CN108336304A - Hydro-thermal method prepares stainless (steel) wire load FeCO3The method of negative plate - Google Patents
Hydro-thermal method prepares stainless (steel) wire load FeCO3The method of negative plate Download PDFInfo
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- CN108336304A CN108336304A CN201711444203.XA CN201711444203A CN108336304A CN 108336304 A CN108336304 A CN 108336304A CN 201711444203 A CN201711444203 A CN 201711444203A CN 108336304 A CN108336304 A CN 108336304A
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- steel
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- wire
- feco
- negative plate
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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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- 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 present invention relates to a kind of hydro-thermal methods to prepare stainless (steel) wire load FeCO3The method of negative plate, includes the following steps：A, hydrothermal reaction kettle is put into after taking stainless (steel) wire cleaning；B, hexa is added while stirring in deionized water, adjusts pH value of solution≤7, then adds polyethylene glycol, FeCl is added after mixing2·4H2O obtains reaction precursor liquid after mixing；C, reaction precursor liquid is poured into the hydrothermal reaction kettle of step a, until submerging stainless (steel) wire matrix, capping kettle, reaction kettle is placed in heater and carries out hydro-thermal reaction, after reaction, opens reaction kettle, stainless (steel) wire is taken out, is dried after ultrasonic cleaning, stainless (steel) wire load FeCO is obtained3Negative plate.The present invention uses stainless steel steel mesh for matrix, with FeCl2·4H2O is source of iron, polyethylene glycol is template, hexa is that precipitating reagent prepares stainless (steel) wire growth FeCO3Nanometer plate electrode eliminates modulation slurry and applies blade technolgy, and technological process is simple, and properties of product are excellent.
Description
Technical field
The present invention relates to electrode material technical fields, and in particular to hydro-thermal method prepares stainless (steel) wire load FeCO3Negative plate
Method.
Background technology
Lithium ion battery negative material is based on graphitized carbon material at present, but carbon material is raw in discharge process for the first time
At SEI films, irreversible capacity loss can be caused, also result in variation and the poor electric contact of carbon electrode internal structure sometimes；
It may cause battery failure because of the decomposition of protective layer or cause safety issue when high temperature；The unit bodies of graphite cathode simultaneously
Product capacity is relatively low, it is difficult to meet the necks such as electric vehicle, wind and solar energy energy storage, intelligent grid energy storage and conversion
The requirement of domain high energy density cells." transformant " negative material ferrous carbonate as novel lithium ion battery negative material,
Compared with the graphite cathode being commercialized at present, with higher theoretical capacity, wide applicability, good stability etc.
Advantage.Meanwhile when lithium ion is embedded into ferrous carbonate, obtained Li is reacted2CO3It is embedded into traditional metal oxygen than it
The Li of reaction gained in compound20 stablizes so that ferrous carbonate can keep the lasting charge and discharge of high current density.Ferrous carbonate
When preparing battery cathode sheet as negative material, need by sizing mixing, being coated with and the techniques such as roll-in, it is relatively complicated.Therefore, such as
What prepares large specific surface area, the more and orderly mesoporous ferrous carbonate negative material in mesoporous channel, and how to simplify electrode slice
Preparation process is a problem to be solved.
Invention content
The purpose of the present invention is deficiencies to solve above-mentioned technical problem, provide hydro-thermal method and prepare stainless (steel) wire load
FeCO3The method of negative plate.
The deficiency of the present invention to solve above-mentioned technical problem, used technical solution are：Hydro-thermal method prepares stainless (steel) wire
Load FeCO3The method of negative plate, includes the following steps：
A, it takes stainless (steel) wire first to boil corrosion treatment with dilute acid soln, is then cleaned by ultrasonic and is dried with deionized water, obtain table
The stainless (steel) wire matrix of face cleaning, is put into hydrothermal reaction kettle, spare；
B, hexa is added while stirring in deionized water, adjusts pH value of solution≤7, then adds polyethylene glycol, mixes
FeCl is added after closing uniformly2·4H2O obtains reaction precursor liquid after mixing；
C, reaction precursor liquid is poured into the hydrothermal reaction kettle of step a, until submerging stainless (steel) wire matrix, capping kettle will
Reaction kettle is placed in heater, and controlling reaction temperature is 150~180 DEG C, reacts 12~18h, after reaction, opens reaction
Kettle takes out stainless (steel) wire, is put into 5~10s of ultrasonic cleaning in deionization, dries, obtains stainless at a temperature of 60~70 DEG C
Steel mesh loads FeCO3Negative plate.
