CN105789550A - Electrode and preparation method of electrode material - Google Patents
Electrode and preparation method of electrode material Download PDFInfo
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- CN105789550A CN105789550A CN201610270555.7A CN201610270555A CN105789550A CN 105789550 A CN105789550 A CN 105789550A CN 201610270555 A CN201610270555 A CN 201610270555A CN 105789550 A CN105789550 A CN 105789550A
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- dichloride
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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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- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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 an electrode and a preparation method of an electrode material. The preparation method of the electrode material includes the steps: putting a dried filter tip into solution of one of vanadium dichloride, lead dichloride, tungsten dichloride and nickel dichloride or solution of at least two of the vanadium dichloride, lead dichloride, tungsten dichloride and nickel dichloride mixed according to an arbitrary proportion, and soaking the dried filter tip in the solution under the circumstance of ultrasonic oscillation for 60-120 minutes; taking out the filter tip from the solution, subjecting the filter tip to drying prior to high temperature carbonization to enable cellulose acetate fibers to form a porous layered carbon material of a micropore structure, respectively generating metallic fine particles and corresponding metallic oxide fine particles, evenly distributing the metallic fine particles and the metallic oxide fine particles in surface micropores of the porous layered carbon material or between folds among layers of the layered carbon material to obtain the carbonized material for making the electrode. The electrode material has excellent electrochemical performance, and is low in cost and beneficial to energy conservation and environmental protection.
Description
Technical field
The present invention relates to a kind of electrode material, especially relate to the preparation method of a kind of electrode and electrode material.
Background technology
Beyond secondary cell is in addition to chemical energy are converted into electric energy and discharges, can be by making electricity
Flow to flow with contrary direction during electric discharge, convert electrical energy into chemical energy and the battery that is charged.Closely
Nian Lai, the research and development of the aluminum secondary battery using aluminum metal to be negative pole are the most actively carried out.Aluminum cell by
In aluminum metal high ionization be inclined to, such as with manganese cell as use zinc metal be the conventional of negative pole
Battery is compared, it is possible to increase electromotive force, it is possible to expect high voltage and high power capacity.But, using chlorination
Ferrum is as in the aluminum cell of positive active material, due to the dissolution in the electrolyte of this iron chloride, and therefore this aluminum
The cycle characteristics of battery extremely deteriorates.
Summary of the invention
In view of this, the present invention proposes one and has better electrical chemical property and lower-cost electrode and electricity
The preparation method of pole material.
A kind of preparation method of electrode material, it includes step:
(1) cigarette filter being made up of acetate fiber is removed wrapping paper；
(2) dry filter plug is put into vanadium dichloride, lead dichloride, tungsten dichloride and Nickel Chloride its
One of solution, or two kinds of solution being mixed by any ratio of at least a part of which, and at supersonic oscillations environment
Under in above-mentioned solution soak 60-120 minute；
(3) from above-mentioned solution, take out filter plug, be dried, then process through high temperature cabonization, make acetic acid fine
Dimension forms the porous laminated material with carbon element with microcellular structure, and vanadium dichloride, lead dichloride, tungsten dichloride
Or/and Nickel Chloride generates vanadium, lead, tungsten or/and the metal of nickel is thin in high temperature cabonization processing procedure respectively
Microparticle and vanadium oxide, lead oxide, tungsten oxide or/and the metal-oxide fine particle of nickel oxide, and
Above-mentioned metal fine particle and above-mentioned metal-oxide fine particle are evenly distributed in porous laminated material with carbon element
Surface micropore among or the fold between layers of stratiform material with carbon element between, obtain for making electrode
Carbonization composite.
Wherein, in step (2), solution concentration is 3wt%～5wt%.
Wherein, step (1) also includes the most fully soaking cigarette filter, and ultrasound wave is clear
Wash 26-12 hour, dried for standby.
A kind of electrode, it includes above-mentioned carbonization composite powder, acetylene black and the binding agent prepared,
And the mass ratio of carbonization composite powder, acetylene black and binding agent is 75:15:10, appropriate N-
N-methyl-2-2-pyrrolidone N.
Wherein, binding agent is politef.
