CN106207148A - A kind of preparation method of lithium ion battery negative material micro nano structure CuO - Google Patents

A kind of preparation method of lithium ion battery negative material micro nano structure CuO Download PDF

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Publication number
CN106207148A
CN106207148A CN201610783345.8A CN201610783345A CN106207148A CN 106207148 A CN106207148 A CN 106207148A CN 201610783345 A CN201610783345 A CN 201610783345A CN 106207148 A CN106207148 A CN 106207148A
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China
Prior art keywords
cuo
lithium ion
ion battery
nano structure
battery negative
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CN201610783345.8A
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Chinese (zh)
Inventor
许赞扬
张鑫
巩海波
樊帆
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Qinghai Zhongxing New Energy Co Ltd
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Qinghai Zhongxing New Energy Co Ltd
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Priority to CN201610783345.8A priority Critical patent/CN106207148A/en
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    • 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
    • H01M4/483Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00Compounds of copper
    • C01G3/02Oxides; Hydroxides
    • 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
    • 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
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Electrochemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Composite Materials (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

The invention discloses can be as micro nano structure CuO (the Copper oxide of a kind of lithium ion battery negative material, it is called for short CuO) preparation method of material, the method is with copper sulphate pentahydrate for copper source, carbamide is as precipitant, under conditions of without adding any surfactant, hydro-thermal method is used to be successfully prepared the CuO material of the micro nano structure being self-assembly of by nanometer sheet;This method equipment is simple, and technological parameter is controlled, repeatable high.Prepare needed raw material to enrich, low cost, produce without garbage.CuO is applied in fields such as high-temperature superconductor, optical switch, ultracapacitor, lithium ion battery negative materials as a kind of P-type semiconductor.

Description

A kind of preparation method of lithium ion battery negative material micro nano structure CuO
Technical field
The invention belongs to technical field of nanometer material preparation, particularly relate to a kind of use hydro-thermal method to prepare lithium ion battery to bear The method of pole material micro-nano rice structure C uO.
Background technology
Lithium ion battery owing to having that output voltage is high, energy density big, have extended cycle life and the advantage such as green non-pollution, It is widely used to all kinds of portable electric appts, electric automobile field, and has wide in terms of new forms of energy electric power storage Application prospect.But, current business-like lithium ion battery mainly with graphite as negative pole, theoretical specific capacity low (372mAh/g), To can not meet the new forms of energy electric power storage high power and high energy application demand that develop rapidly.Metal-oxide is because of its specific capacity The advantages such as height, rich reserves and environmental protection become potential graphite substituted type negative material.Negative pole as lithium ion battery Material C uO is that the advantage of the aspects such as a kind of specific capacity high (670mAh/g), cheap, nontoxic, preparation is simple receives much concern. CuO as a kind of P-type semiconductor in fields such as high-temperature superconductor, optical switch, ultracapacitor, lithium ion battery negative materials It is applied.
Summary of the invention
It is an object of the invention to overcome the defect of prior art, it is provided that a kind of micro-nano knot of lithium ion battery negative material The preparation method of structure CuO, the method low cost, simple to operate.
It is an object of the invention to be achieved through the following technical solutions, a kind of micro-nano knot of lithium ion battery negative material The preparation method of structure CuO, the method comprises the following steps:
(1) distilled water, carbamide 50:1 in mass ratio is mixed, and stir more than 5 hours, obtain clear liquor;
(2) under conditions of stirring, the clear liquor in step 1 drips in copper sulfate solution, copper sulfate and step 1 The mol ratio of carbamide is 1:2, obtains light blue color contamination liquid after being stirred at room temperature 30-60min, by light blue color contamination liquid, transfers to water Thermal response still reacts at 180 DEG C 8h;
(3) by centrifugal for the product obtained by step 2 and use deionized water and absolute ethanol washing, vacuum drying successively After obtain CuO.
The invention has the beneficial effects as follows: this method equipment is simple, and technological parameter is controlled, repeatable high.Preparation is required Abundant raw material, low cost, produce without garbage.Preparation micro nano structure CuO negative material lithium ion battery and other Field has great potentiality to apply.
Accompanying drawing explanation
Fig. 1 is the SEM picture of micro nano structure CuO of the present invention;
Fig. 2 is the SEM picture of micro nano structure CuO of the present invention;
Fig. 3 is the SEM picture of micro nano structure CuO of the present invention;
Fig. 4 is sample XRD spectra and the contrast of standard spectrogram of CuO of the present invention;
Detailed description of the invention
Below in conjunction with specific embodiment, it is further elucidated with the present invention.Should be understood that these embodiments are merely to illustrate the present invention Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art The present invention is made various changes or modifications by member, and these equivalent form of values fall within the model that the application appended claims is limited equally Enclose.
The method of lithium ion battery negative material micro nano structure CuO of the present invention, comprises the following steps:
(1) distilled water, carbamide 50:1 in mass ratio is mixed, stir more than 5 hours, obtain clarifying mixed liquid;
(2) under conditions of stirring, the clear liquor in step 1 drips in copper sulfate solution, copper sulfate and step 1 The mol ratio of carbamide is 1:2, after being stirred at room temperature 30-60min, by light blue color contamination liquid, transfers in hydrothermal reaction kettle in 180 8h is reacted at DEG C;
(3) by centrifugal for product, use deionized water and absolute ethanol washing, vacuum drying successively after obtain CuO powder.
Embodiment 1
(1) 60ml distilled water is mixed with 1.2g carbamide, magnetic agitation 6 hours, obtain settled solution;
(2) under conditions of stirring, the clear liquor in step 1 drips 0.01mol copper-bath, at room temperature stirs After mixing 50min, light blue solution is transferred to react at 180 DEG C in hydrothermal reaction kettle 8h;
(3) by centrifugal for product, use deionized water and absolute ethanol washing twice successively, obtain after putting into vacuum drying CuO micro-nano powder.Spherical micro nano structure CuO pattern obtained by the present invention is shown in scanned picture 1,2,3, can from figure Going out, obtained self assembly CuO nanostructured, form is homogeneous, regular, is petal lamellar spherical structure.This petal lamellar The CuO of spherical structure is especially beneficial lithium ion battery in charging process, more Lithium-ion embeding negative material, thus can increase The charge/discharge capacity of big lithium ion battery, and improve the charge-discharge electric power of lithium ion battery.
Fig. 4 is sample XRD spectra and the contrast of standard spectrogram of CuO of the present invention, is found by contrast, and the present invention is spherical micro- The position of all diffraction maximums of X-ray diffraction of nano-sized CuO and diffracted intensity and CuO standard diffraction spectrogram (JCPDS NO.04-004-5685) suffer from well mating, thus can determine that the lithium ion battery negative material obtained by the present invention is micro- Nano-sized CuO purity is fabulous, and the oxide etc. without other copper exists.
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert The detailed description of the invention of the present invention is only limitted to this, for general technical staff of the technical field of the invention, is not taking off On the premise of present inventive concept, it is also possible to make some simple deduction or replace, all should be considered as belonging to the present invention by institute The claims submitted to determine scope of patent protection.