Stainless (steel) wire, which is prepared, as hydro-thermal method of the present invention loads FeCO3The method of negative plate advanced optimizes：In step b
With the pH value of HCl tune solution.
Stainless (steel) wire, which is prepared, as hydro-thermal method of the present invention loads FeCO3The method of negative plate advanced optimizes：It is described poly-
The degree of polymerization of ethylene glycol is 600-20000, and polyethylene glycol addition is 1/5~1/4 of deionized water weight in step 1.
Stainless (steel) wire, which is prepared, as hydro-thermal method of the present invention loads FeCO3The method of negative plate advanced optimizes：It is described
FeCl2·4H2The addition of O is the 1/100~1/50 of deionized water weight.
Advantageous effect
One, the present invention uses stainless steel steel mesh for matrix, with FeCl2·4H2O is source of iron, polyethylene glycol is template, hexa-methylene
Tetramine is that precipitating reagent prepares stainless (steel) wire growth FeCO3Nanometer plate electrode, electrode high mechanical strength obtained, and due to being free of
Binder so that electric conductivity is very good, and eliminates modulation slurry and apply blade technolgy, and technological process is simple, and properties of product are excellent
It is good.
Two, the present invention prepares stainless (steel) wire load FeCO under hydrothermal conditions3Negative plate, in hydrothermal reaction process, six times
Tetramine, which decomposes, generates formaldehyde, and formaldehyde, which continues to decompose, generates CO3 2-, in the presence of polyethylene glycol, CO3 2-With FeCl2·4H2O exists
Stainless (steel) wire is not upper to generate mesoporous FeCO3, FeCO3Large specific surface area, mesoporous channel is more and orderly, can be used as high-power power
The negative material of battery.
Description of the drawings
Fig. 1 is that stainless (steel) wire load FeCO is made in the embodiment of the present invention 13The XRD spectra of negative plate.
Fig. 2 is that stainless (steel) wire load FeCO is made in the embodiment of the present invention 13The SEM photograph of negative plate.
Specific implementation mode
Further technical scheme of the present invention is illustrated below in conjunction with specific implementation mode.
Embodiment 1
Hydro-thermal method prepares stainless (steel) wire load FeCO3The method of negative plate, includes the following steps：
A, it takes stainless (steel) wire first to boil corrosion treatment with dilute acid soln, is then cleaned by ultrasonic and is dried with deionized water, obtain table
The stainless (steel) wire matrix of face cleaning, is put into hydrothermal reaction kettle, spare；
B, hexa is added while stirring in deionized water, calls HCl solution pH≤7, then adds poly- second two
FeCl is added in alcohol after mixing2·4H2O obtains reaction precursor liquid after mixing；The degree of polymerization of polyethylene glycol is 600, is gathered
Ethylene glycol addition is the 1/4 of deionized water weight；FeCl2·4H2The addition of O is 1/ of deionized water weight in step 1
100；
C, reaction precursor liquid is poured into the hydrothermal reaction kettle of step a, until submerging stainless (steel) wire matrix, capping kettle will
Reaction kettle is placed in heater, and controlling reaction temperature is 160 DEG C, reacts 16h, after reaction, reaction kettle is opened, by stainless steel
Net takes out, and is put into ultrasonic cleaning 8s in deionization, is dried at a temperature of 65 DEG C, obtains stainless (steel) wire load FeCO3Negative plate.
Embodiment 2：
Hydro-thermal method prepares stainless (steel) wire load FeCO3The method of negative plate, includes the following steps：
A, it takes stainless (steel) wire first to boil corrosion treatment with dilute acid soln, is then cleaned by ultrasonic and is dried with deionized water, obtain table
The stainless (steel) wire matrix of face cleaning, is put into hydrothermal reaction kettle, spare；
B, hexa is added while stirring in deionized water, calls HCl solution pH≤7, then adds poly- second two
FeCl is added in alcohol after mixing2·4H2O obtains reaction precursor liquid after mixing；The degree of polymerization of polyethylene glycol is 1200,
Polyethylene glycol addition is the 1/4 of deionized water weight；FeCl2·4H2The addition of O is deionized water weight in step 1
1/90；
C, reaction precursor liquid is poured into the hydrothermal reaction kettle of step a, until submerging stainless (steel) wire matrix, capping kettle will
Reaction kettle is placed in heater, and controlling reaction temperature is 150 DEG C, reacts 18h, after reaction, reaction kettle is opened, by stainless steel
Net takes out, and is put into ultrasonic cleaning 5s in deionization, is dried at a temperature of 70 DEG C, obtains stainless (steel) wire load FeCO3Negative plate.
