CN108328657A - A method of preparing high-power power battery negative material - Google Patents
A method of preparing high-power power battery negative material Download PDFInfo
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- CN108328657A CN108328657A CN201711446686.7A CN201711446686A CN108328657A CN 108328657 A CN108328657 A CN 108328657A CN 201711446686 A CN201711446686 A CN 201711446686A CN 108328657 A CN108328657 A CN 108328657A
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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
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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
- H01M4/58—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
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- 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 present invention relates to a kind of methods preparing high-power power battery negative material, include the following steps：One, 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；Three, FeCl is added into solution B2·4H2O obtains solution C；Four, solution C is transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, the compactedness of control thermal response kettle is 70~80%, and reaction temperature is 150~180 DEG C, and the reaction time is 12~18h, and hydrothermal synthesis product D is obtained through hydro-thermal reaction；Five, cell negative electrode material will be obtained after hydrothermal synthesis product D separating, washings, drying and grinding.The present invention is with FeCl2·4H2O is source of iron, polyethylene glycol is template, hexa is precipitating reagent, and mesoporous FeCO is prepared using hydro-thermal method3Material, technological process is simple, and large specific surface area, the orderly mesoporous FeCO in mesoporous channel can be made3Nano material can be used as the negative material of high-power power battery.
Description
Technical field
The present invention relates to electrode material technical fields, and in particular to a kind of side preparing high-power power battery negative material
Method.
Background technology
Due to high-power power battery needed for new-energy automobile there is an urgent need to and lithium-ion-power cell presently, there are
The bottleneck problems such as price and safety, lithium-ion-power cell critical material are faced with new challenge.Lithium ion battery at present
Negative material is based on graphitized carbon material, but the SEI films that carbon material generates in discharge process for the first time, can cause irreversible
Capacitance loss also results in variation and the poor electric contact of carbon electrode internal structure sometimes；It may be because of protective layer when high temperature
It decomposes, leads to battery failure or cause safety issue；The unit volume capacity of graphite cathode is relatively low simultaneously, it is difficult to meet
The requirement of the fields high energy density cells such as electric vehicle, wind and solar energy energy storage, intelligent grid energy storage and conversion.
Therefore, it researches and develops high power capacity and the negative material of high performance-price ratio is very urgent.
" transformant " negative material ferrous carbonate is as novel lithium ion battery negative material, with the stone being commercialized at present
Black cathode is compared, with higher theoretical capacity, the advantages that wide applicability, good stability etc..Meanwhile when lithium from
When son is embedded into ferrous carbonate, obtained Li is reacted2CO3It is embedded into reaction gained in traditional metal oxide than it
Li20 stablizes so that ferrous carbonate can keep the lasting charge and discharge of high current density.How large specific surface area is prepared, it is mesoporous logical
Road is more and orderly mesoporous ferrous carbonate negative material is a problem to be solved.
Invention content
The purpose of the present invention is deficiency to solve above-mentioned technical problem, provides and a kind of preparing high-power power battery cathode
Large specific surface area, the FeCO more than mesoporous channel can be made in the method for material3Nano material is used as high-power power battery
Negative material.
The deficiency of the present invention to solve above-mentioned technical problem, used technical solution are：It is a kind of to prepare high-power power
The method of cell negative electrode material, includes the following steps：
One, under magnetic agitation, hexa is added in deionized water, with HCl tune pH value of solution≤7, avoids FeCl2·
4H2O is added to form hydroxide precipitation, obtains solution A；
Two, polyethylene glycol is added into solution A, obtains solution B after mixing；
Three, FeCl is added into solution B2·4H2O, stirring is to being completely dissolved to obtain solution C；
Four, solution C being transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, the compactedness of control thermal response kettle is 70~80%,
Hydrothermal temperature is 150~180 DEG C, and the hydro-thermal reaction time is 12~18h, and hydrothermal synthesis product D is obtained through hydro-thermal reaction；
Five, cell negative electrode material will be obtained after hydrothermal synthesis product D separating, washings, drying and grinding.
As a kind of advanced optimizing for method preparing high-power power battery negative material of the invention：The poly- second two
The degree of polymerization of alcohol is 600-20000, and polyethylene glycol addition is 1/5~1/4 of deionized water weight in step 1.
