CN108002444A - A kind of KMn8O16The preparation method of positive electrode - Google Patents
A kind of KMn8O16The preparation method of positive electrode Download PDFInfo
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- CN108002444A CN108002444A CN201711247445.XA CN201711247445A CN108002444A CN 108002444 A CN108002444 A CN 108002444A CN 201711247445 A CN201711247445 A CN 201711247445A CN 108002444 A CN108002444 A CN 108002444A
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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
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- 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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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
The invention discloses a kind of KMn8O16The preparation method of positive electrode.Potassium hydroxide and potassium permanganate are dissolved in deionized water first, obtain purple mixed solution, then manganese sulfate is dissolved in deionized water, obtains lightpink solution.Under magnetic stirring, above-mentioned lightpink solution is slowly dropped into above-mentioned purple mixed solution, precipitation quickly forms, and continues to stir and still aging, presoma is obtained after filtration drying.Presoma is placed in deionized water and carries out hydro-thermal process, is placed on again after filtration drying in Muffle furnace and carries out calcination processing, up to final product KMn after cooling8O16.KMn prepared by the present invention8O16Positive electrode crystallinity is high and without other impurities element, and particle is smaller, the insertion and abjection of lithium ion of being more convenient for, with excellent chemical property during as anode material for lithium-ion batteries.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries and technical field of new energy material preparation, and in particular to a kind of
KMn8O16The preparation method of positive electrode.
Background technology
The energy and environmental problem are world today's subjects under discussion of greatest concern.At present, the annual consumption of fossil energy accounts for entirely
More than the 85% of ball energy total flow, and fossil energy reserves are limited, meanwhile, the use of fossil energy can trigger environment dirty
The environmental problems such as dye, greenhouse effects, haze, therefore be badly in need of exploring new energy system.Solar energy, wind energy, tide energy etc. can be again
The raw energy has the function of natural self-regeneration, but since these new energy systems have very strong region and intermittence, makes
Obtain its effective utilizes and be faced with many technical problems, and scale energy storage is to solve the key technology of these problems.In various storages
In energy mode, electrochemical energy storage is a kind of the easiest, efficient mode, becomes the mainstream of energy storage technology development.Wherein lithium from
Sub- battery is because it is with energy density is high, operating voltage is high, have extended cycle life, self-discharge rate is small and the protrusion such as environmentally protective is excellent
Gesture, is widely applied in fields such as mobile phone, laptop, digital camera, electric tools, and progressively to new-energy automobile
Expanded with fields such as energy storage.
For the lithium ion battery of high-energy-density, oxide is a kind of electrode material being widely used.In oxygen
Strong oxygen metallic bond in compound causes transition metal oxide to have high ionic feature so that compound has high electricity
Position.Manganese and oxygen compound not only aboundresources, it is cheap, and have the function of it is changeable form, complicated structure and peculiar.
The KMn of Cryptomelane types8O16It is the natural manganese and oxygen compound with pore passage structure for tetragonal system, it is by every two, side
The MnO on side altogether6Octahedron connects into the pore passage structure of 2*2, and channel diameter is about 0.46nm or so, and the cation in duct is with K
For main component.The presence of K ions can not only holding structure stability, the diffusion rate of ion can also be improved.
The KMn of Cryptomelane types at present8O16Synthetic method mainly have hydro-thermal method, microwave process for synthesizing, the precipitation method, stream
Covert method etc..Most synthetic methods are acid synthesis condition, and the material morphology of microwave process for synthesizing synthesis is poor and particle diameter is in micron
It is more than level, and the more difficult control of reaction temperature, it is difficult to realize large-scale production.Partially synthetic method also there is length experimental period,
The problems such as energy waste is serious.
The content of the invention
For existing KMn8O16Long preparation period, the problems such as energy waste is serious, synthesis condition is single, the present invention provide
A kind of simple and practicable, electrochemical performance KMn8O16The preparation method of positive electrode.
The technical scheme is that：
A kind of KMn8O16The preparation method of positive electrode, includes the following steps：
(1) at room temperature, KOH is dissolved in deionized water, KMnO is added after solution cooling4, magnetic agitation is to complete
Purple mixed solution is obtained after dissolving；By MnSO4·H2O is added in deionized water, and magnetic agitation obtains light pink to after being completely dissolved
Color solution；
(2) above-mentioned MnSO is slowly added dropwise into purple mixed solution obtained by step (1)4Lightpink solution, after precipitation generation
Continue magnetic agitation 20~30 minutes, obtain dark brown suspension；
(3) by suspension obtained by step (2) be aged at room temperature 12~24 it is small when, before obtaining dark brown after filtration drying
Drive body；
(4) deionized water is added into presoma obtained by step (3), magnetic agitation 10~20 minutes, obtains dark brown and hang
Supernatant liquid；
(5) suspension obtained by step (4) is placed in autoclave and carries out hydro-thermal process, obtain black precipitate；
(6) black precipitate obtained by step (5) is placed in Muffle furnace and carries out calcination processing, that is, obtain final product
KMn8O16。
Further, in step (1), KOH and KMnO4The ratio between the amount of material be 25~35:1.
