CN107946587A - A kind of anode material of lithium-ion battery MnOxPreparation method - Google Patents
A kind of anode material of lithium-ion battery MnOxPreparation method Download PDFInfo
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- CN107946587A CN107946587A CN201711021549.9A CN201711021549A CN107946587A CN 107946587 A CN107946587 A CN 107946587A CN 201711021549 A CN201711021549 A CN 201711021549A CN 107946587 A CN107946587 A CN 107946587A
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- lithium
- ion battery
- anode material
- ammonium persulfate
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
A kind of anode material of lithium-ion battery MnOxPreparation method, manganese acetate and ammonium persulfate are configured to acetic acid manganese solution and ammonium persulfate solution respectively;Lauryl sodium sulfate is dispersed in acetic acid manganese solution and obtains mixed solution;Ammonium persulfate solution is added dropwise in mixed solution, is stirred continuously, it is uniform to system;The system that this is uniformly dissolved moves to ultrasonic generator and is ultrasonically treated to generation black precipitate;Black precipitate is washed, is filtered, drying, up to anode material of lithium-ion battery MnOx.The present invention, using lauryl sodium sulfate as surfactant, first opens manganese source with surfactant-dispersed using manganese acetate and ammonium persulfate as raw material, then adds ammonium persulfate and is uniformly mixed, ultrasound prepares MnOx.Compared with prior art, preparation process of the invention is simple, and raw material is simple and easy to get, and ultrasonic method prepares MnOxThe floriform appearance of piece composition so that the specific surface area active of the negative material substantially increases, and is more advantageous to the embedded abjection of sodium ion, capacity increase.
Description
Technical field
The invention belongs to sodium-ion battery field, and in particular to a kind of anode material of lithium-ion battery MnOxPreparation side
Method.
Background technology
Lithium ion battery is considered as the state-of-the-art power supply of portable electric appts and electric automobile.However, lithium ion
The high cost of battery and limited lithium deposit hinder its application to extensive energy storage, such as regenerative resource and intelligence electricity
Net.In this respect, sodium is due to low cost, in liberal supply (the 4th most abundant element in the earth's crust) and extensive sodium salt mineral deposits,
So that the development of sodium-ion battery is increasingly promoted.Sodium-ion battery with lithium ion battery with some following advantage:(1) it is former
Expect aboundresources, it is of low cost, it is widely distributed;(2) potential of sodium-ion battery compares the high 0.3-0.4V of lithium ion, can utilize
Decomposition potential lower electrolytic salt and electrolyte solvent, the range of choice of electrolyte are more extensive;(3) sodium-ion battery has
Metastable chemical property, use are safer;It there certainly exist some inferior positions, for example the radius of sodium ion is larger, sodium
The insertion abjection process of ion is somewhat more difficult than lithium ion battery, the also higher of the requirement to electrode material structure.Therefore,
It is most important to optimize exploitation of the suitable electrode material for sodium-ion battery.
The positive electrode of sodium-ion battery is mainly oxidized form (A at presentxMO2), i.e., the stratiform knot being made of metal oxide
Structure, the main oxide for studying Na-Co and Na-Mn;Polyanionic, including phosphate material, fluorophosphate, sodium super-ionic are led
Body.For negative material, when alone metallic sodium is as anode, not only by dendrites puzzlement as lithium, but also fusing point is only
, can not safety applications for 97.7 DEG C;By the use of graphite as anode, high transition energy is needed since sodium ion is migrated in graphite layers, is taken off
Embedding difficulty, so the selection of negative material is by as one of significant challenge for eating of research sodium ion point.
