CN110078096A - A kind of Prussian blue material and preparation method thereof - Google Patents
A kind of Prussian blue material and preparation method thereof Download PDFInfo
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- CN110078096A CN110078096A CN201910397256.3A CN201910397256A CN110078096A CN 110078096 A CN110078096 A CN 110078096A CN 201910397256 A CN201910397256 A CN 201910397256A CN 110078096 A CN110078096 A CN 110078096A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/08—Simple or complex cyanides of metals
- C01C3/12—Simple or complex iron cyanides
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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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- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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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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- 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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- 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 Prussian blue material and preparation method thereof, methods specifically: sodium ferrocyanide and deionized water are mixed to get solution I；Manganous salt and deionized water are mixed to get solution II；Sodium salt and deionized water are mixed to get solution III；Then solution I and II solution are added in solution III simultaneously, Prussian blue sill is obtained after coprecipitation reaction.Prussian blue sill disclosed by the invention is applied in sodium-ion battery anode, is remarkably improved the capacity and cyclical stability of sodium-ion battery.
Description
Technical field
The present invention relates to the technical fields of novel energy storage cell, and in particular to a kind of Prussian blue material and its preparation side
Method.
Background technique
With society, expanding economy, energy consumption is increasingly aggravated, and traditional fossil energy is constantly reduced, and the mankind are to tradition
While the consumption of fossil energy, cause that environmental pollution is serious, it is cleaning, renewable, cheap novel under this overall situation
The energy is as national governments' exploitation to picture, and the specific gravity of wind energy, solar energy and ocean energy in energy consumption is constantly increasing at present
Add, but these renewable energy are affected by weather and period, there is apparent unstable, discontinuous and uncontrollable spy
Property, need to develop and build matched electric energy storage (energy storage) device i.e. battery to guarantee the continuity and stabilization of power generation, power supply
Property, and large-scale battery energy storage is used for " peak load shifting " of electric power in power industry, it will significantly improve the confession of electric power
Contradiction is needed, the utilization rate of generating equipment is improved.Requirement of the large-scale energy-storage battery to electrode material has certain energy density, longevity
Outside life, safety have higher requirements, to cost, higher requirements are also raised.Lead-acid battery is although at low cost, but its raw material master
To be lead and sulfuric acid, there are environment easy to pollute, service life enable it is short, there are memory effect, battery weight greatly there is also transport at
This high problem；Although lithium ion battery has many advantages, such as big energy density, long service life and memory-less effect,
Lithium raw material reserves are limited, and lithium ion battery is at high cost, and security performance is bad, in the long run, are not able to satisfy extensive energy storage
It is required that.Compared with lithium ion battery, sodium-ion battery is resourceful, has a safety feature, and has at low cost, environmentally friendly etc.
Advantage is very suitable to extensive stored energy application.
Certain prussian blue materials due in structure contain biggish vacancy and have open architecture, be conducive to volume compared with
The insertion and abjection of big sodium ion, therefore capacity is higher, especially the material charging/discharging voltage containing manganese is higher, is adapted as
Sodium-ion battery positive material.But this kind of compound chemistry and electrochemical stability are undesirable, and therefore, it is necessary to optimize preparation process
Route improves its chemical property.
Summary of the invention
The invention discloses a kind of preparation method of Prussian blue material, this method is made up of optimizing raw material, and gained produces
Object has chemistry and electrochemical stability well, is applied in sodium-ion battery electrode, is remarkably improved sodium ion electricity
The chemical property in pond, especially capacity and cyclical stability.Meanwhile the preparation method is also beneficial to reduce synthesis cost, subtracts
The generation of by-product and the impact to environment less.
The technical solution adopted in the present invention is as follows: a kind of preparation method of Prussian blue material, comprising the following steps:
1) sodium ferrocyanide and deionized water are mixed to get solution I；
2) soluble manganous salt and deionized water are mixed to get solution II；
3) sodium salt and surfactant and deionized water are mixed to get solution III；
4) solution I and II are instilled in solution III simultaneously, is obtained through coprecipitation reaction and post-processing described Prussian blue
Material.
The present invention also has following technical characteristic:
In step 1),
Preferably, the concentration of sodium ferrocyanide is 0.03~0.3mol/L in the solution I, raw material is removed selected from ferrous cyanogen
Change sodium, is further selected from the hydrate of sodium ferrocyanide.With this condition, product crystallinity is preferable, and the content of sodium is higher in product.