Embodiment 3：
Hydro-thermal method prepares stainless (steel) wire load FeCO3The method of negative plate, includes the following steps：
A, it takes stainless (steel) wire first to boil corrosion treatment with dilute acid soln, is then cleaned by ultrasonic and is dried with deionized water, obtain table
The stainless (steel) wire matrix of face cleaning, is put into hydrothermal reaction kettle, spare；
B, hexa is added while stirring in deionized water, calls HCl solution pH≤7, then adds poly- second two
FeCl is added in alcohol after mixing2·4H2O obtains reaction precursor liquid after mixing；The degree of polymerization of polyethylene glycol is 5000,
Polyethylene glycol addition is the 1/5 of deionized water weight；FeCl2·4H2The addition of O is deionized water weight in step 1
1/80；
C, reaction precursor liquid is poured into the hydrothermal reaction kettle of step a, until submerging stainless (steel) wire matrix, capping kettle will
Reaction kettle is placed in heater, and controlling reaction temperature is 180 DEG C, reacts 12h, after reaction, reaction kettle is opened, by stainless steel
Net takes out, and is put into ultrasonic cleaning 10s in deionization, is dried at a temperature of 60 DEG C, obtains stainless (steel) wire load FeCO3Cathode
Piece.
Embodiment 4：
Hydro-thermal method prepares stainless (steel) wire load FeCO3The method of negative plate, includes the following steps：
A, it takes stainless (steel) wire first to boil corrosion treatment with dilute acid soln, is then cleaned by ultrasonic and is dried with deionized water, obtain table
The stainless (steel) wire matrix of face cleaning, is put into hydrothermal reaction kettle, spare；
B, hexa is added while stirring in deionized water, calls HCl solution pH≤7, then adds poly- second two
FeCl is added in alcohol after mixing2·4H2O obtains reaction precursor liquid after mixing；The degree of polymerization of polyethylene glycol is 15000,
Polyethylene glycol addition is the 1/4 of deionized water weight；FeCl2·4H2The addition of O is deionized water weight in step 1
1/60；
C, reaction precursor liquid is poured into the hydrothermal reaction kettle of step a, until submerging stainless (steel) wire matrix, capping kettle will
Reaction kettle is placed in heater, and controlling reaction temperature is 170 DEG C, reacts 14h, after reaction, reaction kettle is opened, by stainless steel
Net takes out, and is put into ultrasonic cleaning 6s in deionization, is dried at a temperature of 66 DEG C, obtains stainless (steel) wire load FeCO3Negative plate.
Embodiment 5：
Hydro-thermal method prepares stainless (steel) wire load FeCO3The method of negative plate, includes the following steps：
A, it takes stainless (steel) wire first to boil corrosion treatment with dilute acid soln, is then cleaned by ultrasonic and is dried with deionized water, obtain table
The stainless (steel) wire matrix of face cleaning, is put into hydrothermal reaction kettle, spare；
B, hexa is added while stirring in deionized water, calls HCl solution pH≤7, then adds poly- second two
FeCl is added in alcohol after mixing2·4H2O obtains reaction precursor liquid after mixing；The degree of polymerization of polyethylene glycol is 20000,
Polyethylene glycol addition is the 1/4 of deionized water weight；FeCl2·4H2The addition of O is deionized water weight in step 1
1/50；
C, reaction precursor liquid is poured into the hydrothermal reaction kettle of step a, until submerging stainless (steel) wire matrix, capping kettle will
Reaction kettle is placed in heater, and controlling reaction temperature is 150 DEG C, reacts 16h, after reaction, reaction kettle is opened, by stainless steel
Net takes out, and is put into ultrasonic cleaning 9s in deionization, is dried at a temperature of 68 DEG C, obtains stainless (steel) wire load FeCO3Negative plate.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make out a little change or repair
Decorations are the equivalent embodiment of equivalent variations, as long as being without departing from technical solution of the present invention content, according to the technical essence of the invention
To any simple modification, equivalent change and modification made by above example, in the range of still falling within technical solution of the present invention.