Further, in step (2), MnSO4·H2O and KMnO4The ratio between the amount of material be 1.5~3.0:1.
Further, in step (4), the mass ratio of presoma and deionized water is 1:20~30.
Further, in step (5), hydro-thermal process temperature is 160~200 DEG C, when hydrothermal conditions are 8~24 small.
Further, the calcination processing in step (6), is specially：With the heating rate of 5~10 DEG C/min, from room temperature liter
To 450~550 DEG C, when insulation 2~4 is small, it is cooled to room temperature afterwards.
With the KMn synthesized at present8O16Compare, KMn prepared by the present invention8O16With following advantage：
(1) present invention prepares KMn using chemical precipitation method and hydro-thermal method8O16, have preparation flow simple, be easy to repeat,
It is energy saving during section, the advantages that mild condition；
(2) KMn prepared by the present invention8O16, the KMn with other methods preparation8O16To compare, its particle is smaller, is nanoscale,
Crystallinity is high and without other impurities element, as anode material for lithium-ion batteries, has very excellent chemical property.
Brief description of the drawings
Fig. 1 is KMn prepared by the embodiment of the present invention 48O16X-ray diffraction (XRD) figure of positive electrode；
Fig. 2 is KMn prepared by the embodiment of the present invention 48O16(amplification factor is scanning electron microscope (SEM) figure of positive electrode
25000 times)；
Fig. 3 is KMn prepared by the embodiment of the present invention 48O16Positive electrode is in 50mA g-1Charging and discharging curve under current density
Figure；
Fig. 4 is KMn prepared by the embodiment of the present invention 48O16As positive electrode, using lithium piece as to electrode, button is assembled into
Battery.(20~25 DEG C) at room temperature, in the voltage range of 1.5~4.2V, 50mA g-1Charge-discharge test is carried out under current density
Cycle life figure.
Embodiment
With reference to specific embodiment, the present invention will be further described, but the present invention is not limited thereto.
Test method in following embodiments, is conventional method unless otherwise instructed.
Embodiment 1
(20~25 DEG C) at room temperature, the KOH of 8.42g are dissolved in the deionized water of 40mL, magnetic force stirs at 500 rpm
Mix 10 minutes, after solution cooling, add the KMnO of 0.79g4, magnetic agitation 10 minutes, are configured to 50mL's at 500 rpm
Purple mixed solution；By the MnSO of 1.27g4·H2O is dissolved in the deionized water of 50mL, and magnetic agitation 10 is divided at 500 rpm
Clock, obtains lightpink solution；Under the magnetic agitation of 500rpm, it is molten that above-mentioned lightpink solution is slowly dropped into above-mentioned purple mixing
In liquid, dark brown precipitation is quickly generated, and is continued magnetic agitation 30 minutes, is obtained dark brown suspension；Suspension is placed in
When ageing 16 is small at room temperature, dark brown presoma is obtained after filtration drying；Weigh 2.0g presomas to be placed in autoclave, add
Enter 40mL deionized waters, at 500 rpm magnetic agitation 15 minutes, obtain dark brown suspension；It is carried out at 180 DEG C of hydro-thermals
Manage 12 it is small when, cooling centrifugal drying after obtain black solid；Black solid is moved into porcelain boat, is placed in Muffle furnace and calcines, with 5
DEG C/heating rate of min, 500 DEG C are raised to from room temperature, when insulation 2 is small, is cooled to room temperature obtains final product afterwards
KMn8O16。
Embodiment 2
(20~25 DEG C) at room temperature, the KOH of 8.42g are dissolved in the deionized water of 40mL, magnetic force stirs at 500 rpm
Mix 10 minutes, after solution cooling, add the KMnO of 0.79g4, magnetic agitation 10 minutes, are configured to 50mL's at 500 rpm
Purple mixed solution；By the MnSO of 1.69g4·H2O is dissolved in the deionized water of 50mL, and magnetic agitation 10 is divided at 500 rpm
Clock, obtains lightpink solution；Under the magnetic agitation of 500rpm, it is molten that above-mentioned lightpink solution is slowly dropped into above-mentioned purple mixing
