CN108281606A - The method that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa - Google Patents
The method that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa Download PDFInfo
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- CN108281606A CN108281606A CN201711444202.5A CN201711444202A CN108281606A CN 108281606 A CN108281606 A CN 108281606A CN 201711444202 A CN201711444202 A CN 201711444202A CN 108281606 A CN108281606 A CN 108281606A
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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
- H01M4/04—Processes of manufacture in general
- H01M4/049—Manufacturing of an active layer by chemical means
- H01M4/0497—Chemical precipitation
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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 present invention relates to a kind of the method that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa：Stainless (steel) wire is put into hydrothermal reaction kettle, then precursor liquid made of addition deionized water, precipitating reagent hexa, polyethylene glycol and ferrous salt takes out stainless (steel) wire after hydro-thermal reaction, and cleaning, drying is placed in Muffle furnace, and roasting obtains battery cathode.The present invention prepares stainless (steel) wire load FeO battery cathode under hydrothermal conditions, and in hydrothermal reaction process, hexamethylenetetramine, which decomposes, generates formaldehyde, and formaldehyde, which continues to decompose, generates CO3 2‑, in the presence of polyethylene glycol, CO3 2‑With FeCl2·4H2O is in the not upper mesoporous FeCO of generation of stainless (steel) wire3, mesoporous FeCO3Pass through Roasting Decomposition under an ar atmosphere into mesoporous FeO materials, entire technological process is simple, and large specific surface area, the more and orderly mesoporous FeO nano-electrode materials in mesoporous channel can be loaded on stainless (steel) wire.
Description
Technical field
The present invention relates to technical field of battery electrode materials, and in particular to using hexa as precipitating reagent hydro-thermal legal system
The method of standby stainless (steel) wire load FeO battery cathode.
Background technology
Iron resource is abundant, of low cost, environmental-friendly.Lower valency transition metal oxide（FeO）Not with organic bath
Side reaction occurs, there is higher stability.FeO energy gaps are 2.4eV, and excitation energy is smaller, and the electronics in valence band holds very much
Easily enter conduction band.Ferrous iron is easily converted to ferric iron, so FeO is usually nonstoichiometric compound.Since there are Fe3+, in order to
Keep the electroneutral of compound, 3 Fe2+Only need 2 Fe3+, thus there are a Fe2+Vacancy, generate lattice defect, change
The electric conductivity of kind material, electronics can rapidly shift between two kinds of oxidation state of iron, have stronger electric conductivity.In conclusion
FeO is the ideal novel anode material of comprehensive performance.When FeO prepares battery cathode sheet as negative material, need by sizing mixing,
The techniques such as coating and roll-in, it is relatively complicated.Therefore, large specific surface area, the more and orderly mesoporous FeO in mesoporous channel how to be prepared
Negative material, and the preparation process for how simplifying electrode slice is a problem to be solved.
Invention content
The purpose of the present invention is deficiency to solve above-mentioned technical problem, provide using hexa as precipitating reagent hydro-thermal
The method that method prepares stainless (steel) wire load FeO battery cathode.
The deficiency of the present invention to solve above-mentioned technical problem, used technical solution are：It is heavy with hexa
The method that shallow lake agent hydro-thermal method prepares stainless (steel) wire load FeO battery cathode：It is put into stainless (steel) wire in hydrothermal reaction kettle, then adds
Enter that deionized water, precipitating reagent hexa, precursor liquid takes out after hydro-thermal reaction made of polyethylene glycol and ferrous salt
Stainless (steel) wire, cleaning, drying are placed in Muffle furnace, and roasting obtains battery cathode.
As the present invention side that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa
Method advanced optimizes：The ferrous salt is four water frerrous chlorides, the addition of ferrous salt be deionized water weight 1/100~
1/50。
As the present invention side that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa
Method advanced optimizes：The degree of polymerization of the polyethylene glycol is 600-20000, and polyethylene glycol addition is deionized water weight
1/5~1/4.
As the present invention side that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa
Method advanced optimizes：The preparation method of precursor liquid is specially：Hexa is added while stirring in deionized water, uses
HCl tune sequentially adds polyethylene glycol and FeCl behind pH value of solution≤72·4H2O。
As the present invention side that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa
Method advanced optimizes：The temperature of hydro-thermal reaction is 150~180 DEG C, and the reaction time is 12~18h.