Claims (4)
1. hydro-thermal method prepares stainless (steel) wire load FeCO3The method of negative plate, it is characterised in that：Include the following steps：
A, it takes stainless (steel) wire first to boil corrosion treatment with dilute acid soln, is then cleaned by ultrasonic and is dried with deionized water, obtain table
The stainless (steel) wire matrix of face cleaning, is put into hydrothermal reaction kettle, spare；
B, hexa is added while stirring in deionized water, adjusts pH value of solution≤7, then adds polyethylene glycol, mixes
FeCl is added after closing uniformly2·4H2O obtains reaction precursor liquid after mixing；
C, reaction precursor liquid is poured into the hydrothermal reaction kettle of step a, until submerging stainless (steel) wire matrix, capping kettle will
Reaction kettle is placed in heater, and controlling reaction temperature is 150~180 DEG C, reacts 12~18h, after reaction, opens reaction
Kettle takes out stainless (steel) wire, is put into 5~10s of ultrasonic cleaning in deionization, dries, obtains stainless at a temperature of 60~70 DEG C
Steel mesh loads FeCO3Negative plate.
2. hydro-thermal method as described in claim 1 prepares stainless (steel) wire load FeCO3The method of negative plate, it is characterised in that：Step b
The middle pH value with HCl tune solution.
3. hydro-thermal method as described in claim 1 prepares stainless (steel) wire load FeCO3The method of negative plate, it is characterised in that：It is described poly-
The degree of polymerization of ethylene glycol is 600-20000, and polyethylene glycol addition is 1/5~1/4 of deionized water weight in step 1.
4. hydro-thermal method as described in claim 1 prepares stainless (steel) wire load FeCO3The method of negative plate, it is characterised in that：It is described
FeCl2·4H2The addition of O is the 1/100~1/50 of deionized water weight.
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| CN201711444203.XA CN108336304B (en) | 2017-12-27 | 2017-12-27 | Hydrothermal method for preparing stainless steel mesh loaded FeCO3Method for preparing negative plate |
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| CN108336304A true CN108336304A (en) | 2018-07-27 |
| CN108336304B CN108336304B (en) | 2020-09-11 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948140A (en) * | 2010-09-20 | 2011-01-19 | 上海理工大学 | Method for preparing Fe2O3 and Fe3O4 nano materials by taking F2<2+> salt as raw material |
| CN103288122A (en) * | 2013-05-28 | 2013-09-11 | 浙江大学 | Rhombus zinc oxide nanorod array and preparation method thereof |
| CN103840132A (en) * | 2014-03-03 | 2014-06-04 | 湖南雅城新材料发展有限公司 | Ferrous carbonate/graphene composite material and preparation method and applications thereof |
| CN104993125A (en) * | 2015-05-29 | 2015-10-21 | 北京科技大学 | Preparation method of lithium ion battery novel cathode material Fe3O4/Ni/C |
| CN105552329A (en) * | 2015-12-23 | 2016-05-04 | 芜湖天弋能源科技有限公司 | Preparation method for precursor FeCO3 of lithium ion battery positive electrode material LiPeO4 |
| CN107317019A (en) * | 2017-08-02 | 2017-11-03 | 中国石油大学(华东) | A kind of sodium-ion battery negative pole ferrous carbonate/graphene composite material and preparation method and application |
-
2017
- 2017-12-27 CN CN201711444203.XA patent/CN108336304B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948140A (en) * | 2010-09-20 | 2011-01-19 | 上海理工大学 | Method for preparing Fe2O3 and Fe3O4 nano materials by taking F2<2+> salt as raw material |
| CN103288122A (en) * | 2013-05-28 | 2013-09-11 | 浙江大学 | Rhombus zinc oxide nanorod array and preparation method thereof |
| CN103840132A (en) * | 2014-03-03 | 2014-06-04 | 湖南雅城新材料发展有限公司 | Ferrous carbonate/graphene composite material and preparation method and applications thereof |
| CN104993125A (en) * | 2015-05-29 | 2015-10-21 | 北京科技大学 | Preparation method of lithium ion battery novel cathode material Fe3O4/Ni/C |
| CN105552329A (en) * | 2015-12-23 | 2016-05-04 | 芜湖天弋能源科技有限公司 | Preparation method for precursor FeCO3 of lithium ion battery positive electrode material LiPeO4 |
| CN107317019A (en) * | 2017-08-02 | 2017-11-03 | 中国石油大学(华东) | A kind of sodium-ion battery negative pole ferrous carbonate/graphene composite material and preparation method and application |
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| Title |
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