In liquid, dark brown precipitation is quickly generated, and is continued magnetic agitation 20 minutes, is obtained dark brown suspension；Suspension is placed in
When ageing 12 is small at room temperature, dark brown presoma is obtained after filtration drying；Weigh 2.0g presomas to be placed in autoclave, add
Enter 45mL deionized waters, at 500 rpm magnetic agitation 20 minutes, obtain dark brown suspension；It is carried out at 180 DEG C of hydro-thermals
Manage 24 it is small when, cooling centrifugal drying after obtain black solid；Black solid is moved into porcelain boat, is placed in Muffle furnace and calcines, with 5
DEG C/heating rate of min, 450 DEG C are raised to from room temperature, when insulation 4 is small, is cooled to room temperature obtains final product afterwards
KMn8O16。
Embodiment 3
(20~25 DEG C) at room temperature, the KOH of 8.42g are dissolved in the deionized water of 40mL, magnetic force stirs at 500 rpm
Mix 10 minutes, after solution cooling, add the KMnO of 0.79g4, magnetic agitation 10 minutes, are configured to 50mL's at 500 rpm
Purple mixed solution；By the MnSO of 2.54g4·H2O is dissolved in the deionized water of 50mL, and magnetic agitation 10 is divided at 500 rpm
Clock, obtains lightpink solution；Under the magnetic agitation of 500rpm, it is molten that above-mentioned lightpink solution is slowly dropped into above-mentioned purple mixing
In liquid, dark brown precipitation is quickly generated, and is continued magnetic agitation 25 minutes, is obtained dark brown suspension；Suspension is placed in
When ageing 20 is small at room temperature, dark brown presoma is obtained after filtration drying；Weigh 2.0g presomas to be placed in autoclave, add
Enter 55mL deionized waters, at 500 rpm magnetic agitation 10 minutes, obtain dark brown suspension；It is carried out at 200 DEG C of hydro-thermals
Manage 12 it is small when, cooling centrifugal drying after obtain black solid；Black solid is moved into porcelain boat, is placed in Muffle furnace and calcines, with 5
DEG C/heating rate of min, 550 DEG C are raised to from room temperature, when insulation 3 is small, is cooled to room temperature obtains final product afterwards
KMn8O16。
Embodiment 4
(20~25 DEG C) at room temperature, the KOH of 8.42g are dissolved in the deionized water of 40mL, magnetic force stirs at 500 rpm
Mix 10 minutes, after solution cooling, add the KMnO of 0.79g4, magnetic agitation 10 minutes, are configured to 50mL's at 500 rpm
Purple mixed solution；By the MnSO of 2.37g4·H2O is dissolved in the deionized water of 50mL, and magnetic agitation 10 is divided at 500 rpm
Clock, obtains lightpink solution；Under the magnetic agitation of 500rpm, it is molten that above-mentioned lightpink solution is slowly dropped into above-mentioned purple mixing
In liquid, dark brown precipitation is quickly generated, and is continued magnetic agitation 30 minutes, is obtained dark brown suspension；Suspension is placed in
When ageing 24 is small at room temperature, dark brown presoma is obtained after filtration drying；Weigh 2.0g presomas to be placed in autoclave, add
Enter 50mL deionized waters, at 500 rpm magnetic agitation 20 minutes, obtain dark brown suspension；It is carried out at 200 DEG C of hydro-thermals
Manage 24 it is small when, cooling centrifugal drying after obtain black solid；Black solid is moved into porcelain boat, is placed in Muffle furnace and calcines, with 5
DEG C/heating rate of min, 500 DEG C are raised to from room temperature, when insulation 2 is small, is cooled to room temperature obtains final product afterwards
KMn8O16。
The products obtained therefrom of embodiment 1 to 4 is used for all kinds of characterizations, gained characterization result is basically identical, below with the institute of embodiment 4
Be illustrated exemplified by product.
As shown in Figure 1, by with KMn8O16Standard card PDF 06-0547 contrast as can be seen that embodiment 4 prepare
KMn8O16Positive electrode and KMn8O16Characteristic diffraction peak coincide very well, free from admixture peak, the main component for showing material is
KMn8O16。
As shown in Fig. 2, KMn made from embodiment 48O16Positive electrode particle is smaller, is nanoscale, is more advantageous to lithium ion
Quick deintercalation, and there is excellent chemical property.