Compared with prior art, there is advantages that
Owing to acetate fiber is through vanadium dichloride VCl2, lead dichloride PbCl2, tungsten dichloride WCl2With/
Or dichloride nickel Cl2Activation processing after high temperature cabonization, forms the porous layer with microcellular structure
Shape material with carbon element, the surface area of porous laminated material with carbon element is relatively big, and the pore-size distribution of the micropore on surface is preferable,
A large amount of electrolytic ion can be absorbed, there is quick ion transport, therefore improve its chemical property,
Further, appropriate metal (vanadium, lead, tungsten are or/and the nickel) granule that generates during high temperature cabonization and right
The metal-oxide answered (vanadium oxide, lead oxide, tungsten oxide are or/and nickel oxide) is evengranular to be distributed in
Among the surface micropore of porous laminated material with carbon element or between the fold between layers of stratiform material with carbon element, thus
Improve chemical property；One of raw material is the cigarette filter extensively abandoned, and is conducive to turning waste into wealth,
Meet the industry development main trend of energy-conserving and environment-protective, there is wide marketing implementation prospect.
Accompanying drawing explanation
Fig. 1 is cyclic voltammetric (CV) curve synoptic diagram under electrode different scanning rates.
Fig. 2 is the schematic diagram of electrode constant current charge-discharge respectively under electric current density is 1A/g～10A/g.
Detailed description of the invention
The preparation method of a kind of electrode material that the present invention proposes, including step: (1) will be by acetate fiber
After the cigarette filter made removes wrapping paper, the most fully soak (general immersion 2-4 days),
Ultrasonic waves for cleaning 26-12 hour, dried for standby；(2) dried filter plug is put into vanadium dichloride VCl2、
Lead dichloride PbCl2, tungsten dichloride WCl2With Nickel Chloride NiCl2The solution of one of them, or the most extremely
Few two kinds of solution being mixed by any ratio, solution concentration is that 3wt%～5wt% is preferred, and in supersonic oscillations
Soak 60-120 minute in above-mentioned solution under environment；(3) from above-mentioned solution, take out filter plug, be dried,
Process through high temperature cabonization again, obtain carbonization composite powder.This carbonization composite powder is available
In the material making electrode.
Wherein, during high temperature cabonization processes, there is following chemical reaction: 3XCl2+2C+3O2=X+
3Cl2+2XCO3(high temperature), XCO3=XO+CO2(high temperature), wherein X represent V, Pb, W or
Ni.In above-mentioned chemical reaction process, C comes from acetate fiber, the O being carbonized2From remaining in pyrocarbon
Changing the oxygen in processing environment, above-mentioned chemical reaction process is also to acetate fiber (the i.e. carbon material being carbonized
Material) it is corroded thus forms the process of substantial amounts of microcellular structure.It can thus be seen that vanadium dichloride, two
Lead chloride, tungsten dichloride are or/and Nickel Chloride is in the mistake processed the acetate fiber of filter plug at high temperature cabonization
Cheng Zhong, generates vanadium, lead, tungsten respectively or/and the fine particle of nickel, and some generates the most again
Vanadium oxide, lead oxide, tungsten oxide are or/and the fine particle of nickel oxide.
Owing to the acetate fiber of filter plug is elongated and uniform diameter, by vanadium dichloride VCl2, lead dichloride
PbCl2, tungsten dichloride WCl2Or/and dichloride nickel Cl2After the activation processing of solution high temperature cabonization,
Acetate fiber becomes that to have porous micro-and for the stratiform material with carbon element of layer structure, the vanadium of generation, lead, tungsten or/
The vanadium oxide that with the fine particle of nickel and generates, lead oxide, tungsten oxide are or/and nickel oxide is the thinnest
Microparticle, be evenly distributed among the surface micropore of porous laminated material with carbon element or stratiform material with carbon element layer with
Between Ceng between fold.
Above-mentioned use cigarette filter is for twice laid, reduces the cigarette filter pollution without environment.
Then, it is also possible to directly use acetate fiber.
By carbonization composite powder, acetylene black and the binding agent 75:15:10 in mass ratio of above-mentioned preparation
Mixing, drips appropriate METHYLPYRROLIDONE, constantly grinds and is stirred until homogeneous pasty state；By above-mentioned paste
Shape mixture is spread evenly across on metal bar (such as aluminum, copper etc.), and vacuum drying is i.e. fabricated to electrode,
Or above-mentioned pasty mixture is spread upon equably on the one side of nickel foam, be then placed on dry
In case be dried, more dried nickel foam is placed on tablet machine carry out tabletting process can also make electrode.
