CN106335930A - Porous spherical cobaltosic oxide electrode material and preparation method and application thereof - Google Patents
Porous spherical cobaltosic oxide electrode material and preparation method and application thereof Download PDFInfo
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- CN106335930A CN106335930A CN201610670497.7A CN201610670497A CN106335930A CN 106335930 A CN106335930 A CN 106335930A CN 201610670497 A CN201610670497 A CN 201610670497A CN 106335930 A CN106335930 A CN 106335930A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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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
- 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
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
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- 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
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- 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
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Abstract
The invention discloses a porous spherical cobaltosic oxide electrode material and a preparation method and an application thereof. The preparation method comprises the steps: mixing a cobalt salt, urea and a solvent to form a solution M; atomizing the solution M, then heating to obtain a spherical cobaltosic oxide material; and calcining the spherical cobaltosic oxide material to obtain the porous spherical cobaltosic oxide electrode material. The prepared porous spherical cobaltosic oxide electrode material is spherical, has a porous structure, facilitates penetration and diffusion of an electrolyte solution, and also facilitates transfer of lithium ions; and the porous spherical cobaltosic oxide electrode material has relatively high specific capacity.
Description
Technical field
The present invention relates to lithium ion battery electrode material field, in particular it relates to porous spherical cobaltosic oxide electrode material
Material and its preparation method and application.
Background technology
Lithium ion battery has voltage height, and electric discharge is steady, heavy-current discharge performance, and specific energy is high, pollution-free, cycle performance
The advantages of good.Lithium ion battery industry is day by day ripe in recent years, is therefore widely used in mobile phone, computer, automobile etc. various
In product, improve constantly with performance of lithium ion battery and improve, the research of the positive electrode of lithium ion battery is also suggested higher
Require.
3d transition metal oxide with cobaltosic oxide as representative is of increased attention, in lithium-ion electric
The fields such as pond, fuel cell, ultracapacitor all show preferable application prospect.In terms of lithium ion battery, four oxidations three
The reversible capacity of cobalt reaches more than the twice of traditional material with carbon element.Battery-grade cobaltosic oxide removes and requires to possess higher purity and shake
Real density is outer, its pattern, structure also have certain requirement.
Content of the invention
It is an object of the invention to provide a kind of porous spherical cobaltosic oxide electrode material and its preparation method and application, system
The porous spherical cobaltosic oxide electrode material obtaining is spherical in shape, has loose structure, is conducive to infiltration and the diffusion of electrolyte, with
When be easy to the transmission of lithium ion, tap density is high, the lithium-ion electric being obtained using this porous spherical cobaltosic oxide electrode material
Pond possesses higher specific capacity.
To achieve these goals, the invention provides a kind of preparation side of porous spherical cobaltosic oxide electrode material
Method, described preparation method includes:
(1) cobalt salt, urea and solvent are mixed, form solution m；
(2) described solution m is heated after atomization, obtained spherical cobaltic-cobaltous oxide material；
(3) described spherical cobaltic-cobaltous oxide material is calcined, obtained porous spherical cobaltosic oxide electrode material.
Present invention also offers a kind of porous spherical cobaltosic oxide electrode material, described porous spherical cobaltosic oxide electricity
Pole material is obtained by above-mentioned preparation method.
Present invention also offers a kind of according to above-mentioned porous spherical cobaltosic oxide electrode material in lithium ion battery
Application.
By technique scheme, the invention provides a kind of porous spherical cobaltosic oxide electrode material and its preparation side
Method and application, described preparation method includes: cobalt salt, urea and solvent is mixed, forms solution m；By described solution m after atomization
Heated, obtained spherical cobaltic-cobaltous oxide material；Described spherical cobaltic-cobaltous oxide material is calcined, is obtained porous spherical
Cobaltosic oxide electrode material；The porous spherical cobaltosic oxide electrode material of preparation is spherical in shape, has loose structure, is conducive to
The infiltration of electrolyte and diffusion, simultaneously facilitate the transmission of lithium ion；This porous spherical cobaltosic oxide electrode material has higher
Specific capacity, under 0.2c multiplying power, discharge capacity is up to 1730mah/g first；Four oxygen that the preparation method that the present invention provides obtains
Change three cobalt scantlings at 1～4 micron, tap density is high；And the method is low for equipment requirements, can be with serialization, scale
Produced in enormous quantities.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Brief description
Accompanying drawing is used to provide a further understanding of the present invention, and constitutes the part of specification, with following tool
Body embodiment is used for explaining the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the electron scanning micrograph of the porous spherical cobaltosic oxide electrode material that embodiment 1 is obtained；
Fig. 2 is the electron scanning micrograph of the porous spherical cobaltosic oxide electrode material that embodiment 2 is obtained；
Fig. 3 is the electron scanning micrograph of the porous spherical cobaltosic oxide electrode material that embodiment 3 is obtained；
Fig. 4 is the electron scanning micrograph of the porous spherical cobaltosic oxide electrode material that embodiment 4 is obtained；
Fig. 5 is the electron scanning micrograph of the porous spherical cobaltosic oxide electrode material that embodiment 5 is obtained；
Fig. 6 is the electron scanning micrograph of the porous spherical cobaltosic oxide electrode material that comparative example 1 is obtained；
Fig. 7 is the charging and discharging curve figure of the lithium ion battery that application examples 1 is obtained.