The KMn that will be prepared in embodiment 48O16Positive electrode and conductive agent acetylene black, binding agent Kynoar (PVDF)
In mass ratio 8:1:1 mixing, instills 1-methyl-2-pyrrolidinone (NMP) and is modulated into slurry, be evenly coated with slurry with coating machine
Pole piece is obtained on aluminium foil, after then putting it into when 110 DEG C of dryings 12 are small in vacuum drying chamber, with tablet press machine by pole piece pressure
System uniformly obtains pole piece to be measured.Using lithium piece as to electrode, with the LiPF of 1M6Ethyl carbonate ester (EC) and dimethyl carbonate
(DMC) (volume ratio 1:1) solution is electrolyte, and membrane uses the battery diaphragm of model celgerd 2300, in argon gas
The button cell of CR2025 is assembled into the glove box of atmosphere.(20~25 DEG C) at room temperature, charge-discharge test is carried out to battery,
The voltage range of test is 1.5~4.2V.In 50mA g-1Under current density, its first discharge specific capacity is up to 136.7mAh g-1, initial charge specific capacity is 130.9mAh g-1, as shown in Figure 3.After 50 circulations, its specific discharge capacity still maintains
86.5mAh g-1, and its coulombic efficiency remains at more than 90%, as shown in Figure 4.
Claims (6)
- A kind of 1. KMn8O16The preparation method of positive electrode, it is characterised in that include the following steps：(1) at room temperature, KOH is dissolved in deionized water, KMnO is added after solution cooling4, magnetic agitation is to after being completely dissolved Obtain purple mixed solution；By MnSO4·H2O is added in deionized water, and it is molten that magnetic agitation obtains lightpink to after being completely dissolved Liquid；(2) above-mentioned MnSO is slowly added dropwise into purple mixed solution obtained by step (1)4Lightpink solution, precipitation generation after continue into Row magnetic agitation 20~30 minutes, obtains dark brown suspension；(3) by suspension obtained by step (2) be aged at room temperature 12~24 it is small when, obtain dark brown forerunner after filtration drying Body；(4) deionized water is added into presoma obtained by step (3), magnetic agitation 10~20 minutes, obtains dark brown suspension；(5) suspension obtained by step (4) is placed in autoclave and carries out hydro-thermal process, obtain black precipitate；(6) black precipitate obtained by step (5) is placed in Muffle furnace and carries out calcination processing, that is, obtain final product KMn8O16。
- 2. KMn according to claim 18O16The preparation method of positive electrode, it is characterised in that in step (1), KOH with KMnO4The ratio between the amount of material be 25~35:1.
- 3. KMn according to claim 18O16The preparation method of positive electrode, it is characterised in that in step (2), MnSO4· H2O and KMnO4The ratio between the amount of material be 1.5~3.0:1.
- 4. KMn according to claim 18O16The preparation method of positive electrode, it is characterised in that in step (4), presoma Mass ratio with deionized water is 1:20~30.
- 5. KMn according to claim 18O16The preparation method of positive electrode, it is characterised in that in step (5), at hydro-thermal It is 160~200 DEG C to manage temperature, when hydrothermal conditions are 8~24 small.
- 6. KMn according to claim 18O16The preparation method of positive electrode, it is characterised in that the calcining in step (6) Processing, is specially：With the heating rate of 5~10 DEG C/min, 450~550 DEG C, when insulation 2~4 is small are raised to from room temperature, Zhi Houleng But to room temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109701547A (en) * | 2018-12-26 | 2019-05-03 | 华中科技大学 | A kind of high methyl hydride catalyzed active manganese cerium catalyst preparation method and product |
| CN112794367A (en) * | 2019-11-13 | 2021-05-14 | 中国科学院大连化学物理研究所 | Preparation method of potassium permanganate |
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| CN104129815A (en) * | 2014-07-25 | 2014-11-05 | 武汉理工大学 | Synthesis method and use of monodispersed KMn8O16 nanospheres |
| US20160175806A1 (en) * | 2014-12-17 | 2016-06-23 | University Of Connecticut | Adsorptive desulfurization |
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| US20070027344A1 (en) * | 2005-06-16 | 2007-02-01 | The University Of Connecticut | Method of producing imines |
| CN101927179A (en) * | 2010-07-09 | 2010-12-29 | 北京工业大学 | OMS-2 catalyst used in elimination of benzene series at low temperature and preparation and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109701547A (en) * | 2018-12-26 | 2019-05-03 | 华中科技大学 | A kind of high methyl hydride catalyzed active manganese cerium catalyst preparation method and product |
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