CN104966839A - Lithium battery negative electrode material modifying method - Google Patents
Lithium battery negative electrode material modifying method Download PDFInfo
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- CN104966839A CN104966839A CN201510416508.4A CN201510416508A CN104966839A CN 104966839 A CN104966839 A CN 104966839A CN 201510416508 A CN201510416508 A CN 201510416508A CN 104966839 A CN104966839 A CN 104966839A
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- diphenol
- ethylamino
- benzene
- negative electrode
- cell cathode
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M4/58—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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
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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 lithium battery negative electrode material modifying method. According to the method, the negative electrode of a lithium battery is coated and modified with a novel biological material 4-(2-ethylamino) benzene-1,2-diphenol, a uniform coating layer is formed on the surface of the negative electrode so that the cycle performance of the corresponding negative electrode can be improved. The lithium battery negative electrode material modifying method has the advantages that the negative electrode material is only stirred in a water solution of 4-(2-ethylamino) benzene-1,2-diphenol for a certain period of time, and then the stirred mixture is filtered and dried, and thus the modification operation is completed. The process is simple, and the cycle performance of the modified negative electrode material can be obviously improved. The modifying method provides a simple and feasible process for preparing the negative electrode material with excellent performance, so that the performance of the lithium battery is further improved.
Description
Technical field
The present invention relates to lithium cell cathode material technical field, be specifically related to a kind of lithium cell cathode material method of modifying.
Background technology
Lithium battery is the green high-capacity environment-protecting battery occurred the nineties in 20th century, there is operating voltage high, specific energy is large, and self discharge is little, has extended cycle life, memory-less effect, the advantage such as quickly-chargeable and non-environmental-pollution is video camera, mobile phone, the ideal source of the portable electric appts such as notebook computer is also following desirable light high-energy power source used for electric vehicle.But the negative material of lithium battery is the key factor that its performance of restriction promotes further always.Such as common graphite, silicon, the lithium cell cathode materials such as lithium titanate all have cyclicity poor, the defects such as coulombic efficiency is low, are mainly the side reaction of the volumetric expansion of negative material in charge and discharge process (volumetric expansion of silicon can reach 300%-400%) and negative material and electrolyte caused (as the common intercalation of solvent causes coming off of graphite linings in the electrolytic solution).
Therefore, the modification of lithium cell cathode material is become to the key technology step improving lithium battery performance, existing a large amount of document and patent certificate, carrying out coated to lithium cell cathode material is a kind of alternative good method of modifying.As carried out coating modification by the method for polymer monomer living polymerization to lithium titanate in patent CN103730649 A, the coated lithium titanate first charge-discharge capacity of gained conductive carbon layer reaches 165mAh/g, cyclicity also significantly improves, and after 800 circulations, capacity still can keep more than 90%.In patent CN 103208624 A, PAA coated iron oxide nano particle carbonization, obtained high power capacity, the modified oxidized iron negative material that cyclicity is excellent.
But in existing bibliographical information and patent, the cladding process of employing comprises and adds surfactant, use the toxic solvents such as acetone, easily to environment, and cladding process is complicated, complex operation.
Summary of the invention
The object of the present invention is to provide a kind of simple to operate, excellent performance, and be expected to industrialized lithium cell cathode material method of modifying.The present invention, to be polymerized coated lithium cell cathode material to suppress the volumetric expansion in its charge and discharge process in water containing the compound of catechol functional group, improves the formation of SEI film and component to improve the cycle performance of respective negative material,
For solving the problem, the present invention adopts following scheme:
A kind of lithium cell cathode material method of modifying, is characterized in that, under 4-(2-ethylamino-) benzene-1,2-diphenol exists, carries out coating modification to lithium cell cathode material.Containing catechol functional group, there is stronger adsorption capacity, be attached on lithium cell cathode material surface, improve that it is dispersed, suppress the volumetric expansion in its charge and discharge process, improve the formation of SEI film and component to improve the cycle performance of respective negative material.
It has been generally acknowledged that, the irreversible capacity first of material is usually relevant with the specific surface area active of material, and the little graphite material of Selection radio surface area of should trying one's best is as modified feedstock.The present invention carries out preferably to existing lithium cell cathode material, finds to adopt 4-(2-ethylamino-) benzene-1,2-diphenol coated graphite, and silicon, when lithium titanate and iron oxide, the material list after coated reveals good initial coulombic efficiency and cycle performance.
Specifically comprising the steps: of said method
(1) cushioning liquid of 4-(2-ethylamino-) benzene-1,2-diphenol is prepared with 4-(2-ethylamino-) benzene-1,2-diphenol and water, alkaline matter;
(2) mixed by the cushioning liquid of lithium cell cathode material and 4-(2-ethylamino-) benzene-1,2-diphenol, stir 2-36h under 0-50 DEG C of condition, then filtering drying, to obtain final product.By regulating solution concentration and the reaction time of 4-(2-ethylamino-) benzene-1,2-diphenol, can coating thickness be controlled, optimizing and obtaining best modified condition.