Reference
1- first time charging curve 11- first time discharge curve
2- second discharge curve of second charging curve 21-
3- third time charging curve 31- third time discharge curve
Specific embodiment
Hereinafter the specific embodiment of the present invention is described in detail.It should be appreciated that it is described herein concrete
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of preparation method of porous spherical cobaltosic oxide electrode material, wherein, described preparation side
Method includes: cobalt salt, urea and solvent is mixed, forms solution m；Described solution m is heated after atomization, is obtained spherical four
Co 3 O material；Described spherical cobaltic-cobaltous oxide material is calcined, is obtained porous spherical cobaltosic oxide electrode material.
So that cobalt salt, urea and solvent can preferably dissolve each other, the present invention one kind preferred embodiment in, institute
State preparation method also to include: carry out ultrasonic disperse after cobalt salt, urea and solvent are mixed, and the time of described ultrasonic disperse is 4-
6min.
So that cobalt salt can preferably dissolve in a solvent, described solvent is deionized water and/or absolute ethyl alcohol.
In the present invention, cobalt salt is selected from one or more of cobalt nitrate, cobalt chloride and cobalt acetate.
The present invention one kind preferred embodiment in, with respect to the described solvent of 20ml, the consumption of described cobalt salt is
0.002-0.04mol, the consumption of described urea is not more than 1g.
So that be obtained porous spherical cobaltosic oxide electrode material possess the excellent infiltration beneficial to electrolyte and
The structure of diffusion, and improve its tap density, in step (2), the temperature of heating is 350-600 DEG C；The temperature of calcining in step (3)
Spend for 300-800 DEG C, the time of calcining is 1-10h.
Present invention also offers a kind of porous spherical cobaltosic oxide electrode material, described porous spherical cobaltosic oxide electricity
Pole material is obtained by above-mentioned preparation method.
Present invention also offers a kind of according to above-mentioned porous spherical cobaltosic oxide electrode material in lithium ion battery
Application, described application process is: by porous spherical cobaltosic oxide electrode material, super p-li conductive black and pvdf bond
Agent is ground, and is tuned into uniform sizing material, on coating Copper Foil, prepared sheet metal a1；Above-mentioned prepared sheet metal a1 is placed in lazy
Property gas in assemble, prepared lithium ion battery；Wherein, with respect to the porous spherical cobaltosic oxide electrode material of 70 weight portions,
The consumption of described super p-li conductive black is 18-22 weight portion, and the consumption of described pvdf adhesive is 8-12 weight portion.
Hereinafter will be described the present invention by embodiment.
Embodiment 1
8g cobalt nitrate hexahydrate, 0.25g urea and 20ml water are mixed and ultrasonic 5min, forms solution m；By described solution m
Heated (heating-up temperature is 350 DEG C) after atomization, obtained spherical cobaltic-cobaltous oxide material；By described spherical cobaltic-cobaltous oxide
Material is calcined (temperature of calcining is 600 DEG C, and calcination time is 2h), obtains porous spherical cobaltosic oxide electrode material
a1；Its SEM (sem) photo such as Fig. 1.
Embodiment 2
8g cobalt nitrate hexahydrate, 0.5g urea and 20ml water are mixed and ultrasonic 5min, forms solution m；By described solution m warp
Heated (heating-up temperature is 450 DEG C) after atomization, obtained spherical cobaltic-cobaltous oxide material；By described spherical cobaltic-cobaltous oxide material
Material is calcined (temperature of calcining is 300 DEG C, and calcination time is 10h), obtains porous spherical cobaltosic oxide electrode material a2；
Its SEM (sem) photo such as Fig. 2.