Mn oxide has big transmission channel, can provide the gap of sodium ion storage and transport, therefore is ground extensively
Study carefully as anode material of lithium-ion battery.Su et al. is successfully prepared the β-MnO containing exposure crystal face by hydro-thermal method2Nanometer rods
As high performance anode material of lithium-ion battery, 350mAh g are shown-1Charge/discharge capacity.[Su D,Ahn H J,Wang
G.β-MnO2nanorods with exposed tunnel structures as high-performance cathode
materials for sodium-ion batteries[J].Npg Asia Materials,2013,5(11):e70.].But
It is this method long preparation period, is worth in industrial applications little.Zhang et al. is prepared for MnO electrodes, and this electrode is in room
Reversible sodium-ion battery discharge capacity 145mAh g are shown under temperature-1。[Zhang L,Batuk D,Chen G,et
al.Electrochemically activated MnO as a cathode material for sodium-ion
batteries[J].Electrochemistry Communications,2017,77].This method is relatively new, is to be based on
NaPF6Decomposition thought under high voltages, but prepared MnO is not very as the capacity of anode material of lithium-ion battery
It is high.Li et al. people is prepared for MnO/RGO nano wires by two-step method (hydro-thermal+heat treatment), shows good cycle performance
191mAh g-1It is 50mA g in current density-1Under.[Li,Fei,Ma Jingyao,Ren Haijing,et al.,
Fabrication of MnO nanowires implanted in graphene as an advanced anode
material for sodium-ion batteries,Materials Letters 206(2017)132-135.].This method
Preparation process is complex, and graphene is expensive as the prices of raw materials, it is difficult to large-scale industrialized production.
The content of the invention
The object of the present invention is to provide a kind of preparation method is simple, environmental protection, pattern is homogeneous, the sodium-ion battery of excellent performance
Negative material MnOxPreparation method.
For achieving the above object, its specific technical solution is as follows:
1) manganese acetate and ammonium persulfate is taken to be configured to the acetic acid manganese solution and matter that mass fraction is 0.12%-2.37% respectively
Measure the ammonium persulfate solution that fraction is 0.11-3.56%;
2) lauryl sodium sulfate is dispersed in acetic acid manganese solution, stirring is configured to dodecyl sulphur until being completely dissolved
The mass fraction of sour sodium is 1.96%-9% mixed solutions;
3) take 60ml ammonium persulfate solutions to be added dropwise in the mixed solution of 50-180ml, be stirred continuously, it is equal to system
It is even;
4) system for being uniformly dissolved this moves to ultrasonic generator and is ultrasonically treated to generation black precipitate;
5) black precipitate obtained by step 4) is washed, filtered, drying, up to anode material of lithium-ion battery MnOx。
The stirring of the step 2) is magnetic agitation.
The dropwise addition of the step 3) is added dropwise using buret.
The time of the stirring of the step 3) is 1-5h.
Ultrasonic generator in the step 4) is supersonic cleaning machine.
Ultrasonic power in the step 4) is 40-100W.
The ultrasonic time of the step 4) is 2-8h.
The washing of the step 5) is alternately washed using water and acetone.
The present invention is using manganese acetate and ammonium persulfate as raw material, using lauryl sodium sulfate as surfactant, first by manganese
Source is opened with surfactant-dispersed, is then added ammonium persulfate and is uniformly mixed, ultrasound prepares MnOx, can be as sodium-ion battery
Negative material.Compared with prior art, preparation process of the invention is simple, and raw material is simple and easy to get, and ultrasonic method prepares MnOxPiece
The floriform appearance of composition so that the specific surface area active of the negative material substantially increases, and is more advantageous to the embedded abjection of sodium ion,
Capacity increases.
Brief description of the drawings
Fig. 1 is anode material of lithium-ion battery MnO prepared by the present inventionxSEM (scanning electron microscope) figure (amplification factor 20,000
Times).
Fig. 2 is anode material of lithium-ion battery MnO prepared by the present inventionxXRD (X-ray diffraction) figure.
Fig. 3 is anode material of lithium-ion battery MnO prepared by the present inventionxHigh rate performance figure.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and embodiments.
Embodiment 1:
1) manganese acetate and ammonium persulfate is taken to be configured to the acetic acid manganese solution and mass fraction that mass fraction is 0.12% respectively
For 0.11% ammonium persulfate solution;
2) lauryl sodium sulfate is dispersed in acetic acid manganese solution, magnetic agitation is configured to dodecane until being completely dissolved
The mass fraction of base sodium sulphate is 1.96% mixed solution;
3) take 60ml ammonium persulfate solutions to be added dropwise to using buret in the mixed solution of 100ml, 2h is stirred, to body
System is uniform;
4) system for being uniformly dissolved this moves to the supersonic cleaning machine supersound process 3h that power is 40W and sinks to black is produced
Form sediment;
5) black precipitate obtained by step 4) is replaced into washes clean using water and acetone, filtered, drying, up to sodium ion
Cell negative electrode material MnOx.