Preferably, described alkaline matter is one or more in NaOH, trishydroxymethylaminomethane and hydrochloride thereof, carbonic hydroammonium, ammonium carbonate or ammoniacal liquor.
Although 4-(2-ethylamino-) benzene-1, the coated chemical property to improving negative material of 2-diphenol has very great help, but coating layer is also not easily blocked up or excessively thin, when coated thickness is too large, although interfacial reaction is suppressed very well, but the migration distance of the graphite layers of Lithium-ion embeding graphite layers increases, migration difficulty increases, and embedding lithium capacity starts to reduce; When coated thickness is too little, the graphite-structure of electrode surface fails to be effectively covered, and electrolyte component can not be effectively controlled in the reduction reaction of graphite surface, and electrode property also can therefore by impact to a certain extent.By regulating 4-(2-ethylamino-) benzene-1, the concentration of 2-diphenol cushioning liquid and reaction time, coating thickness can be controlled, therefore, the present invention studies rear discovery, described 4-(2-ethylamino-) benzene-1, in 2-diphenol cushioning liquid, when the mass concentration of 4-(2-ethylamino-) benzene-1,2-diphenol is 0.05%-2%, obtain preferably coating thickness.
Dopamine molecule contains catechol and amido functional group, in alkaline solution and oxidation environment, can at substrate material surface from poly-compound, form the DOPA amine layer with high-adhesiveness, but when pH value is excessive, be unfavorable for the carrying out that anti-disproportionated reaction and follow-up cross-linking reaction occur between dopamine and dopamine quinone, therefore, the pH value of the preferred 4-of the present invention (2-ethylamino-) benzene-1,2-diphenol cushioning liquid is 7-9.
The attachment behavior of dopamine to substrate material surface derives from catechol and the amido functional group of dopamine, this structure can set up covalency and non-covalent interaction with organic and inorganic surface, thus make dopamine cross-linked layer brute force be attached on material surface, drying and processing effectively can remove the moisture of dopamine film surface attachment, but temperature is too high, easily cause the destruction of chemical bond between dopamine film and lithium cell cathode material, affect the characterization of adsorption of dopamine, therefore, the condition of the drying and processing that the present invention is preferred is: dry 2 ~ 30h at 40 ~ 200 DEG C.
Present invention also offers a kind of lithium ion battery, comprise the lithium ion battery negative material adopting above-mentioned lithium cell cathode material method of modifying to prepare.
Compared with prior art, the advantage of this invention is:
1 operation is easy, is easy to industrialization, without using surfactant, organic solvent etc., environmentally friendly, is applicable to large-scale production;
2, by regulating solution concentration and the reaction time of 4-(2-ethylamino-) benzene-1,2-diphenol, can control coating thickness, optimize and obtain best modified condition.
3 due to the good auto polymerization performance of 4-(2-ethylamino-) benzene-1,2-diphenol, can form uniform coating layer on the negative material surface of pre-modification.
4 through the negative material of modified gained, and cycle performance all improves.
Accompanying drawing explanation
The transmission electron microscope photo (TEM) of Figure 14-(2-ethylamino-) benzene-1,2-diphenol polymerization coated graphite;
The electron scanning micrograph (SEM) of the non-coated iron oxide sample of Fig. 2;
The electron scanning micrograph (SEM) of Figure 34-(2-ethylamino-) benzene-1,2-diphenol polymerization coated iron oxide;
Iron oxide charge and discharge cycles figure before Fig. 4 is not coated
Iron oxide charge and discharge cycles figure after Fig. 5 is coated
The cyclicity of the coated rear graphite of Fig. 6.
Embodiment
Embodiment below by specifics illustrates the present invention:
Embodiment one is got 2.25g 4-(2-ethylamino-) benzene-1,2-diphenol and is dissolved in 450ml deionized water, adds 1.35g TRIS again after stirring and dissolving, regulates solution PH to 8.5, finally 1.8g graphite is added solution, stir 24h under room temperature condition.After having reacted, filter products therefrom, and spend deionized water repeatedly, and in an oven under 70 DEG C of conditions dry 6h. it forms the uniform coating layer of one deck at graphite surface as seen from Figure 1.