In step 2),
Preferably, the concentration of manganese salt is 0.1~1mol/L in the solution II；The soluble manganous salt is
Manganese chloride, manganese sulfate, manganese nitrate, manganese acetate or the above manganous salt hydrate；Ferrous cyanogen in manganese salt and solution I in solution II
The molar ratio for changing sodium is 1.0~1.2:1；With this condition, product crystallinity is preferable, and defect is less in crystal.
In step 3),
Preferably, the concentration of sodium salt is 0.1~1mol/L in the solution III；The sodium salt is sodium chloride, fluorine
Change sodium, sodium bromide, sodium nitrate or sodium acetate, with this condition, product crystallinity is preferable, and defect is less in crystal.
In step 4), when dropwise addition, the volume ratio of solution I and solution II is 1~5:1, the volume ratio of solution I and solution III
For 1:1~5；Preferably, the temperature of the coprecipitation reaction is 50~90 DEG C；With this condition, product crystallinity is preferable, brilliant
Defect is less in body, and product has micro-nano structure, while having high activity and chemical/electrochemical stability.
Product after coprecipitation reaction also needs post-treated, including cooling, washing, separation, drying process.
The invention also discloses the Prussian blue materials prepared according to the above method, which is characterized in that product has
NaxMnFe(CN)6General formula, in formula, NaxMnFe(CN)6For the Prussian blue material, there are monocline phase structure, 1≤x≤2；
The Prussian blue material has micro-nano structure, and primary particle size is 400 nanometers~900 sodium rices, and primary particle is mutually viscous
Knot, 4 microns~10 microns of the second particle size of formation, nanostructure is conducive to the raising of lytic activity, so that capacity is improved,
Micrometer structure is conducive to the raising of product chemistry/electrochemical stability again, to improve cyclical stability.
Compared with prior art, the present invention has the advantage that products therefrom of the present invention has chemistry well and electrification
Stability is learned, is applied in sodium-ion battery electrode, is remarkably improved the chemical property of sodium-ion battery, especially holds
Amount and cyclical stability.Meanwhile the preparation method is also beneficial to reduce synthesis cost, reduces the generation of by-product and to environment
Impact.The present invention passes through while introducing sodium salt, improves the temperature of coprecipitation reaction, improves product sodium content, improves product lattice
Integrality makes product have micro-nano structure.Preparation method of the invention, with simple process, at low cost, the period is short, low energy consumption
And the advantages that suitable industrialized production.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) map of Prussian blue material prepared by embodiment 1；
Fig. 2 is scanning electron microscope (SEM) map of Prussian blue material prepared by embodiment 1；
Fig. 3 is the charging and discharging curve of the sodium-ion battery assembled with Prussian blue material prepared by embodiment 1.
Specific embodiment
Embodiment 1
Sodium ferrocyanide is dissolved in deionized water, being uniformly mixing to obtain the concentration in terms of ferrous cyanide ion is
The solution I of 0.03mol/L；Protochloride manganese is dissolved in deionized water, is obtained with Mn2+The solution that concentration is 0.18mol/L is counted,
Middle sodium ferrocyanide liquor capacity is 5 times of protochloride manganese solution volume, through being sufficiently stirred to obtain solution II；Sodium chloride is dissolved in
In deionized water, the solution III that concentration is 0.3mol/L is obtained, wherein solution III volume is identical with solution I volume；Then exist
Be stirred continuously down, solution I and solution II be added in solution III simultaneously, through coprecipitation reaction at 90 DEG C, then through cooling,
Prussia material Na is obtained after washing, separation, dryingxMnFe(CN)6。
Fig. 1 is the XRD of Prussia's material of this implementation preparation, is analyzed as monoclinic phase.Fig. 2 is manufactured in the present embodiment general
The SEM photograph of Shandong scholar's blue material, primary particle are mutually bonded having a size of 400 nanometers~900 sodium rices, primary particle, and the two of formation
4 microns~10 microns of secondary particle size.Using Prussian blue material manufactured in the present embodiment as anode, using metallic sodium as cathode,
Glass fibre (trade mark Whatman GF/D) is diaphragm, NaPF6Ethylene carbonate (EC)/diethyl carbonate (DEC) solution be
Electrolyte assembles battery in the glove box full of argon gas, carries out charge-discharge test, current density 15mA/g, and voltage range 2~
4V, charging and discharging curve is as shown in figure 3, the initial capacity of product recycles, capacity retention ratio up to 142mAh/g by 100 times
89%.
Comparative example 1
The preparation of material is a difference in that in solution III with embodiment 1 that sodium chloride is not added, although obtaining monocline knot
The Na of structurexMnFe(CN)6Material, but electro-chemical test shows that product initial capacity is 121mAh/g, recycles, produces by 100 times
The capacity retention ratio of object is 73%.