Embodiment 2:
1) manganese acetate and ammonium persulfate is taken to be configured to the acetic acid manganese solution and mass fraction that mass fraction is 0.56% respectively
For 0.75% ammonium persulfate solution;
2) lauryl sodium sulfate is dispersed in acetic acid manganese solution, magnetic agitation is configured to dodecane until being completely dissolved
The mass fraction of base sodium sulphate is 3.5% mixed solution;
3) take 60ml ammonium persulfate solutions to be added dropwise to using buret in the mixed solution of 50ml, 2h is stirred, to body
System is uniform;
4) system for being uniformly dissolved this moves to the supersonic cleaning machine supersound process 2h that power is 90W and sinks to black is produced
Form sediment;
5) black precipitate obtained by step 4) is replaced into washes clean using water and acetone, filtered, drying, up to sodium ion
Cell negative electrode material MnOx.
Embodiment 3:
1) manganese acetate and ammonium persulfate is taken to be configured to the acetic acid manganese solution and mass fraction that mass fraction is 2.01% respectively
For 1.22% ammonium persulfate solution;
2) lauryl sodium sulfate is dispersed in acetic acid manganese solution, magnetic agitation is configured to dodecane until being completely dissolved
The mass fraction of base sodium sulphate is 5.5% mixed solution;
3) take 60ml ammonium persulfate solutions to be added dropwise to using buret in the mixed solution of 80ml, 4h is stirred, to body
System is uniform;
4) system for being uniformly dissolved this moves to the supersonic cleaning machine supersound process 4h that power is 60W and sinks to black is produced
Form sediment;
5) black precipitate obtained by step 4) is replaced into washes clean using water and acetone, filtered, drying, up to sodium ion
Cell negative electrode material MnOx.
Embodiment 4:
1) manganese acetate and ammonium persulfate is taken to be configured to the acetic acid manganese solution and mass fraction that mass fraction is 0.88% respectively
For 2.52% ammonium persulfate solution;
2) lauryl sodium sulfate is dispersed in acetic acid manganese solution, magnetic agitation is configured to dodecane until being completely dissolved
The mass fraction of base sodium sulphate is 7.5% mixed solution;
3) take 60ml ammonium persulfate solutions to be added dropwise to using buret in the mixed solution of 130ml, 1h is stirred, to body
System is uniform;
4) system for being uniformly dissolved this moves to the supersonic cleaning machine supersound process 6h that power is 70W and sinks to black is produced
Form sediment;
5) black precipitate obtained by step 4) is replaced into washes clean using water and acetone, filtered, drying, up to sodium ion
Cell negative electrode material MnOx.
Embodiment 5:
1) manganese acetate and ammonium persulfate is taken to be configured to the acetic acid manganese solution and mass fraction that mass fraction is 2.37% respectively
For 3.56% ammonium persulfate solution;
2) lauryl sodium sulfate is dispersed in acetic acid manganese solution, magnetic agitation is configured to dodecane until being completely dissolved
The mass fraction of base sodium sulphate is 9% mixed solution;
3) take 60ml ammonium persulfate solutions to be added dropwise to using buret in the mixed solution of 180ml, 5h is stirred, to body
System is uniform;
4) system for being uniformly dissolved this moves to the supersonic cleaning machine supersound process 7h that power is 80W and sinks to black is produced
Form sediment;
5) black precipitate obtained by step 4) is replaced into washes clean using water and acetone, filtered, drying, up to sodium ion
Cell negative electrode material MnOx.
