CN110127768A - A kind of CuFe2O4The preparation method of ion battery electrode materials - Google Patents
A kind of CuFe2O4The preparation method of ion battery electrode materials Download PDFInfo
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- CN110127768A CN110127768A CN201910461103.0A CN201910461103A CN110127768A CN 110127768 A CN110127768 A CN 110127768A CN 201910461103 A CN201910461103 A CN 201910461103A CN 110127768 A CN110127768 A CN 110127768A
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- cufe
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or 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
- 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
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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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- C—CHEMISTRY; METALLURGY
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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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- 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
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Abstract
The invention discloses a kind of CuFe2O4The preparation method of ion battery electrode materials, using sol-gal process, including preparing colloidal sol, desiccant gel and last calcining step.Wherein, pore-forming agent is added during preparing colloidal sol, during calcining to xerogel, it is suitable for CuFe as electrode material that Gel Precursor, which is formed,2O4Material, and simultaneously pore-forming agent also resolve into gas evolution during formed pore structure, obtain the material with pore structure, by control pore-forming agent dosage, can regulate and control hole number, density.Simple process and low cost of the invention, CuFe suitable for mass production, and being prepared2O4Large specific surface area, electric property obtains raising by a relatively large margin, has broad application prospects.
Description
Technical field
The present invention relates to a kind of ion battery electrode materials, more particularly, to a kind of CuFe2O4Ion battery electrode materials
Preparation method.
Background technique
In recent years, electronic equipment obtains rapid development, and laptop, mobile phone, even electric vehicle have all entered thousand ten thousand
Family.One critical component of these electronic equipments, i.e. battery, restrict the service performance of equipment.
The battery with high-energy density is studied and prepared, is the key point for improving electronic equipment usability.In recent years
Come, ion battery is because it is with energy density height, and small in size, charging is fast, and the small feature of loop attenuation is increasingly weighed extensively
Depending on.
Ion battery is mainly made of positive electrode, negative electrode material and electrolyte three parts.It is any a part all to from
The performance of sub- battery has great influence.
The CuFe of spinel structure2O4, it is a kind of multifunctional semiconductor material, while being also a kind of common ion battery
Negative electrode material.Preparation method is simple, at low cost, can effectively improve the capacity of ion battery, it is considered to be one kind has wide
The ion battery electrode materials of wealthy application prospect.
Summary of the invention
The purpose of the present invention is to provide a kind of CuFe as ion battery cathode material2O4Preparation method.
The purpose of the present invention is achieved through the following technical solutions:
A kind of CuFe2O4The preparation method of ion battery electrode materials, includes the following steps:
(1) according to molysite: the molar ratio of mantoquita is the ratio of 2-2.2:1, and molysite and mantoquita are add to deionized water,
It stirs evenly, complexing agent is then added and continues to be uniformly mixing to obtain mixture；
(2) mixture is heated in 40-60 DEG C of water-bath and is persistently slowly stirred, while pore-forming agent is added, then to
Lye is added in mixture until forming colloidal sol；
(3) bath temperature is improved to 80-90 DEG C, is simultaneously stopped stirring, colloidal sol gradually becomes gel, and gel drying is obtained
Xerogel；
(4) xerogel is calcined in resistance furnace to get the CuFe with pore structure is arrived2O4Ion battery electrode materials, institute
The temperature of calcining is stated not less than 400 DEG C.
Wherein it is preferred to which the molysite is one of ferric nitrate, iron chloride, ferric sulfate, ironic citrate or a variety of, institute
Stating mantoquita is one of copper nitrate, copper chloride, copper sulphate or a variety of.
Preferably, the complexing agent is citric acid, and additional amount is the 3-5% of mantoquita quality.There is complexing by being added
The citric acid of effect occurs complexing with metal ion and then forms colloidal sol.
Preferably, the pore-forming agent is melamine or hexa, and additional amount is the 1- of mantoquita quality
10%.By selecting pore-forming agent, gas is generated during subsequent calcination, gas evolution is to form pore structure.Control
The dosage of pore-forming agent can control the hole density of product.