As the present invention side that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa
Method advanced optimizes：The stainless (steel) wire taken out after hydro-thermal reaction is put into 5~10s of ultrasonic cleaning in deionization, 60~70
It dries, is subsequently placed in Muffle furnace at a temperature of DEG C.
As the present invention side that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa
Method advanced optimizes：The temperature of roasting controls within the scope of 200-250 DEG C.
As the present invention side that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa
Method advanced optimizes：Roasting carries out under an ar atmosphere, and gas flow rate control is within the scope of 400-600SCCM.
Advantageous effect
One, the present invention uses stainless steel steel mesh for carrier, with FeCl2·4H2O is source of iron, polyethylene glycol is template, hexa-methylene
Tetramine is that precipitating reagent prepares stainless (steel) wire and loads FeO battery cathode, electrode high mechanical strength obtained, and due to being free of bonding
Agent 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.
Two, the present invention prepares stainless (steel) wire load FeO battery cathode, in hydrothermal reaction process, six times under hydrothermal conditions
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, mesoporous FeCO3Pass through Roasting Decomposition under an ar atmosphere into mesoporous FeO materials, entire work
Skill flow is simple, and large specific surface area, the more and orderly mesoporous FeO nano-electrodes material in mesoporous channel can be loaded on stainless (steel) wire
Material.
Description of the drawings
Fig. 1 is the electromicroscopic photograph a that the embodiment of the present invention 1 is made that stainless (steel) wire grows FeO battery cathode.
Fig. 2 is the electromicroscopic photograph b that the embodiment of the present invention 1 is made that stainless (steel) wire grows FeO battery cathode.
Specific implementation mode
Further technical scheme of the present invention is illustrated below in conjunction with specific implementation mode.
Embodiment 1
The method that stainless (steel) wire loads FeO battery cathode, including following step are prepared by precipitating reagent hydro-thermal method of hexa
Suddenly：
One, under magnetic agitation, hexa is added in deionized water, with HCl tune pH value of solution≤7, obtains solution A；
Two, polyethylene glycol is added into solution A, obtains solution B after mixing, the degree of polymerization of polyethylene glycol is 600, polyethylene glycol
Addition is the 1/4 of deionized water weight；
Three, FeCl is added into solution B2·4H2O stirs to solution C is completely dissolved to obtain, solution C is transferred to polytetrafluoroethylene (PTFE)
In liner hydrothermal reaction kettle, FeCl2·4H2The addition of O is 1/100 of deionized water weight in step 1；
Four, the stainless (steel) wire cleaned up is put into hydrothermal reaction kettle, be immersed in solution C, control the compactedness of thermal response kettle
It is 75%, hydrothermal temperature is 160 DEG C, the hydro-thermal reaction time 16h, carries out hydro-thermal reaction；
Five, after hydro-thermal reaction, stainless (steel) wire is taken out, is put into ultrasonic cleaning 8s in deionization, is dried at a temperature of 75 DEG C
It is dry, it is subsequently placed in Muffle furnace, under an ar atmosphere, control calcination temperature is 230 DEG C, and gas flow rate 500SCCM, roasting obtains
Stainless (steel) wire loads FeO battery cathode.
Embodiment 2：
The method that stainless (steel) wire loads FeO battery cathode, including following step are prepared by precipitating reagent hydro-thermal method of hexa
Suddenly：
One, under magnetic agitation, hexa is added in deionized water, with HCl tune pH value of solution≤7, obtains solution A；
Two, polyethylene glycol is added into solution A, obtains solution B after mixing, the degree of polymerization of polyethylene glycol is 1200, poly- second two
Alcohol addition is the 1/4 of deionized water weight；
Three, FeCl is added into solution B2·4H2O stirs to solution C is completely dissolved to obtain, solution C is transferred to polytetrafluoroethylene (PTFE)
In liner hydrothermal reaction kettle, FeCl2·4H2The addition of O is 1/90 of deionized water weight in step 1；
Four, the stainless (steel) wire cleaned up is put into hydrothermal reaction kettle, be immersed in solution C, control the compactedness of thermal response kettle
It is 70%, hydrothermal temperature is 150 DEG C, the hydro-thermal reaction time 18h, carries out hydro-thermal reaction；
Five, after hydro-thermal reaction, stainless (steel) wire is taken out, is put into ultrasonic cleaning 5 in deionization, is dried at a temperature of 70 DEG C
It is dry, it is subsequently placed in Muffle furnace, under an ar atmosphere, control calcination temperature is 200 DEG C, and gas flow rate 600SCCM, roasting obtains
Stainless (steel) wire loads FeO battery cathode.