Comparative example 2
The preparation of material is a difference in that the concentration of sodium ferrocyanide is 0.02mol/L, although obtaining list with embodiment 1
The Na of biassed fabricxMnFe(CN)6Material, but primary particle size is lower than 300 nanometers, and does not form micro-nano structure, electrochemistry
Test shows that product initial capacity is 141mAh/g, recycles by 100 times, and the capacity retention ratio of product is 70%.
Comparative example 3
The preparation of material is a difference in that coprecipitation reaction carries out at 40 DEG C, does not obtain complete list with embodiment 1
The Na of biassed fabricxMnFe(CN)6Material, and primary particle size is lower than 300 nanometers, and does not form micro-nano structure, electrochemistry
Test shows that product initial capacity is 110mAh/g, recycles by 100 times, and the capacity retention ratio of product is 67%.
Comparative example 4
The preparation of material is a difference in that the concentration of protochloride manganese is 0.2mol/L, although obtaining monocline knot with embodiment 1
The Na of structurexMnFe(CN)6Material, but electro-chemical test shows that product initial capacity is 124mAh/g, recycles, produces by 100 times
The capacity retention ratio of object is 77%.
Embodiment 2
Sodium ferrocyanide is dissolved in deionized water, being uniformly mixing to obtain the concentration in terms of ferrous cyanide ion is 0.1
The solution I of mol/L；Manganese sulfate is dissolved in deionized water, is obtained with Mn2+Counting concentration is the molten of 0.33mol/L
Liquid, wherein sodium ferrocyanide solution volume is 3 times of manganese sulfate liquor capacity, through being sufficiently stirred to obtain solution II；It will fluorination
Sodium is dissolved in deionized water, and obtaining concentration is 0.3mol/L solution III, and wherein solution III volume is 3 times of solution I volume；So
Afterwards under constant stirring, solution I and solution II are added in solution III simultaneously, through coprecipitation reaction at 70 DEG C, then through cold
But, wash, separate, obtain the Prussia material Na of the monoclinic phase with micro-nano structure after dryingxMnFe(CN)6.It is surveyed through electrochemistry
Examination, the initial capacity of product recycle, capacity retention ratio 85% up to 141mAh/g by 100 times.
Embodiment 3
Ten hydration sodium ferrocyanides are dissolved in deionized water, being uniformly mixing to obtain the concentration in terms of ferrous cyanide ion is
The solution I of 0.3mol/L；Mn nitrate is dissolved in deionized water, is obtained with Mn2+The solution that concentration is 0.3mol/L is counted, wherein
Ten hydration sodium ferrocyanide solution volumes are identical with Mn nitrate liquor capacity, through being sufficiently stirred to obtain solution II；By sodium acetate
It is dissolved in deionized water, obtaining concentration is 0.6 solution III, and wherein solution III volume is 5 times of solution I volume；Then not
Under disconnected stirring, solution I and solution II are added in solution III simultaneously, through coprecipitation reaction at 50 DEG C, then through cooling, wash
Wash, separate, dry after obtain the monoclinic phase Prussia material Na with micro-nano structurexMnFe(CN)6.Through electro-chemical test, product
Initial capacity up to 135mAh/g, recycled by 100 times, capacity retention ratio 82%.
Claims (8)
1. a kind of preparation method of Prussian blue material, which comprises the following steps:
1) sodium ferrocyanide and deionized water are mixed to get solution I；
2) soluble manganous salt and deionized water are mixed to get solution II；
3) sodium salt and deionized water are mixed to get solution III；
4) solution I and II are instilled in solution III simultaneously, obtains Prussian blue material through coprecipitation reaction and post-processing.
2. the preparation method of Prussian blue material according to claim 1, which is characterized in that ferrous in the solution I
The concentration of Cymag is 0.03~0.3mol/L, in solution II in manganese salt and solution I the molar ratio of sodium ferrocyanide be 1.0~
1.2:1mol/L；Sodium salt concentration is 0.1~1mol/L in solution III.
3. the preparation method of Prussian blue material according to claim 1 or 2, which is characterized in that step 4), when dropwise addition,
The volume ratio of solution I and solution II is 1~5:1, and the volume ratio of solution I and solution III is 1:1~5.
4. the preparation method of Prussian blue material according to claim 1 or 2, which is characterized in that described in step 2)
Soluble manganous salt is the hydrate of manganese chloride, manganese sulfate, manganese nitrate, manganese acetate or the above manganous salt.