Preferably, the lye is ammonium hydroxide.
Preferably, the drying in step (3) is freeze-drying.
Preferably, the calcination temperature is 400-700 DEG C, in this temperature range, guarantees that pore-forming agent can decompose
Gas is formed, while forming the CuFe with spinel structure after xerogel calcining2O4Ion battery electrode materials.
Technical solution of the present invention synthesizes CuFe using sol-gal process2O4Material, first by molysite, mantoquita according to metering
Than being configured to solution, lye and complexing agent is then added, forms colloidal sol under water bath condition, and then form gel.It is molten preparing
It is added during glue and is easy distillation or the substance decomposed as pore-forming agent, then xerogel calcined, before gel
Driving body and being formed is suitable for CuFe as electrode material2O4Material, and simultaneously at calcination temperatures, pore-forming agent also decomposes distillation, gas
Hole is formed during body evolution, obtains the material with pore structure.
The present invention can comparatively fast form colloidal sol, gel by the additional amount of control complexing agent during water-bath.Pass through control
The dosage of drilling forming agent can regulate and control number, the density of hole, obtain the material with required hole density structure.
The present invention uses sol-gal process, and simple process and low cost is suitable for mass production.On the other hand, of the invention
Product be and then to increase the CuFe as electrode material with pore structure2O4Specific surface area, therefore electric property obtains
Raising by a relatively large margin, therefore have broad application prospects.
Detailed description of the invention
Fig. 1 is the CuFe that embodiment 1 obtains2O4XRD spectrum.
Specific embodiment
The following are a specific embodiment of the invention, the present invention to be explained and illustrated.
Embodiment 1
A kind of CuFe2O4The preparation method of ion battery electrode materials, includes the following steps:
(1) according to ferric nitrate: the molar ratio of copper chloride is the ratio of 2.2:1, and ferric nitrate, copper chloride are added to deionization
It in water, stirs evenly, complexing agent citric acid is then added and continues to be uniformly mixing to obtain mixture, wherein the additional amount of citric acid
It is the 3% of chlorination copper mass；
(2) mixture is heated in 60 DEG C of water-baths and is persistently slowly stirred, while pore-forming agent hexa-methylene four is added
Amine, additional amount are the 10% of chlorination copper mass, and ammonium hydroxide is then added into mixture until forming colloidal sol；
(3) bath temperature is improved to 90 DEG C, is simultaneously stopped stirring, colloidal sol gradually becomes gel, and gel refrigeration drying is obtained
To xerogel；
(4) xerogel is calcined in resistance furnace to get the CuFe with pore structure is arrived2O4Ion battery electrode materials, institute
The temperature for stating calcining is 600 DEG C.
Fig. 1 is the CuFe being prepared2O4The XRD spectrum of ion battery electrode materials.
The CuFe that will be obtained2O4Ion battery electrode materials carry out circulation experiment under the current density of 0.3A/g, reversible
Capacity is within the scope of 220-300mAh/g.
Embodiment 2
A kind of CuFe2O4The preparation method of ion battery electrode materials, includes the following steps:
(1) according to (iron chloride+ironic citrate): the molar ratio of copper sulphate is the ratio of 2:1, and molysite and mantoquita are added to
It in deionized water, stirs evenly, is then added and complexing agent citric acid and continues to be uniformly mixing to obtain mixture, wherein citric acid
Additional amount is the 5% of chlorination copper mass；
(2) mixture is heated in 40 DEG C of water-baths and is persistently slowly stirred, while pore-forming agent melamine is added, added
Enter 1% that amount is chlorination copper mass, ammonium hydroxide is then added into mixture until forming colloidal sol；
(3) bath temperature is improved to 80 DEG C, is simultaneously stopped stirring, colloidal sol gradually becomes gel, and gel is spontaneously dried
To xerogel；
(4) xerogel is calcined in resistance furnace to get the CuFe with pore structure is arrived2O4Ion battery electrode materials, institute
The temperature for stating calcining is 400 DEG C.
