CN104979544A - Negative electrode active material, preparation method and battery - Google Patents
Negative electrode active material, preparation method and battery Download PDFInfo
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- CN104979544A CN104979544A CN201510449769.6A CN201510449769A CN104979544A CN 104979544 A CN104979544 A CN 104979544A CN 201510449769 A CN201510449769 A CN 201510449769A CN 104979544 A CN104979544 A CN 104979544A
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- shell material
- active core
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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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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
Abstract
The invention discloses a preparation method of a negative electrode active material. The preparation method comprises the following steps: mixing lithium chloride solution and alcohol solvent according to volume ratio, stirring, adding titanium alkoxide according to the volume ratio of titanium alkoxide to the alcohol solvent until white precipitates occur; sealing the solution, and standing to obtain solution containing hydrated titanium oxide microspheres; under the stirring state, adding lithium acetate into the solution containing the hydrated titanium oxide microspheres according to the number ratio of lithium atoms to titanium atoms being 0.8-0.85 under the stirring state; adding pyrrole into the solution obtained through the steps according to the volume ratio of titanium alkoxides to pyrrole being (5-10) to 1, and then carrying out in situ polymerization on pyrrole by adding an oxidizing agent; evaporating the solvent in the solution to obtain a precursor; and calcining the precursor at 700-900 DEG C under the protection of inert gas. The invention also provides a negative electrode active material obtained through the method and a battery using the composite material.
Description
Technical field
The present invention relates to a kind of negative active core-shell material, preparation method and the battery containing this negative active core-shell material, particularly a kind of negative active core-shell material for lithium ion battery and preparation method.
Background technology
Spinel type lithium titanate (Li
4ti
5o
12) be the lithium ion battery negative material of a kind of " zero strain ", namely at Lithium-ion embeding with deviate from process, its lattice structure changes hardly, and therefore cyclical stability is excellent.Relative to lithium metal, the intercalation potential of lithium titanate is about 1.55V, therefore can not cause the precipitation of lithium metal or Li dendrite, and few with the side reaction of electrolyte, thus prevent electrolyte in the reduction of electrode surface, not only fail safe is high, and coulombic efficiency is high, have extended cycle life.In addition, because spinelle skeleton structure exists three-dimensional lithium ion diffusion admittance, lithium ion diffusion coefficient (2 × 10
-8cm
2/) more than an order of magnitude higher than commercialization graphite cathode material, therefore there is the high rate capability of potential excellence.But spinel type lithium titanate also has the deficiency of himself as lithium ion battery negative material, as high discharge platform can cause cell voltage low, thus make the specific energy of battery low; The conductance of himself is lower, and when high current charge-discharge, capacity attenuation is fast, and high rate performance is poor.
The effective way improving lithium titanate anode material high rate performance comprise use nanocrystalline material and carbon coated etc.Wherein, nanocrystalline barium titanate lithium titanate cathode material is used to be that the contact area of electrode and the electrolyte utilizing it larger and less lithium ion dilation angle are to improve charge-discharge velocity.But the same with other nano-electrode material, the heap real density of nano lithium titanate is low, although therefore can effectively improve its charge-discharge velocity, can reduce the specific energy of battery simultaneously.For this reason, in order to improve heap real density, and electrode slurrying and pole plate brushing are more prone to, battery enterprise favors the micron-size spherical lithium titanate anode material in uniform particle sizes more.Carbon is coated is improve one of very effective method of lithium titanate anode material high rate performance, but existing carbon method for coating is all usually after synthesis lithium titanate powdery, it is coated that recycling gas phase or the method for liquid phase carry out secondary, not only process is complicated, energy consumption is high, and many because of lithium titanate powdery dispersion uneven, cause carbon covered effect undesirable.The coated method of carbon is carried out in organic carbon hydrate hydro-thermal (as the glucose) reaction particularly usually adopted, and not only yields poorly, poor controllability, and has peculiar smell, and needs large water gaging or alcoholic solvent washing etc., is unfavorable for energy-conserving and environment-protective.
Summary of the invention
The invention provides a kind of negative active core-shell material, its preparation method and the battery containing this negative active core-shell material, can solve the problem.