As a kind of advanced optimizing for method preparing high-power power battery negative material of the invention：It is described
FeCl2·4H2The addition of O is 1/50~1/25 of deionized water weight in step 1.
As a kind of advanced optimizing for method preparing high-power power battery negative material of the invention：The step 5
Specific method be：It is centrifuged under 8000-10000rpm speed conditions, then uses deionized water and ethyl alcohol to wash, connect
It and dries 12-24h at a temperature of 80~90 DEG C, it is finally ground to obtain mesoporous FeCO3。
Advantageous effect
The present invention is with FeCl2·4H2O is source of iron, polyethylene glycol is template, hexa is precipitating reagent, in hydrothermal condition
Under, 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 generates mesoporous FeCO3, technological process is simple, and large specific surface area, the orderly mesoporous FeCO in mesoporous channel can be made3
Nano material can be used as the negative material of high-power power battery.
Description of the drawings
Fig. 1 is the XRD spectra that cell negative electrode material is made in the embodiment of the present invention 1.
Fig. 2 is the SEM photograph that cell negative electrode material is made in the embodiment of the present invention 1.
Specific implementation mode
Further technical scheme of the present invention is illustrated below in conjunction with specific implementation mode.
Embodiment 1
A method of preparing high-power power battery negative material, it is characterised in that：Include the following steps：
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, stirring is to being completely dissolved to obtain solution C；The FeCl2·4H2O's adds
Enter 1/50 that amount is deionized water weight in step 1.
Four, solution C being transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, the compactedness of control thermal response kettle is 70%,
Hydrothermal temperature is 150 DEG C, the hydro-thermal reaction time 18h, and hydrothermal synthesis product D is obtained through hydro-thermal reaction；
Five, hydrothermal synthesis product D is centrifuged under 8000rpm speed conditions, deionized water and ethyl alcohol is then used to wash,
Then 12h is dried at a temperature of 90 DEG C, it is finally ground to obtain cell negative electrode material.
Embodiment 2：
A method of preparing high-power power battery negative material, it is characterised in that：Include the following steps：
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 the polyethylene glycol is 20000, is gathered
Ethylene glycol addition is the 1/5 of deionized water weight.
Three, FeCl is added into solution B2·4H2O, stirring is to being completely dissolved to obtain solution C；The FeCl2·4H2O's adds
Enter 1/25 that amount is deionized water weight in step 1.
Four, solution C being transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, the compactedness of control thermal response kettle is 80%,
Hydrothermal temperature is 180 DEG C, the hydro-thermal reaction time 12h, and hydrothermal synthesis product D is obtained through hydro-thermal reaction；
Five, hydrothermal synthesis product D is centrifuged under 10000rpm speed conditions, is then washed using deionized water and ethyl alcohol
It washs, is then dried for 24 hours at a temperature of 80 DEG C, it is finally ground to obtain cell negative electrode material.
Embodiment 3：
A method of preparing high-power power battery negative material, it is characterised in that：Include the following steps：
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 the polyethylene glycol is 10000, is gathered
Ethylene glycol addition is 0.21 times of deionized water weight.
Three, FeCl is added into solution B2·4H2O, stirring is to being completely dissolved to obtain solution C；The FeCl2·4H2O's adds
Enter 0.03 times that amount is deionized water weight in step 1.
Four, solution C being transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, the compactedness of control thermal response kettle is 75%,
Hydrothermal temperature is 160 DEG C, the hydro-thermal reaction time 16h, and hydrothermal synthesis product D is obtained through hydro-thermal reaction；
Five, hydrothermal synthesis product D is centrifuged under 9000rpm speed conditions, deionized water and ethyl alcohol is then used to wash,
Then 16h is dried at a temperature of 85 DEG C, it is finally ground to obtain cell negative electrode material.
Embodiment 4：
A method of preparing high-power power battery negative material, it is characterised in that：Include the following steps：
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 the polyethylene glycol is 8000, is gathered
Ethylene glycol addition is 0.23 times of deionized water weight in step 1.
Three, FeCl is added into solution B2·4H2O, stirring is to being completely dissolved to obtain solution C；The FeCl2·4H2O's adds
Enter 0.25 times that amount is deionized water weight in step 1.