Embodiment 3
A kind of CuFe2O4The preparation method of ion battery electrode materials, includes the following steps:
(1) according to (ferric nitrate+ferric sulfate): the molar ratio of (copper nitrate+copper sulphate) is the ratio of 2:1, by molysite and copper
Salt is add to deionized water, and is stirred evenly, and complexing agent citric acid is then added and continues to be uniformly mixing to obtain mixture, wherein
The additional amount of citric acid is the 4% of chlorination copper mass；
(2) mixture is heated in 50 DEG C of water-baths and is persistently slowly stirred, while pore-forming agent melamine is added, added
Enter 6% that amount is chlorination copper mass, ammonium hydroxide is then added into mixture until forming colloidal sol；
(3) bath temperature is improved to 85 DEG C, is simultaneously stopped stirring, colloidal sol gradually becomes gel, and gel is spontaneously dried
To xerogel；
(4) xerogel is calcined in resistance furnace to get the CuFe with pore structure is arrived2O4Ion battery electrode materials, institute
The temperature for stating calcining is 700 DEG C.
The CuFe that embodiment 1-3 is obtained2O4It is real that ion battery electrode materials carry out circulation under the current density of 0.3A/g
It tests, reversible capacity (50 circulations) within the scope of 220-300mAh/g.
Claims (7)
1. a kind of CuFe2O4The preparation method of ion battery electrode materials, which is characterized in that the preparation method includes following step
It is rapid:
(1) according to molysite: the molar ratio of mantoquita is the ratio of 2-2.2:1, and molysite and mantoquita are add to deionized water, and is stirred
Uniformly, complexing agent is then added and continues to be uniformly mixing to obtain mixture；
(2) mixture is heated in 40-60 DEG C of water-bath and is persistently slowly stirred, while pore-forming agent is added, then to mixing
Lye is added in object until forming colloidal sol；
(3) bath temperature is improved to 80-90 DEG C, is simultaneously stopped stirring, and colloidal sol gradually becomes gel, gel drying is obtained dry solidifying
Glue；
(4) xerogel is calcined in resistance furnace to get the CuFe with pore structure is arrived2O4Ion battery electrode materials, it is described to forge
The temperature of burning is not less than 400 DEG C.
2. a kind of CuFe according to claim 12O4The preparation method of ion battery electrode materials, which is characterized in that described
Molysite is one of ferric nitrate, iron chloride, ferric sulfate, ironic citrate or a variety of, and the mantoquita is copper nitrate, copper chloride, sulphur
One of sour copper is a variety of.
3. a kind of CuFe according to claim 12O4The preparation method of ion battery electrode materials, which is characterized in that described
Complexing agent is citric acid, and additional amount is the 3-5% of mantoquita quality.
4. a kind of CuFe according to claim 12O4The preparation method of ion battery electrode materials, which is characterized in that described
Pore-forming agent is melamine or hexa, and additional amount is the 1-10% of mantoquita quality.
5. a kind of CuFe according to claim 12O4The preparation method of ion battery electrode materials, which is characterized in that described
Lye is ammonium hydroxide.
6. a kind of CuFe according to claim 12O4The preparation method of ion battery electrode materials, which is characterized in that step
(3) drying in is freeze-drying.
7. a kind of CuFe according to claim 42O4The preparation method of ion battery electrode materials, which is characterized in that described
Calcination temperature be 400-700 DEG C.
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Citations (8)
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|---|---|---|---|---|
| CN102154817A (en) * | 2011-02-15 | 2011-08-17 | 江苏大学 | Silver-loaded copper ferrite magnetic nanometer composite fiber and preparation method and application thereof |
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| CN105600828A (en) * | 2016-01-04 | 2016-05-25 | 南京林业大学 | Preparation method of porous nano CuFe2O4 |
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2019
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Application publication date: 20190816 |