Embodiment 3：
The method that stainless (steel) wire loads FeO battery cathode, including following step are prepared by precipitating reagent hydro-thermal method of hexa
Suddenly：
One, under magnetic agitation, hexa is added in deionized water, with HCl tune pH value of solution≤7, obtains solution A；
Two, polyethylene glycol is added into solution A, obtains solution B after mixing, the degree of polymerization of polyethylene glycol is 5000, poly- second two
Alcohol addition is the 1/5 of deionized water weight；
Three, FeCl is added into solution B2·4H2O stirs to solution C is completely dissolved to obtain, solution C is transferred to polytetrafluoroethylene (PTFE)
In liner hydrothermal reaction kettle, FeCl2·4H2The addition of O is 1/80 of deionized water weight in step 1；
Four, the stainless (steel) wire cleaned up is put into hydrothermal reaction kettle, be immersed in solution C, control the compactedness of thermal response kettle
It is 80%, hydrothermal temperature is 180 DEG C, the hydro-thermal reaction time 12h, carries out hydro-thermal reaction；
Five, after hydro-thermal reaction, stainless (steel) wire is taken out, is put into ultrasonic cleaning 10s in deionization, is dried at a temperature of 60 DEG C
It is dry, it is subsequently placed in Muffle furnace, under an ar atmosphere, control calcination temperature is 250 DEG C, and gas flow rate 400SCCM, roasting obtains
Stainless (steel) wire loads FeO battery cathode.
Embodiment 4：
The method that stainless (steel) wire loads FeO battery cathode, including following step are prepared by precipitating reagent hydro-thermal method of hexa
Suddenly：
One, under magnetic agitation, hexa is added in deionized water, with HCl tune pH value of solution≤7, obtains solution A；
Two, polyethylene glycol is added into solution A, obtains solution B after mixing, the degree of polymerization of polyethylene glycol is 15000, poly- second two
Alcohol addition is the 1/4 of deionized water weight；
Three, FeCl is added into solution B2·4H2O stirs to solution C is completely dissolved to obtain, solution C is transferred to polytetrafluoroethylene (PTFE)
In liner hydrothermal reaction kettle, FeCl2·4H2The addition of O is 1/60 of deionized water weight in step 1；
Four, the stainless (steel) wire cleaned up is put into hydrothermal reaction kettle, be immersed in solution C, control the compactedness of thermal response kettle
It is 75%, hydrothermal temperature is 170 DEG C, the hydro-thermal reaction time 114h, carries out hydro-thermal reaction；
Five, after hydro-thermal reaction, stainless (steel) wire is taken out, is put into ultrasonic cleaning 6s in deionization, is dried at a temperature of 68 DEG C
It is dry, it is subsequently placed in Muffle furnace, under an ar atmosphere, control calcination temperature is 240 DEG C, and gas flow rate 450SCCM, roasting obtains
Stainless (steel) wire loads FeO battery cathode.
Embodiment 5：
The method that stainless (steel) wire loads FeO battery cathode, including following step are prepared by precipitating reagent hydro-thermal method of hexa
Suddenly：
One, under magnetic agitation, hexa is added in deionized water, with HCl tune pH value of solution≤7, obtains solution A；
Two, polyethylene glycol is added into solution A, obtains solution B after mixing, the degree of polymerization of polyethylene glycol is 20000, poly- second two
Alcohol addition is the 1/4 of deionized water weight；
Three, FeCl is added into solution B2·4H2O stirs to solution C is completely dissolved to obtain, solution C is transferred to polytetrafluoroethylene (PTFE)
In liner hydrothermal reaction kettle, FeCl2·4H2The addition of O is 1/50 of deionized water weight in step 1；
Four, the stainless (steel) wire cleaned up is put into hydrothermal reaction kettle, be immersed in solution C, control the compactedness of thermal response kettle
It is 80%, hydrothermal temperature is 150 DEG C, the hydro-thermal reaction time 16h, carries out hydro-thermal reaction；
Five, after hydro-thermal reaction, stainless (steel) wire is taken out, is put into ultrasonic cleaning 8s in deionization, is dried at a temperature of 62 DEG C
It is dry, it is subsequently placed in Muffle furnace, under an ar atmosphere, control calcination temperature is 210 DEG C, and gas flow rate 550SCCM, roasting obtains
Stainless (steel) wire loads FeO battery cathode.