Wherein, binding agent prepares, by existing, any one that electrode is used, and such as, binding agent is poly-four
Fluorothene.
When studying battery electrode material, it is common that utilize three electrode test systems to carry out test assessment.On
Stating prepared electrode slice is working electrode, is platinized platinum to electrode, and reference electrode is silver/silver chloride electrode,
Testing in the KOH electrolyte of 5mol/L under room temperature, test equipment is electrochemical workstation.Circulation volt
The potential window of peace test is set to 0V～0.5V, sweeps speed for 10mV/s～200mV/s.The survey of constant current charge-discharge
Examination window is 0V～0.5V, and electric current density is respectively 1A/g～10A/g.
Fig. 1 is that (abscissa is electricity to cyclic voltammetric (CV) curve synoptic diagram under electrode different scanning rates
Pressure, vertical coordinate is electric current).By above-mentioned electrode in the KOH solution of 5mol/L, under different scanning rates
Cyclic voltammetric (CV) curve, it is evident that sweep speed is the biggest, and the area that curve is enclosed is the biggest,
Additionally from the point of view of the shape of cyclic voltammetry curve, when sweeping speed less than 100mV/s, the cyclic voltammetric of sample
The figure that curve is surrounded, close to rectangle, illustrates that corresponding electrode material possesses good transmission electric charge and electricity
Solve the ability of liquid intermediate ion.
Fig. 2 is the schematic diagram (figure of electrode constant current charge-discharge respectively under electric current density is 1A/g～10A/g
In 2,4 curve respectively electric current densities from left to right are under 10A/g, 5A/g, 2A/g and 1A/g
Constant current charge-discharge curve).As can be seen from Figure 2 under the conditions of electric current density is 1A/g, electrode constant current
Charging and discharging curve is approximately rendered as symmetric shape, illustrates that it has an excellent chemical property, but its shape
Again some with oxide-based seemingly, and along with the reduction of electric current density is more and more obvious, is embodied in and fills
In electric process, voltage speedup in time is increasingly slower, and the slope of charging curve reduces, and deviate from material with carbon element
Common linear rise feature, metal-oxide (vanadium oxide, the oxidation contained in this explanation electrode material
Lead, tungsten oxide are or/and nickel oxide) the most effectively participate in the storage of electricity, for improving the electricity of material
Chemical property is made that contribution.
To sum up, owing to acetate fiber is through vanadium dichloride VCl2, lead dichloride PbCl2, tungsten dichloride WCl2
And/or dichloride nickel Cl2Activation processing after high temperature cabonization, forms the porous with microcellular structure
Stratiform material with carbon element, the surface area of porous laminated material with carbon element is relatively big, and the pore-size distribution of the micropore on surface is preferable,
A large amount of electrolytic ion can be absorbed, there is quick ion transport, therefore improve its chemical property,
Further, appropriate metal (vanadium, lead, tungsten are or/and the nickel) granule that generates during high temperature cabonization and right
The metal-oxide answered (vanadium oxide, lead oxide, tungsten oxide are or/and nickel oxide) is evengranular to be distributed in
Among the surface micropore of porous laminated material with carbon element or between the fold between layers of stratiform material with carbon element, thus
Improve chemical property.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this
Any amendment, equivalent and the improvement etc. made within the spirit of invention and principle, should be included in this
Within the protection domain of invention.
Claims (5)
1. the preparation method of an electrode material, it is characterised in that include step:
(1) cigarette filter being made up of acetate fiber is removed wrapping paper；
(2) dry filter plug is put into vanadium dichloride, lead dichloride, tungsten dichloride and Nickel Chloride its
One of solution, or two kinds of solution being mixed by any ratio of at least a part of which, and at supersonic oscillations environment
Under in above-mentioned solution soak 60-120 minute；
(3) from above-mentioned solution, take out filter plug, be dried, then process through high temperature cabonization, make acetic acid fine
Dimension forms the porous laminated material with carbon element with microcellular structure, and vanadium dichloride, lead dichloride, tungsten dichloride
Or/and Nickel Chloride generates vanadium, lead, tungsten or/and the metal of nickel is thin in high temperature cabonization processing procedure respectively
Microparticle and vanadium oxide, lead oxide, tungsten oxide or/and the metal-oxide fine particle of nickel oxide, and
Above-mentioned metal fine particle and above-mentioned metal-oxide fine particle are evenly distributed in porous laminated material with carbon element
Surface micropore among or the fold between layers of stratiform material with carbon element between, obtain for making electrode
Carbonization composite.