A preparation method for negative active core-shell material, comprises the following steps:
S1: by lithium chloride solution and alcohols solvent by volume 1 ~ 10:1000 mix, under stirring, add Titanium alkoxides, until there is white precipitate by Titanium alkoxides and alcohols solvent volume ratio 1 ~ 10:100;
S2: the solution sealing obtained by step S1, leaves standstill the solution obtained containing hydration titania microsphere;
S3: under stirring, be that 0.80 ~ 0.85:1 adds lithium acetate to described containing in the solution of hydration titania microsphere by the number ratio of lithium atom and titanium atom, wherein, the lithium atom in lithium chloride is contained in aforementioned proportion;
S4: under stirring, adds pyrroles as carbon source in the solution obtained in step S3 for 5 ~ 10:1 by the volume ratio of Titanium alkoxides and pyrroles, then adds oxidant and make pyrroles's in-situ polymerization;
S5: the solvent evaporation in the solution obtained by step S4, obtains the lithium titanate microballoon presoma that polypyrrole is coated;
S6: by the lithium titanate microballoon presoma that obtains under inert gas shielding, 700 ~ 900 DEG C of calcinings.
Further, described alcohols solvent is methyl alcohol, ethanol, isopropyl alcohol, normal propyl alcohol, ethylene glycol or its mixing.
Further, described lithium chloride solution and alcohols solvent by volume 4 ~ 8:1000 mix.
Further, described Titanium alkoxides and alcohols solvent add Titanium alkoxides according to volume ratio 3 ~ 9:100.
Further, described Titanium alkoxides is isopropyl titanate or butyl titanate, purity 98 more than wt.%.
Further, described pyrroles and Titanium alkoxides by volume 1:5 ~ 10 add as carbon source, and use hydrogen peroxide to cause the in-situ polymerization of pyrroles as oxidant;
Further, the solvent evaporation in the solution that obtains for 40 ~ 80 DEG C thus by step S4 of control temperature.
Further, described inert gas is nitrogen or rare gas, and the heating rate in calcination process is 1 ~ 5 DEG C/min, and the sintering soak time is 2 ~ 10h, finally with the cold cooling of stove.
The present invention also provides a kind of negative active core-shell material obtained by above-mentioned preparation method, wherein, described negative active core-shell material comprises the lithium titanate of kernel and is coated on the carbon on lithium titanate surface, and described negative active core-shell material is microspheroidal, and particle diameter is between 0.5 μm ~ 3 μm.
Further, described lithium titanate is spinel type lithium titanate.
The present invention also provides a kind of battery comprising above-mentioned negative active core-shell material further, comprising: positive pole; Negative pole; And electrolyte; Wherein, described negative pole comprises above-mentioned negative active core-shell material.
The preparation method of negative active core-shell material provided by the invention, under room temperature and condition of normal pressure, the lithium titanate microballoon presoma that organic carbon source is coated is prepared in same precursor solution, then burning till to be coated on carbon in once calcining and completing of lithium titanate is made, thus reach Simplified flowsheet, reduce costs, realize the object of mass production.In addition, negative active core-shell material provided by the invention and the battery containing this negative active core-shell material, also have higher specific capacity and good cycle performance.
Accompanying drawing explanation
Preparation method's flow chart of the negative active core-shell material that Fig. 1 provides for the embodiment of the present invention.
The stereoscan photograph of the negative active core-shell material that Fig. 2 provides for the embodiment of the present invention 1.
The X ray diffracting spectrum of the negative active core-shell material that Fig. 3 provides for the embodiment of the present invention 1.
When the negative active core-shell material that Fig. 4 provides for the embodiment of the present invention 1 is as lithium ion battery negative, at the first cycle charge-discharge curve of 2C speed.
Fig. 5 for the negative active core-shell material that provides for the embodiment of the present invention 1 as lithium ion battery negative time, at the cyclic curve of 2C speed.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.Be understandable that, specific embodiment described herein is only for explaining the present invention, but not limitation of the invention.It also should be noted that, for convenience of description, illustrate only part related to the present invention in accompanying drawing but not entire infrastructure.
Please refer to Fig. 1, a kind of preparation method of negative active core-shell material, comprises the following steps:
S1: by lithium chloride solution and alcohols solvent by volume 1 ~ 10:1000 mix, under stirring, add Titanium alkoxides, until there is white precipitate by Titanium alkoxides and alcohols solvent volume ratio 1 ~ 10:100;
S2: the solution sealing obtained by step S1, leaves standstill the solution obtained containing hydration titania microsphere;
S3: under stirring, be that 0.80 ~ 0.85:1 adds lithium acetate to described containing in the solution of hydration titania microsphere by the number ratio of lithium atom and titanium atom, wherein, the lithium atom in lithium chloride is contained in aforementioned proportion;
S4: under stirring, adds pyrroles as carbon source in the solution obtained in step S3 for 5 ~ 10:1 by the volume ratio of Titanium alkoxides and pyrroles, then adds oxidant and make pyrroles's in-situ polymerization;
S5: the solvent evaporation in the solution obtained by step S4, obtains the lithium titanate microballoon presoma that polypyrrole is coated;
S6: by the lithium titanate microballoon presoma that obtains under inert gas shielding, 700 ~ 900 DEG C of calcinings.
