace is opened, predetermined temperature is raised to from room temperature 500-800 DEG C, programming rate is 3-5 °/min, and in predetermined temperature, 500-800 DEG C is incubated 2-10 hours, then takes out, is cooled to Room temperature, obtains lithium ion battery negative material nanometer CuO.
Further, preferably, step(1)Described in a water acetic acid copper purity > 99.9%.
Compared with prior art, the beneficial effects of the invention are as follows:
(1)The inventive method has the reaction time short, and technique is simple, easily realizes industrialization large-scale production;
(2)Prepared nanometer CuO material electrochemical performance is excellent, there is potential application in lithium ion battery.
Brief description of the drawings
The XRD of sample prepared by Fig. 1 embodiments 1.
The SEM figures of sample prepared by Fig. 2 embodiments 1.
The cycle performance figure of sample prepared by Fig. 3 embodiments 1.
Embodiment
Embodiment 1
A kind of preparation method of lithium ion battery negative material nanometer CuO, it comprises the following steps:
(1)Purity is put into the Muffle furnace with heating schedule for a 99.95% water acetic acid copper, Muffle furnace is opened, from room temperature 500-800 DEG C of predetermined temperature is raised to, programming rate is 3-5 °/min, and 500-800 DEG C is incubated 2-10 hours in predetermined temperature, so After take out, be cooled to room temperature, obtain lithium ion battery negative material nanometer CuO.
X-ray diffraction, which is determined, shows that obtained nanometer CuO is monoclinic crystal structure(Accompanying drawing 1), surveyed by stereoscan photograph Surely it is ~ 300 nm to show nanometer CuO particle size(Accompanying drawing 2).
With the nanometer CuO of the present invention:SP:PVDF=8:1:1 (weight ratio), plus appropriate NMP mixing are tuned into pulpous state, are coated on Negative plate is made within 12 hours on Copper Foil and in drying in vacuum drying chamber, using metal lithium sheet be to electrode, Celgard films for every Film, electrolyte is 1M liPF6/ EC+DEC+DMC=1:1:1, it is assembled into CR2032 type batteries in the glove box that argon gas is protected. Battery pack stands 8h after installing, then carries out constant current charge-discharge test with CT2001A battery test systems, and test voltage is 0.02 ~3V.Fig. 3 is cycle performance figure of the prepared nanometer CuO as lithium ion battery negative, first under 0.5 A/g current densities Secondary specific discharge capacity is up to 1058 mAh/g, and specific discharge capacity is respectively 342.4 mAh/g after 40 circulations, it is shown that very well Stable circulation performance.

Claims (2)

1. a kind of preparation method of lithium ion battery negative material nanometer CuO, it is characterised in that it comprises the following steps:
(1)One water acetic acid copper is put into the Muffle furnace with heating schedule, Muffle furnace is opened, predetermined temperature is raised to from room temperature 500-800 DEG C, programming rate is 3-5 °/min, and in predetermined temperature, 500-800 DEG C is incubated 2-10 hours, then takes out, is cooled to Room temperature, obtains lithium ion battery negative material nanometer CuO.
2. preparation method according to claim 1, it is characterised in that step(1)In, a described water acetic acid copper is pure Spend > 99.9%.
CN201710039267.5A 2017-01-19 2017-01-19 A kind of preparation method of lithium ion battery negative material nanometer CuO Pending CN106938852A (en)

Priority Applications (1)

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CN201710039267.5A CN106938852A (en) 2017-01-19 2017-01-19 A kind of preparation method of lithium ion battery negative material nanometer CuO

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Application Number Priority Date Filing Date Title
CN201710039267.5A CN106938852A (en) 2017-01-19 2017-01-19 A kind of preparation method of lithium ion battery negative material nanometer CuO

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Publication Number Publication Date
CN106938852A true CN106938852A (en) 2017-07-11

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107732224A (en) * 2017-09-15 2018-02-23 福建翔丰华新能源材料有限公司 The method for improving negative material CuO cyclical stabilities
CN107792890A (en) * 2017-09-15 2018-03-13 福建翔丰华新能源材料有限公司 The method for preparing nano NiO lithium ion battery negative material
CN108862364A (en) * 2018-09-21 2018-11-23 东北大学 A kind of molten salt solvent method preparation nanometer Cu2The method of O particle
CN108987703A (en) * 2018-07-17 2018-12-11 澳洋集团有限公司 A kind of preparation method based on copper oxide composite lithium ion battery negative electrode material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103172506A (en) * 2013-03-21 2013-06-26 常州大学 Method for preparing croconic acid by using nanometer copper oxide as catalyst
CN103979600A (en) * 2014-05-30 2014-08-13 上海沃凯生物技术有限公司 Preparation method of ultrathin copper oxide powder

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103172506A (en) * 2013-03-21 2013-06-26 常州大学 Method for preparing croconic acid by using nanometer copper oxide as catalyst
CN103979600A (en) * 2014-05-30 2014-08-13 上海沃凯生物技术有限公司 Preparation method of ultrathin copper oxide powder

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
KELI ZHANG等: "The kinetics of thermal dehydration of copper(II) acetate monohydrate in air", 《THERMOCHIMICA ACTA 》 *
ZHENKUN LIN等: "Study on thermal decomposition of copper(II) acetate monohydrate in air", 《J THERM ANAL CALORIM》 *
吕军军等: "草酸铜及纳米氧化铜的制备与表征", 《火***学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107732224A (en) * 2017-09-15 2018-02-23 福建翔丰华新能源材料有限公司 The method for improving negative material CuO cyclical stabilities
CN107792890A (en) * 2017-09-15 2018-03-13 福建翔丰华新能源材料有限公司 The method for preparing nano NiO lithium ion battery negative material
CN108987703A (en) * 2018-07-17 2018-12-11 澳洋集团有限公司 A kind of preparation method based on copper oxide composite lithium ion battery negative electrode material
CN108862364A (en) * 2018-09-21 2018-11-23 东北大学 A kind of molten salt solvent method preparation nanometer Cu2The method of O particle

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Application publication date: 20170711

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