The preparation method of electrode material the most according to claim 1, it is characterised in that step (2)
Middle solution concentration is 3wt%～5wt%.
The preparation method of electrode material the most according to claim 1, it is characterised in that step (1)
Also include the most fully soaking cigarette filter, ultrasonic waves for cleaning 26-12 hour, be dried and treat
With.
4. an electrode, it is characterised in that include that claim 1 or 2 or 3 carbonization prepared is multiple
Condensation material powder, acetylene black and binding agent, and the matter of carbonization composite powder, acetylene black and binding agent
Amount ratio is 75:15:10, appropriate METHYLPYRROLIDONE.
Electrode the most according to claim 4, it is characterised in that binding agent is politef.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610270555.7A CN105789550A (en) | 2016-04-26 | 2016-04-26 | Electrode and preparation method of electrode material |
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| CN201610270555.7A CN105789550A (en) | 2016-04-26 | 2016-04-26 | Electrode and preparation method of electrode material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106252646A (en) * | 2016-08-24 | 2016-12-21 | 浙江超威创元实业有限公司 | A kind of lithium ion battery lithium manganate material synthetic method |
| CN108832084A (en) * | 2018-06-05 | 2018-11-16 | 复旦大学 | Lithium-sulfur cell material and preparation method thereof based on discarded cigarette butt biomass resource |
| CN109616662A (en) * | 2018-10-31 | 2019-04-12 | 欣旺达电子股份有限公司 | Nickel carries tungstic acid negative electrode material and preparation method thereof and lithium ion battery |
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| CN101038816A (en) * | 2007-04-20 | 2007-09-19 | 哈尔滨工程大学 | Method for preparing porous carbon/nano metal oxide composite material |
| CN101060169A (en) * | 2006-04-17 | 2007-10-24 | 三星Sdi株式会社 | Anode active material and method of preparing the same |
| CN103490047A (en) * | 2013-09-18 | 2014-01-01 | 山东理工大学 | Method for preparing three-dimensional hole carbon/nano NiO composite |
| CN103985850A (en) * | 2014-05-20 | 2014-08-13 | 武汉纺织大学 | Method for preparing vanadium pentoxide/conductive substrate composite electrode material |
-
2016
- 2016-04-26 CN CN201610270555.7A patent/CN105789550A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101060169A (en) * | 2006-04-17 | 2007-10-24 | 三星Sdi株式会社 | Anode active material and method of preparing the same |
| CN101038816A (en) * | 2007-04-20 | 2007-09-19 | 哈尔滨工程大学 | Method for preparing porous carbon/nano metal oxide composite material |
| CN103490047A (en) * | 2013-09-18 | 2014-01-01 | 山东理工大学 | Method for preparing three-dimensional hole carbon/nano NiO composite |
| CN103985850A (en) * | 2014-05-20 | 2014-08-13 | 武汉纺织大学 | Method for preparing vanadium pentoxide/conductive substrate composite electrode material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106252646A (en) * | 2016-08-24 | 2016-12-21 | 浙江超威创元实业有限公司 | A kind of lithium ion battery lithium manganate material synthetic method |
| CN106252646B (en) * | 2016-08-24 | 2019-07-09 | 浙江超威创元实业有限公司 | A kind of lithium ion battery lithium manganate material synthetic method |
| CN108832084A (en) * | 2018-06-05 | 2018-11-16 | 复旦大学 | Lithium-sulfur cell material and preparation method thereof based on discarded cigarette butt biomass resource |
| CN109616662A (en) * | 2018-10-31 | 2019-04-12 | 欣旺达电子股份有限公司 | Nickel carries tungstic acid negative electrode material and preparation method thereof and lithium ion battery |
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Application publication date: 20160720 |