In step sl: the object adding described lithium chloride solution is the hydrolysis controlling agent as being Titanium alkoxides.Preferably, make described lithium chloride solution and alcohols solvent by volume 4 ~ 8:1000 mix.Described alcohols solvent can be methyl alcohol, ethanol, isopropyl alcohol, normal propyl alcohol, ethylene glycol or its mixing.Further, described Titanium alkoxides is isopropyl titanate or butyl titanate, purity 98 more than wt.%.Preferably, Titanium alkoxides is added by described Titanium alkoxides and alcohols solvent volume ratio 3 ~ 9:100.
In step s 2, the solution sealing obtained by step S1, leaves standstill more than 10h, preferred standing more than 20h, thus can obtain the solution containing hydration titania microsphere.
In step s3, the object adding excessive elemental lithium is the volatilization in order to compensate lithium in subsequent calcination process.Preferably, be that 0.85:1 adds lithium acetate to described containing in the solution of hydration titania microsphere by the number ratio of lithium atom and titanium atom.
In step s 4 which, described oxidant can be hydrogen peroxide or other can catalysis pyrroles polymerization material.Described pyrroles and hydrogen peroxide can be that 1:1 ~ 5 add hydrogen peroxide according to volume ratio.Be appreciated that described hydrogen peroxide can, as the oxidant of pyrrole monomer, make it at lithium titanate microballoon presoma in situ Polymerization, using the carbon source as lithium titanate material with carbon-coated surface.
In step s 5, the solvent evaporation in the solution that obtains for 40 ~ 80 DEG C thus by step S4 of control temperature.
In step s 6, described inert gas is nitrogen or rare gas, and the heating rate in calcination process is 1 ~ 5 DEG C/min, and calcination time is 2 ~ 10h, and after calcining, temperature retention time is 2 ~ 10h, finally with the cold cooling of stove, obtains the negative active core-shell material of grey black.Preferably, can in 700 ~ 900 DEG C of temperature ranges calcine by steps, preferably, in three temperature ranges such as 700 ~ 750 DEG C, 800 ~ 850 DEG C and 850 ~ 900 DEG C, calcine 2 ~ 12h respectively, thus more good crystallinity can be obtained.
The present invention also provides a kind of negative active core-shell material obtained by above-mentioned preparation method, wherein, described negative active core-shell material comprises the lithium titanate of kernel and is coated on the carbon on lithium titanate surface, and described negative active core-shell material is microspheroidal, and particle diameter is between 0.5 μm ~ 3 μm.Wherein, described lithium titanate is spinel type lithium titanate.
The present invention also provides a kind of battery comprising above-mentioned negative active core-shell material further, comprising: positive pole; Negative pole; And electrolyte; Wherein, described negative pole comprises above-mentioned negative active core-shell material.
Embodiment 1:
0.4ml lithium chloride (0.1M) solution is added the ethanol that 100ml content is 99.5wt.%, under stirring, adds 3ml isopropyl titanate, after there is white precipitate in solution, stop stirring; This solution is sealed, quiet to more than 20h, obtain the solution containing hydration titania microsphere; Under stirring, add lithium acetate by lithium atom and titanium atom quantitative proportion 0.85:1 and fully dissolve; Under stirring, add 0.2ml pyrroles as carbon source, then add 1ml hydrogen peroxide (purity 28 wt.%), the polymerization completing pyrroles is coated; Be heated to 60 DEG C and stir, solvent evaporated, obtaining the lithium titanate microballoon presoma that polypyrrole is coated; Above-mentioned presoma is calcined 5h at 800 DEG C under inert gas shielding, and wherein, heating rate is 5 DEG C/min, and after calcining, temperature retention time is 10h, finally namely obtains the coated lithium titanate microballoon of carbon with the cold cooling of stove.
Please refer to Fig. 2, as we can see from the figure, gained lithium titanate microballoon is black, and illustrate that successfully to achieve carbon coated, epigranular, particle diameter is between 0.5-3 μm.Please refer to Fig. 3, the X ray diffracting spectrum of the coated lithium titanate microballoon of the carbon of Fig. 3 prepared by embodiment 1, what prove synthesis is highly purified spinel type lithium titanate negative material.Please refer to Fig. 4-5, using the coated lithium titanate microballoon of prepared carbon as lithium ion battery negative, be that positive pole prepares half-cell to test the chemical property of the coated lithium titanate microballoon of carbon with lithium metal, at 350 mA/g(2C) time first discharge capacity reach 130 more than mAh/g, 200 circulation after discharge capacities still remain on about 118 mAh/g.