Embodiment 3
8g cobalt nitrate hexahydrate, 1g urea and 20ml absolute ethyl alcohol are mixed and ultrasonic 5min, forms solution m；Will be described molten
Liquid m is heated (heating-up temperature is 600 DEG C) after atomization, obtains spherical cobaltic-cobaltous oxide material；By described spherical four oxidations
Three cobalt materials are calcined (temperature of calcining is 800 DEG C, and calcination time is 1h), obtain porous spherical cobaltosic oxide electrode material
Material a3；Its SEM (sem) photo such as Fig. 3.
Embodiment 4
8g cobalt acetate, 0.5g urea and 20ml absolute ethyl alcohol are mixed and ultrasonic 5min, forms solution m；By described solution m
Heated (heating-up temperature is 600 DEG C) after atomization, obtained spherical cobaltic-cobaltous oxide material；By described spherical cobaltic-cobaltous oxide
Material is calcined (temperature of calcining is 800 DEG C, and calcination time is 1h), obtains porous spherical cobaltosic oxide electrode material
a4；Its SEM (sem) photo such as Fig. 4.
Embodiment 5
8g cobalt chloride, 0.5g urea and 20ml absolute ethyl alcohol are mixed and ultrasonic 5min, forms solution m；By described solution m
Heated (heating-up temperature is 600 DEG C) after atomization, obtained spherical cobaltic-cobaltous oxide material；By described spherical cobaltic-cobaltous oxide
Material is calcined (temperature of calcining is 800 DEG C, and calcination time is 1h), obtains porous spherical cobaltosic oxide electrode material
a5；Its SEM (sem) photo such as Fig. 5.
Application examples 1
Porous spherical cobaltosic oxide electrode material 7g, super p-li conductive black 2g and pvdf that embodiment 1 is obtained
Adhesive 10g is ground, and is tuned into uniform sizing material, on coating Copper Foil, prepared sheet metal；Above-mentioned prepared sheet metal is placed in
Assemble in inert gas, prepared lithium ion battery；And measure its charging and discharging curve under 0.2c multiplying power, see Fig. 7.
Comparative example 1
By 8g cobalt nitrate hexahydrate and the mixing of 20ml water ultrasonic 5min, form solution m；Described solution m is laggard through being atomized
Row heating (heating-up temperature is 350 DEG C), obtains spherical cobaltic-cobaltous oxide material；Described spherical cobaltic-cobaltous oxide material is forged
Burn (temperature of calcining is 600 DEG C, and calcination time is 2h), obtain porous spherical cobaltosic oxide electrode material d1；Its scanning electricity
Sub- microscope (sem) photo such as Fig. 6.
The porous spherical cobaltosic oxide electrode material a1-a5 being obtained within the scope of the present invention, spherical in shape, there is porous knot
Structure, is conducive to infiltration and the diffusion of electrolyte, simultaneously facilitates the transmission of lithium ion, and its size is at 1～4 micron, vibration density
Degree is high.The lithium ion battery being obtained using this porous spherical cobaltosic oxide electrode material, the electric discharge of circulation, charge ratio for the first time
Capacity is respectively 1730mah/g and 1411mah/g, and efficiency for charge-discharge is up to 81.6%；The electric discharge of second circulation, charging specific volume
Amount is respectively 1383mah/g and 1368mah/g, and efficiency for charge-discharge is 98.9%；The electric discharge of the 5th circulation, charge specific capacity divide
Not Wei 1403mah/g and 1372mah/g, efficiency for charge-discharge is 97.8%, and shows good cyclical stability, this spherical
Porous cobaltosic oxide is higher than significantly all cobaltosic oxide as the specific capacity that lithium ion battery negative material is shown
Theoretical capacity (890mah/g), has good application prospect.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, multiple simple variant can be carried out to technical scheme, this
A little simple variant belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to various can
The combination of energy no longer separately illustrates.
Additionally, can also be combined between the various different embodiment of the present invention, as long as it is without prejudice to this
The thought of invention, it equally should be considered as content disclosed in this invention.
Claims (10)
1. a kind of preparation method of porous spherical cobaltosic oxide electrode material is it is characterised in that described preparation method includes:
(1) cobalt salt, urea and solvent are mixed, form solution m；
(2) described solution m is heated after atomization, obtained spherical cobaltic-cobaltous oxide material；
(3) described spherical cobaltic-cobaltous oxide material is calcined, obtained porous spherical cobaltosic oxide electrode material.
2. preparation method according to claim 1, wherein, in step (1), hybrid mode is ultrasonic disperse, and described
The time of ultrasonic disperse is 4-6min.