Claims (1)

1. the preparation method of a lithium ion battery negative material micro nano structure CuO, it is characterised in that the method includes following Step:
(1) distilled water, carbamide 50:1 in mass ratio is mixed, and stir more than 5 hours, obtain clear liquor;
(2) under conditions of stirring, the clear liquor in step 1 drips copper sulfate solution, copper sulfate and carbamide in step 1 Mol ratio be 1:2, obtain light blue color contamination liquid after being stirred at room temperature 30-60min, by light blue color contamination liquid, transfer to hydro-thermal anti- Answer and still reacts at 180 DEG C 8h;
(3) obtain after the product obtained by step 2 being centrifuged and uses deionized water and absolute ethanol washing, vacuum drying successively To CuO.
CN201610783345.8A 2016-08-31 2016-08-31 A kind of preparation method of lithium ion battery negative material micro nano structure CuO Pending CN106207148A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112047372A (en) * 2020-09-08 2020-12-08 浙江大学 CuO porous nanosheet, preparation method thereof and application thereof in thermal catalysis and photo-thermal catalysis
CN113675393A (en) * 2021-08-20 2021-11-19 西安热工研究院有限公司 Morphology-controllable high-performance lithium ion battery negative electrode material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101407332A (en) * 2007-10-12 2009-04-15 新疆大学 Hydro-thermal synthesis method for cupric oxide nano-rod
CN102267714A (en) * 2010-06-03 2011-12-07 合肥学院 Preparation method for hollow silk cocoon-like CuO nanomaterial
CN102381725A (en) * 2010-08-31 2012-03-21 合肥学院 Preparation method of hollow pumpkin-shaped CuO nano-material
CN104108738A (en) * 2013-04-22 2014-10-22 广东致卓精密金属科技有限公司 Method for using copper sulfate waste liquid to prepare high-purity spherical copper oxide

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101407332A (en) * 2007-10-12 2009-04-15 新疆大学 Hydro-thermal synthesis method for cupric oxide nano-rod
CN102267714A (en) * 2010-06-03 2011-12-07 合肥学院 Preparation method for hollow silk cocoon-like CuO nanomaterial
CN102381725A (en) * 2010-08-31 2012-03-21 合肥学院 Preparation method of hollow pumpkin-shaped CuO nano-material
CN104108738A (en) * 2013-04-22 2014-10-22 广东致卓精密金属科技有限公司 Method for using copper sulfate waste liquid to prepare high-purity spherical copper oxide

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
XIAODI LIU ET AL: "Morphology- and facet-controlled synthesis of CuO micro/nanomaterials and analysis of their lithium ion storage properties", 《JOURNAL OF POWER SOURCES》 *
王晨等: "锂离子电池CuO负极材料的制备及其电化学性能研究", 《中国博学位论文全文数据库工程科技Ⅱ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112047372A (en) * 2020-09-08 2020-12-08 浙江大学 CuO porous nanosheet, preparation method thereof and application thereof in thermal catalysis and photo-thermal catalysis
CN112047372B (en) * 2020-09-08 2022-03-25 浙江大学 CuO porous nanosheet, preparation method thereof and application thereof in thermal catalysis and photo-thermal catalysis
CN113675393A (en) * 2021-08-20 2021-11-19 西安热工研究院有限公司 Morphology-controllable high-performance lithium ion battery negative electrode material and preparation method thereof

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