Embodiment 2:
Substantially the same manner as Example 1, difference is, replaces butyl titanate as titanium source using isopropyl titanate.
Embodiment 3
Substantially the same manner as Example 1, difference is, replaces ethanol as solvent using methyl alcohol.
Embodiment 4
Substantially the same manner as Example 1, difference is, replaces ethanol as solvent using ethylene glycol.
Embodiment 5
Substantially the same manner as Example 1, difference is, replaces ethanol as solvent using isopropyl alcohol.
Embodiment 6
Substantially the same manner as Example 1, difference is, replaces ethanol as solvent using normal propyl alcohol.
Experiment proves, embodiment 2-6 all can obtain uniformly, the negative active core-shell material of height ratio capacity and stability.
Note, above are only preferred embodiment of the present invention and institute's application technology principle.Skilled person in the art will appreciate that and the invention is not restricted to specific embodiment described here, various obvious change can be carried out for a person skilled in the art, readjust and substitute and can not protection scope of the present invention be departed from.Therefore, although be described in further detail invention has been by above embodiment, the present invention is not limited only to above embodiment, when not departing from the present invention's design, can also comprise other Equivalent embodiments more, and scope of the present invention is determined by appended right.
Claims (10)
1. a preparation method for negative active core-shell material, is characterized in that, comprises the following steps:
S1: by lithium chloride solution and alcohols solvent by volume 1 ~ 10:1000 mix, under stirring, add Titanium alkoxides, until there is white precipitate by Titanium alkoxides and alcohols solvent volume ratio 1 ~ 10:100;
S2: the solution sealing obtained by step S1, leaves standstill the solution obtained containing hydration titania microsphere;
S3: under stirring, be that 0.80 ~ 0.85:1 adds lithium acetate to described containing in the solution of hydration titania microsphere by the number ratio of lithium atom and titanium atom, wherein, the lithium atom in lithium chloride is contained in aforementioned proportion;
S4: under stirring, adds pyrroles as carbon source in the solution obtained in step S3 for 5 ~ 10:1 by the volume ratio of Titanium alkoxides and pyrroles, then adds oxidant and make pyrroles's in-situ polymerization;
S5: the solvent evaporation in the solution obtained by step S4, obtains the lithium titanate microballoon presoma that polypyrrole is coated;
S6: by the lithium titanate microballoon presoma that obtains under inert gas shielding, 700 ~ 900 DEG C of calcinings.
2. the preparation method of negative active core-shell material according to claim 1, is characterized in that, described alcohols solvent is methyl alcohol, ethanol, isopropyl alcohol, normal propyl alcohol, ethylene glycol or its mixing.
3. the preparation method of negative active core-shell material according to claim 1, is characterized in that, described lithium chloride solution and alcohols solvent by volume 4 ~ 8:1000 mix.
4. the preparation method of negative active core-shell material according to claim 1, is characterized in that, described Titanium alkoxides and alcohols solvent add Titanium alkoxides according to volume ratio 3 ~ 9:100.
5. the preparation method of negative active core-shell material according to claim 1, is characterized in that, described inert gas is nitrogen or rare gas, and the heating rate in calcination process is 1 ~ 5 DEG C/min, calcination time is 2 ~ 10h, and after calcining, temperature retention time is 2 ~ 10h, finally with the cold cooling of stove.
6. the preparation method of negative active core-shell material according to claim 1, is characterized in that, described Titanium alkoxides is isopropyl titanate or butyl titanate, more than purity 98wt.%.
7. the preparation method of negative active core-shell material according to claim 1, is characterized in that, the solvent evaporation in the solution that control temperature obtains for 40 ~ 80 DEG C thus by step S4.
8. the negative active core-shell material by preparation method's acquisition as described in the appended claim 1, it is characterized in that, described negative active core-shell material comprises the lithium titanate of kernel and is coated on the carbon on lithium titanate surface, and described negative active core-shell material is microspheroidal, and particle diameter is between 0.5 μm ~ 3 μm.
9. a negative active core-shell material according to claim 8, is characterized in that, described lithium titanate is spinel type lithium titanate.
10. a battery, comprising:
Positive pole;
Negative pole; And
Electrolyte,
It is characterized in that, described negative pole comprises the negative active core-shell material as described in any one of claim 8-9.
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| CN106784693A (en) * | 2016-12-26 | 2017-05-31 | 上海中聚佳华电池科技有限公司 | A kind of surface has the preparation method of the rich nitrogen nano lithium titanate electrode material of uniform carbon coating layer |
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| WO2019207616A1 (en) * | 2018-04-23 | 2019-10-31 | 株式会社村田製作所 | Lithium ion secondary battery |
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