3. preparation method according to claim 1 and 2, wherein, described solvent is deionized water and/or absolute ethyl alcohol.
4. preparation method according to claim 1, wherein, described cobalt salt is in cobalt nitrate, cobalt chloride and cobalt acetate
Plant or multiple.
5. preparation method according to claim 1, wherein, with respect to the described solvent of 20ml, the consumption of described cobalt salt is
0.002-0.04mol, the consumption of described urea is not more than 1g.
6. preparation method according to claim 1, wherein, in step (2), the temperature of heating is 350-600 DEG C.
7. preparation method according to claim 1, wherein, in step (3), the temperature of calcining is 300-800 DEG C, calcining
Time is 1-10h.
8. a kind of porous spherical cobaltosic oxide electrode material is it is characterised in that described porous spherical cobaltosic oxide electrode material
Preparation method described in any one in claim 1-7 for the material is obtained.
9. application in lithium ion battery for a kind of porous spherical cobaltosic oxide electrode material according to claim 8；
Preferably, described application process is: by porous spherical cobaltosic oxide electrode material, super p-li conductive black and pvdf
Adhesive is ground, and is tuned into uniform sizing material, on coating Copper Foil, prepared sheet metal a1；Above-mentioned prepared sheet metal a1 is put
Assemble in inert gas, prepared lithium ion battery.
10. application according to claim 9 is it is characterised in that porous spherical cobaltosic oxide with respect to 70 weight portions
Electrode material, the consumption of described super p-li conductive black is 18-22 weight portion, and the consumption of described pvdf adhesive is 8-12 weight
Amount part.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108946824A (en) * | 2018-09-14 | 2018-12-07 | 兰州金川新材料科技股份有限公司 | A kind of preparation method of big granularity cobaltosic oxide |
| CN108946825A (en) * | 2018-09-14 | 2018-12-07 | 兰州金川新材料科技股份有限公司 | A kind of preparation method of small grain size cobaltosic oxide |
| CN109205684A (en) * | 2018-09-14 | 2019-01-15 | 兰州金川新材料科技股份有限公司 | A kind of preparation method of small grain size cobaltosic oxide |
| CN110112391A (en) * | 2019-05-10 | 2019-08-09 | 安徽师范大学 | Spherical carbon coating cobaltosic oxide composite material and its preparation method and application |
| CN114242960A (en) * | 2021-10-28 | 2022-03-25 | 广东邦普循环科技有限公司 | Hollow spherical particle anode material with opening and preparation method and application thereof |
| CN114804220A (en) * | 2022-04-25 | 2022-07-29 | 广东邦普循环科技有限公司 | Porous spherical cobalt oxide particles and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108946824A (en) * | 2018-09-14 | 2018-12-07 | 兰州金川新材料科技股份有限公司 | A kind of preparation method of big granularity cobaltosic oxide |
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| CN108946824B (en) * | 2018-09-14 | 2020-04-07 | 兰州金川新材料科技股份有限公司 | Preparation method of large-particle-size cobaltosic oxide |
| CN108946825B (en) * | 2018-09-14 | 2020-07-03 | 兰州金川新材料科技股份有限公司 | Preparation method of small-particle-size cobaltosic oxide |
| CN109205684B (en) * | 2018-09-14 | 2020-07-03 | 兰州金川新材料科技股份有限公司 | Preparation method of small-particle-size cobaltosic oxide |
| CN110112391A (en) * | 2019-05-10 | 2019-08-09 | 安徽师范大学 | Spherical carbon coating cobaltosic oxide composite material and its preparation method and application |
| CN110112391B (en) * | 2019-05-10 | 2021-08-27 | 安徽师范大学 | Spherical carbon-coated cobaltosic oxide composite material and preparation method and application thereof |
| CN114242960A (en) * | 2021-10-28 | 2022-03-25 | 广东邦普循环科技有限公司 | Hollow spherical particle anode material with opening and preparation method and application thereof |
| WO2023071393A1 (en) * | 2021-10-28 | 2023-05-04 | 广东邦普循环科技有限公司 | Hollow-spherical-particle negative electrode material with openings, and preparation method therefor and use thereof |
| CN114804220A (en) * | 2022-04-25 | 2022-07-29 | 广东邦普循环科技有限公司 | Porous spherical cobalt oxide particles and preparation method thereof |
| CN114804220B (en) * | 2022-04-25 | 2023-07-07 | 广东邦普循环科技有限公司 | Porous spherical cobalt oxide particles and preparation method thereof |
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