Embodiment 6:
1) manganese acetate and ammonium persulfate is taken to be configured to the acetic acid manganese solution and mass fraction that mass fraction is 1.25% respectively
For 1.83% ammonium persulfate solution;
2) lauryl sodium sulfate is dispersed in acetic acid manganese solution, magnetic agitation is configured to dodecane until being completely dissolved
The mass fraction of base sodium sulphate is 8% mixed solution;
3) take 60ml ammonium persulfate solutions to be added dropwise to using buret in the mixed solution of 150ml, 3h is stirred, to body
System is uniform;
4) system for being uniformly dissolved this moves to the supersonic cleaning machine that power is 100W and is ultrasonically treated 8h to producing black
Precipitation;
5) black precipitate obtained by step 4) is replaced into washes clean using water and acetone, filtered, drying, up to sodium ion
Cell negative electrode material MnOx.
From Fig. 1 to find out, the flower that sheet is self-assembled into is presented in the MnOx anode material of lithium-ion batteries that the present invention prepares
Shape pattern, and be uniformly distributed, general 1 μm of colored diameter.
Figure it is seen that MnO is prepared by the present invention2With the mixed phase of MnO.
As can be seen that the anode material of lithium-ion battery MnO prepared by the preparation method of the present invention from Fig. 3xTool
There is good chemical property, first discharge specific capacity is 514.7mA h g-1(25mA g-1), 50 circle after obstructed current density
Under circulation after reversible specific capacity be 157.6mAh g-1(50mA g-1)。
Claims (8)
- A kind of 1. anode material of lithium-ion battery MnOxPreparation method, it is characterised in that comprise the following steps:1) manganese acetate and ammonium persulfate is taken to be configured to the acetic acid manganese solution and quality point that mass fraction is 0.12%-2.37% respectively Number is the ammonium persulfate solution of 0.11-3.56%;2) lauryl sodium sulfate is dispersed in acetic acid manganese solution, stirring is configured to lauryl sodium sulfate until being completely dissolved Mass fraction be 1.96%-9% mixed solutions;3) take 60ml ammonium persulfate solutions to be added dropwise in the mixed solution of 50-180ml, be stirred continuously, it is uniform to system;4) system for being uniformly dissolved this moves to ultrasonic generator and is ultrasonically treated to generation black precipitate;5) black precipitate obtained by step 4) is washed, filtered, drying, up to anode material of lithium-ion battery MnOx。
- 2. anode material of lithium-ion battery MnO according to claim 1xPreparation method, it is characterised in that:The step 2) stirring is magnetic agitation.
- 3. anode material of lithium-ion battery MnO according to claim 1xPreparation method, it is characterised in that:The step 3) dropwise addition is added dropwise using buret.
- 4. anode material of lithium-ion battery MnO according to claim 1xPreparation method, it is characterised in that:The step 3) time of stirring is 1-5h.
- 5. anode material of lithium-ion battery MnO according to claim 1xPreparation method, it is characterised in that:The step 4) ultrasonic generator in is supersonic cleaning machine.
- 6. anode material of lithium-ion battery MnO according to claim 1xPreparation method, it is characterised in that:The step 4) ultrasonic power in is 40-100W.
- 7. anode material of lithium-ion battery MnO according to claim 1xPreparation method, it is characterised in that:The step 4) ultrasonic time is 2-8h.
- 8. anode material of lithium-ion battery MnO according to claim 1xPreparation method, it is characterised in that:The step 5) washing is alternately washed using water and acetone.
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Cited By (2)
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CN113213543A (en) * | 2021-05-13 | 2021-08-06 | 陕西科技大学 | MnO (MnO)2/V2O3Process for preparing nano composite material |
CN117548105A (en) * | 2024-01-09 | 2024-02-13 | 西南石油大学 | alpha-MnO 2 Nanorod-loaded RuO 2 Positive electrode catalyst of lithium-sulfur battery and preparation method thereof |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113213543A (en) * | 2021-05-13 | 2021-08-06 | 陕西科技大学 | MnO (MnO)2/V2O3Process for preparing nano composite material |
CN117548105A (en) * | 2024-01-09 | 2024-02-13 | 西南石油大学 | alpha-MnO 2 Nanorod-loaded RuO 2 Positive electrode catalyst of lithium-sulfur battery and preparation method thereof |
CN117548105B (en) * | 2024-01-09 | 2024-03-19 | 西南石油大学 | alpha-MnO 2 Nanorod-loaded RuO 2 Positive electrode catalyst of lithium-sulfur battery and preparation method thereof |
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