Embodiment two is got 9g 4-(2-ethylamino-) benzene-1,2-diphenol and is dissolved in 450ml deionized water, adds 4.05gTRIS again after stirring and dissolving, regulates solution PH to 7, finally 1.8g silicon is added solution, stir 2h under room temperature condition.After having reacted, filter products therefrom, and spend deionized water repeatedly, and dry 30h. under 40 DEG C of conditions in an oven
Embodiment three is got 0.45g 4-(2-ethylamino-) benzene-1,2-diphenol and is dissolved in 450ml deionized water, adds 0.30g TRIS again after stirring and dissolving, regulates solution PH to 9, finally 1.8g lithium titanate is added solution, stir 36h under room temperature condition.After having reacted, filter products therefrom, and spend deionized water repeatedly, and dry 2h. under 200 DEG C of conditions in an oven
Embodiment four is got 0.45g 4-(2-ethylamino-) benzene-1,2-diphenol and is dissolved in 450ml deionized water, adds 0.30g TRIS again after stirring and dissolving, regulates solution PH to 9, finally 1.8g iron oxide is added solution, stir 36h under room temperature condition.After having reacted, filter products therefrom, and spend deionized water repeatedly, and in an oven under 200 DEG C of conditions dry 2h. to compare Fig. 2 and Fig. 3, iron oxide surface pattern changes, namely coated by 4-(2-ethylamino-) benzene-1,2-diphenol institute.
Embodiment five is got 1.25g 4-(2-ethylamino-) benzene-1,2-diphenol and is dissolved in 450ml deionized water, adds 0.95g TRIS again after stirring and dissolving, regulates solution PH to 8.5, finally 1.8g iron oxide is added solution, stir 20h under room temperature condition.After having reacted, filter products therefrom, and spend deionized water repeatedly, and dry 12h. under 60 DEG C of conditions in an oven
Final products therefrom is taken 0.2-0.4g, and with 8:1:1 mass ratio and acetylene black, CMC phase mixes, and water makees solvent and fully stirs, and is applied to Copper Foil after mixing, vacuumize 24h under 70 DEG C of conditions.After cut-parts, in glove box, dress up battery, and do corresponding electrochemical property test at electrochemical workstation.Compare Fig. 4 and Fig. 5, and visible iron oxide significantly improves at coated its cycle performance rear at 4-(2-ethylamino-) benzene-1,2-diphenol.
Although above-mentioned, the specific embodiment of the present invention is described; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (8)
1. a lithium cell cathode material method of modifying, is characterized in that, under 4-(2-ethylamino-) benzene-1,2-diphenol exists, carries out coating modification to lithium cell cathode material.
2. the method for claim 1, is characterized in that, lithium cell cathode material comprises graphite, silicon, and lithium titanate, one or more in iron oxide.
3. the method for claim 1, is characterized in that, comprises the steps:
(1) cushioning liquid of 4-(2-ethylamino-) benzene-1,2-diphenol is prepared with 4-(2-ethylamino-) benzene-1,2-diphenol and water, alkaline matter;
(2) mixed by the cushioning liquid of lithium cell cathode material and 4-(2-ethylamino-) benzene-1,2-diphenol, stir 2-36h under 0-50 DEG C of condition, then filtering drying, to obtain final product.
4. method as claimed in claim 3, is characterized in that, described alkaline matter is one or more in NaOH, trishydroxymethylaminomethane and hydrochloride thereof, carbonic hydroammonium, ammonium carbonate or ammoniacal liquor.
5. method as claimed in claim 3, it is characterized in that, in described 4-(2-ethylamino-) benzene-1,2-diphenol cushioning liquid, the mass concentration of 4-(2-ethylamino-) benzene-1,2-diphenol is 0.05%-2%.
6. method as claimed in claim 3, it is characterized in that, the pH value of described 4-(2-ethylamino-) benzene-1,2-diphenol cushioning liquid is 7-9.
7. method as claimed in claim 3, it is characterized in that, the condition of described drying and processing is: dry 2 ~ 30h at 40 ~ 200 DEG C.
8. a lithium ion battery, is characterized in that: comprise the lithium ion battery negative material prepared containing the lithium cell cathode material method of modifying according to any one of claim 1-7.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106654273A (en) * | 2017-02-06 | 2017-05-10 | 安徽鹰龙工业设计有限公司 | Organic cathode material for lithium battery, and preparation method thereof |
| CN106784734A (en) * | 2017-02-06 | 2017-05-31 | 深圳市斯诺实业发展股份有限公司 | A kind of lithium cell cathode material and preparation method thereof |
| CN115084515A (en) * | 2021-03-11 | 2022-09-20 | 中国科学院上海硅酸盐研究所 | Inorganic oligomer lithium-containing composite metal oxide material, preparation method thereof and application thereof in lithium ion battery cathode material |
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| CN106784734A (en) * | 2017-02-06 | 2017-05-31 | 深圳市斯诺实业发展股份有限公司 | A kind of lithium cell cathode material and preparation method thereof |
| CN115084515A (en) * | 2021-03-11 | 2022-09-20 | 中国科学院上海硅酸盐研究所 | Inorganic oligomer lithium-containing composite metal oxide material, preparation method thereof and application thereof in lithium ion battery cathode material |
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Application publication date: 20151007 |