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 (8)
1. preparing the method that stainless (steel) wire loads FeO battery cathode by precipitating reagent hydro-thermal method of hexa, feature exists
In：Stainless (steel) wire is put into hydrothermal reaction kettle, then be added deionized water, precipitating reagent hexa, polyethylene glycol and
Precursor liquid made of ferrous salt takes out stainless (steel) wire after hydro-thermal reaction, and cleaning, drying is placed in Muffle furnace, and roasting obtains
Battery cathode.
2. preparing stainless (steel) wire as precipitating reagent hydro-thermal method using hexa as described in claim 1 loads FeO battery cathode
Method, it is characterised in that：The ferrous salt is four water frerrous chlorides, and the addition of ferrous salt is the 1/ of deionized water weight
100~1/50.
3. preparing stainless (steel) wire as precipitating reagent hydro-thermal method using hexa as described in claim 1 loads FeO battery cathode
Method, it is characterised in that：The degree of polymerization of the polyethylene glycol is 600-20000, and polyethylene glycol addition is deionized water weight
The 1/5~1/4 of amount.
4. preparing stainless (steel) wire as precipitating reagent hydro-thermal method using hexa as claimed in claim 2 loads FeO battery cathode
Method, it is characterised in that：The preparation method of precursor liquid is specially：Hexa-methylene four is added while stirring in deionized water
Amine, with sequentially adding polyethylene glycol and FeCl behind HCl tune pH value of solution≤72·4H2O。
5. preparing stainless (steel) wire as precipitating reagent hydro-thermal method using hexa as described in claim 1 loads FeO battery cathode
Method, it is characterised in that：The temperature of hydro-thermal reaction is 150~180 DEG C, and the reaction time is 12~18h.
6. preparing stainless (steel) wire as precipitating reagent hydro-thermal method using hexa as described in claim 1 loads FeO battery cathode
Method, it is characterised in that：The stainless (steel) wire taken out after hydro-thermal reaction is put into 5~10s of ultrasonic cleaning in deionization, 60~
It dries, is subsequently placed in Muffle furnace at a temperature of 70 DEG C.
7. preparing stainless (steel) wire as precipitating reagent hydro-thermal method using hexa as described in claim 1 loads FeO battery cathode
Method, it is characterised in that：The temperature of roasting controls within the scope of 200-250 DEG C.
8. preparing stainless (steel) wire as precipitating reagent hydro-thermal method using hexa as described in claim 1 loads FeO battery cathode
Method, it is characterised in that：Roasting carries out under an ar atmosphere, and gas flow rate control is within the scope of 400-600SCCM.
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| CN201711444202.5A CN108281606A (en) | 2017-12-27 | 2017-12-27 | The method that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa |
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| CN201711444202.5A CN108281606A (en) | 2017-12-27 | 2017-12-27 | The method that stainless (steel) wire loads FeO battery cathode is prepared by precipitating reagent hydro-thermal method of hexa |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110357168A (en) * | 2019-05-14 | 2019-10-22 | 江西师范大学 | A kind of preparation method of lithium ion battery negative material |
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2017
- 2017-12-27 CN CN201711444202.5A patent/CN108281606A/en active Pending
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| 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 |
| 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 |
| JP2017103136A (en) * | 2015-12-03 | 2017-06-08 | Tdk株式会社 | Negative electrode active material for lithium ion secondary batteries, negative electrode for lithium ion secondary batteries, and lithium ion secondary battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110357168A (en) * | 2019-05-14 | 2019-10-22 | 江西师范大学 | A kind of preparation method of lithium ion battery negative material |
| CN110357168B (en) * | 2019-05-14 | 2020-04-21 | 江西师范大学 | Preparation method of lithium ion battery negative electrode material |
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