5. the preparation method of Prussian blue material according to claim 1 or 2, which is characterized in that described in step 3)
Sodium salt is sodium chloride, sodium fluoride, sodium bromide, sodium nitrate or sodium acetate.
6. the preparation method of Prussian blue material according to claim 1 or 2, which is characterized in that described total in step 4)
The temperature of precipitation reaction is 50~90 °.
7. a kind of Prussian blue material of preparation method preparation according to claim 1 or 2, which is characterized in that product tool
There is NaxMnFe(CN)6General formula has monocline phase structure, in formula, 1≤x≤2.
8. a kind of Prussian blue material according to claim 7, which is characterized in that the Prussian blue material has micro-
Micro-nano structure, primary particle diameter are 400 nanometers~900 sodium rices, and primary particle mutually bonds, the second particle diameter of formation not 4
Micron~10 microns.
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Cited By (7)
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| CN110451525A (en) * | 2019-08-07 | 2019-11-15 | 清华大学 | A method of quickly preparing the Prussian blue similar object of monoclinic structure |
| CN111600011A (en) * | 2020-04-24 | 2020-08-28 | 国网浙江省电力有限公司电力科学研究院 | Doped prussian blue material and preparation method and application thereof |
| CN112174167A (en) * | 2020-08-13 | 2021-01-05 | 国网浙江省电力有限公司电力科学研究院 | Prussian blue material with core-shell structure and preparation method and application thereof |
| CN112209409A (en) * | 2020-09-28 | 2021-01-12 | 浙江凯恩电池有限公司 | Method for rapidly preparing Prussian white serving as positive electrode material of sodium-ion battery |
| CN112259730A (en) * | 2020-12-08 | 2021-01-22 | 江苏时代新能源科技有限公司 | Prussian blue transition metal cyanide, preparation method thereof, and related positive electrode plate, secondary battery, battery pack and device |
| CN114212803A (en) * | 2021-10-28 | 2022-03-22 | 广东邦普循环科技有限公司 | Preparation method of fluorine-doped Prussian blue type sodium ion battery positive electrode material |
| CN115784258A (en) * | 2022-11-24 | 2023-03-14 | 赣州立探新能源科技有限公司 | Preparation method of manganese-based Prussian blue positive electrode material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451525A (en) * | 2019-08-07 | 2019-11-15 | 清华大学 | A method of quickly preparing the Prussian blue similar object of monoclinic structure |
| CN110451525B (en) * | 2019-08-07 | 2021-05-11 | 清华大学 | Method for rapidly preparing Prussian blue analogue with monoclinic crystal structure |
| CN111600011A (en) * | 2020-04-24 | 2020-08-28 | 国网浙江省电力有限公司电力科学研究院 | Doped prussian blue material and preparation method and application thereof |
| CN112174167A (en) * | 2020-08-13 | 2021-01-05 | 国网浙江省电力有限公司电力科学研究院 | Prussian blue material with core-shell structure and preparation method and application thereof |
| CN112209409A (en) * | 2020-09-28 | 2021-01-12 | 浙江凯恩电池有限公司 | Method for rapidly preparing Prussian white serving as positive electrode material of sodium-ion battery |
| CN112259730A (en) * | 2020-12-08 | 2021-01-22 | 江苏时代新能源科技有限公司 | Prussian blue transition metal cyanide, preparation method thereof, and related positive electrode plate, secondary battery, battery pack and device |
| WO2022121570A1 (en) * | 2020-12-08 | 2022-06-16 | 宁德时代新能源科技股份有限公司 | Prussian blue transition metal cyanide, preparation method therefor, and positive electrode pole piece, secondary battery, battery module, battery pack, and apparatus related to prussian blue transition metal cyanide |
| EP4135073A4 (en) * | 2020-12-08 | 2023-12-27 | Contemporary Amperex Technology Co., Limited | Prussian blue transition metal cyanide, preparation method therefor, and positive electrode pole piece, secondary battery, battery module, battery pack, and apparatus related to prussian blue transition metal cyanide |
| CN114212803A (en) * | 2021-10-28 | 2022-03-22 | 广东邦普循环科技有限公司 | Preparation method of fluorine-doped Prussian blue type sodium ion battery positive electrode material |
| CN114212803B (en) * | 2021-10-28 | 2023-09-12 | 广东邦普循环科技有限公司 | Preparation method of fluorine-doped Prussian blue sodium ion battery positive electrode material |
| CN115784258A (en) * | 2022-11-24 | 2023-03-14 | 赣州立探新能源科技有限公司 | Preparation method of manganese-based Prussian blue positive electrode material |
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