Four, solution C being transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, the compactedness of control thermal response kettle is 78%,
Hydrothermal temperature is 170 DEG C, the hydro-thermal reaction time 14h, and hydrothermal synthesis product D is obtained through hydro-thermal reaction；
Five, hydrothermal synthesis product D is centrifuged under 9000rpm speed conditions, deionized water and ethyl alcohol is then used to wash,
Then 20h is dried at a temperature of 88 DEG C, it is finally ground to obtain cell negative electrode material.
Embodiment 5：
A method of preparing high-power power battery negative material, it is characterised in that：Include the following steps：
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 the polyethylene glycol is 18000, is gathered
Ethylene glycol addition is 0.24 times of deionized water weight in step 1.
Three, FeCl is added into solution B2·4H2O, stirring is to being completely dissolved to obtain solution C；The FeCl2·4H2O's adds
Enter 0.38 times that amount is deionized water weight in step 1.
Four, solution C being transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, the compactedness of control thermal response kettle is 72%,
Hydrothermal temperature is 155 DEG C, the hydro-thermal reaction time 14h, and hydrothermal synthesis product D is obtained through hydro-thermal reaction；
Five, hydrothermal synthesis product D is centrifuged under 10000rpm speed conditions, is then washed using deionized water and ethyl alcohol
It washs, then dries 18h at a temperature of 88 DEG C, it is finally ground to obtain cell negative electrode material.
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. a kind of method preparing high-power power battery negative material, it is characterised in that：Include the following steps：
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；
Three, FeCl is added into solution B2·4H2O, stirring is to being completely dissolved to obtain solution C；
Four, solution C being transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, the compactedness of control thermal response kettle is 70~80%,
Hydrothermal temperature is 150~180 DEG C, and the hydro-thermal reaction time is 12~18h, and hydrothermal synthesis product D is obtained through hydro-thermal reaction；
Five, cell negative electrode material will be obtained after hydrothermal synthesis product D separating, washings, drying and grinding.
2. a kind of method preparing high-power power battery negative material as described in claim 1, it is characterised in that：The poly- second
The degree of polymerization of glycol is 600-20000, and polyethylene glycol addition is 1/5~1/4 of deionized water weight in step 1.
3. a kind of method preparing high-power power battery negative material as described in claim 1, it is characterised in that：It is described
FeCl2·4H2The addition of O is 1/50~1/25 of deionized water weight in step 1.
4. a kind of method preparing high-power power battery negative material as described in claim 1, it is characterised in that：The step
Five specific method is：It is centrifuged under 8000-10000rpm speed conditions, deionized water and ethyl alcohol is then used to wash,
Then 12-24h is dried at a temperature of 80~90 DEG C, it is finally ground to obtain cell negative electrode material.
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Citations (4)
| 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 |
| TWI381995B (en) * | 2008-12-30 | 2013-01-11 | Univ Far East | A method for surface modification of electrolytic induction heating powder |
| KR101305393B1 (en) * | 2011-11-08 | 2013-09-06 | 한국과학기술연구원 | Amine functionalized mesoporous iron oxyhydroxide and method for fabricating the same |
| CN106848192A (en) * | 2017-02-20 | 2017-06-13 | 安徽师范大学 | Layered porous iron oxide electrode material and preparation method thereof, lithium ion cell electrode piece and preparation method thereof and lithium ion battery |
-
2017
- 2017-12-27 CN CN201711446686.7A patent/CN108328657B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI381995B (en) * | 2008-12-30 | 2013-01-11 | Univ Far East | A method for surface modification of electrolytic induction heating powder |
| 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 |
| KR101305393B1 (en) * | 2011-11-08 | 2013-09-06 | 한국과학기술연구원 | Amine functionalized mesoporous iron oxyhydroxide and method for fabricating the same |
| CN106848192A (en) * | 2017-02-20 | 2017-06-13 | 安徽师范大学 | Layered porous iron oxide electrode material and preparation method thereof, lithium ion cell electrode piece and preparation method thereof and lithium ion battery |
Non-Patent Citations (3)
| Title |
|---|
| LIU YI ET AL.: "A simple solution route to control synthesis of Fe3O4 nanomaterials at low temperature and their magnetic", 《SCIENCE IN CHINA SERIES B: CHEMISTRY》 * |
| XIN ZHENG ET AL.: "Template-free growth of well-crystalline a-Fe2O3 nanopeanuts with enhanced visible-light driven photocatalytic properties", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
| 刘伟健等: "碳酸亚铁的制备及电化学性能", 《电池》 * |
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