CN104979544B - Negative electrode active material preparation method for material - Google Patents
Negative electrode active material preparation method for material Download PDFInfo
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- CN104979544B CN104979544B CN201510449769.6A CN201510449769A CN104979544B CN 104979544 B CN104979544 B CN 104979544B CN 201510449769 A CN201510449769 A CN 201510449769A CN 104979544 B CN104979544 B CN 104979544B
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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
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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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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation method of negative active core-shell material, comprise the following steps：Lithium chloride solution is mixed by volume with alcohols solvent, stirred, Titanium alkoxides are added by Titanium alkoxides and alcohols solvent volume ratio, until there is white precipitate；Above-mentioned solution sealing, stands the solution for obtaining the titania microsphere containing hydration；Under stirring, by lithium atom and titanium atom quantity ratio for 0.80~0.85 to it is described containing hydration titania microsphere solution in add lithium acetate；It is 5~10 by the volume ratio of Titanium alkoxides and pyrroles under stirring:1 adds pyrroles in the solution that above-mentioned steps are obtained, and adding oxidant makes pyrroles's in-situ polymerization；By the solvent evaporation in the solution obtained, presoma is obtained；By obtained presoma under inert gas shielding, in 700~900 DEG C of calcinings.
Description
Technical field
The present invention relates to a kind of negative electrode active material preparation method for material, more particularly to a kind of negative pole for lithium ion battery is lived
Property material preparation method.
Background technology
Spinel type lithium titanate (Li4Ti5O12) be a kind of lithium ion battery negative material of " zero strain ", i.e., in lithium ion
During embedded and abjection, its lattice structure hardly changes, therefore cyclical stability is excellent.Relative to lithium metal, titanium
The intercalation potential of sour lithium is about 1.55V, therefore will not cause the precipitation of lithium metal or Li dendrite, and with the side reaction of electrolyte
It is few, so that electrolyte is prevented in the reduction of electrode surface, it is not only safe, and coulombic efficiency is high, has extended cycle life.This
Outside, because spinelle skeleton structure has three-dimensional lithium ion diffusion admittance, lithium ion diffusion coefficient (2 × 10-8cm2/) than business
More than the high an order of magnitude of graphite negative material, therefore with potential excellent high rate capability.But spinel-type titanium
Sour lithium also has the deficiency of its own as lithium ion battery negative material, and such as high discharge platform can cause cell voltage low, so that
Make the specific energy of battery low；The conductance of its own is relatively low, and in high current charge-discharge, capacity attenuation is fast, and high rate performance is poor.
The effective way of lithium titanate anode material high rate performance is improved including the use of nanocrystalline material and carbon coating etc..Its
In, the use of nanocrystalline barium titanate lithium titanate cathode material is the contact area and less lithium ion using its larger electrode and electrolyte
Dilation angle improves charge-discharge velocity.But the same with other nano-electrode materials, the heap real density of nano lithium titanate is low, therefore
Although its charge-discharge velocity can be effectively improved, the specific energy of battery can be reduced simultaneously.Therefore, in order to improve heap real density, and
And be more prone to electrode slurrying and pole plate brushing, battery enterprise more favor in uniform particle sizes micron-size spherical lithium titanate bear
Pole material.Carbon coating is to improve one of very effective method of lithium titanate anode material high rate performance, but existing carbon coating side
Method is generally all that the method that gas phase or liquid phase are recycled after synthesis lithium titanate powdery carries out secondary cladding, and not only process is answered
It is miscellaneous, high energy consumption, and it is many because lithium titanate powdery disperses uneven, cause carbon coating effect undesirable.What is particularly generally used has
The method that machine carbohydrate hydro-thermal (such as glucose) reaction carries out carbon coating, not only yields poorly, poor controllability, and has different
Taste, and need a large amount of water or alcoholic solvent to wash etc., it is unfavorable for energy-conserving and environment-protective.
The content of the invention
The present invention provides a kind of negative electrode active material preparation method for material, can solve the above problems.
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 mixing, under stirring, by Titanium alkoxides
With alcohols solvent volume ratio 1~10:100 add Titanium alkoxides, until there is white precipitate；
S2：The solution sealing that step S1 is obtained, stands the solution for obtaining the titania microsphere containing hydration；
S3：It is 0.80~0.85 by the quantity ratio of lithium atom and titanium atom under stirring:1 contains hydration oxygen to described
Lithium acetate is added in the solution for changing titanium microballoon, wherein, the lithium atom in lithium chloride is contained in aforementioned proportion；
S4：It is 5~10 by the volume ratio of Titanium alkoxides and pyrroles under stirring:1 in the solution that step S3 is obtained
Pyrroles is added as carbon source, adding oxidant makes pyrroles's in-situ polymerization；
S5：Solvent evaporation in the solution that step S4 is obtained, obtains the lithium titanate microballoon presoma of polypyrrole cladding；
S6：By obtained lithium titanate microballoon presoma under inert gas shielding, in 700~900 DEG C of calcinings.
Further, the alcohols solvent is methanol, ethanol, isopropanol, normal propyl alcohol, ethylene glycol or its mixing.
Further, the lithium chloride solution and alcohols solvent by volume 4~8:1000 mixing.
Further, the Titanium alkoxides and alcohols solvent are according to volume ratio 3~9:100 add Titanium alkoxides.
Further, the Titanium alkoxides are isopropyl titanate or butyl titanate, more than purity 98wt.%.
Further, the pyrroles and Titanium alkoxides by volume 1：5~10 additions are made as carbon source, and using hydrogen peroxide
Trigger the in-situ polymerization of pyrroles for oxidant；
Further, the solvent in the solution for controlling temperature by 40~80 DEG C to obtain step S4 evaporates.
Further, described inert gas is that the heating rate in nitrogen or rare gas, and calcination process is 1~5
DEG C/min, the sintering soak time is 2~10h, finally with the cold cooling of stove.
The negative active core-shell material includes the lithium titanate of kernel and is coated on the carbon on lithium titanate surface, and the negative pole is lived
Property material be microspheroidal, particle diameter is between 0.5 μm~3 μm.
Further, the lithium titanate is spinel type lithium titanate.
The preparation method for the negative active core-shell material that the present invention is provided, it is molten in same presoma under room temperature and condition of normal pressure
The lithium titanate microballoon presoma of organic carbon source cladding is prepared in liquid, burning till with carbon coating in once calcining for lithium titanate is then made
Complete, so as to reach simplified technique, reduce cost, realize the purpose of mass production.In addition, the negative electrode active that the present invention is provided
Material and the battery containing the negative active core-shell material, also with higher specific capacity and preferable cycle performance.
Brief description of the drawings
Fig. 1 is the preparation method flow chart of negative active core-shell material provided in an embodiment of the present invention.
Fig. 2 is the stereoscan photograph for the negative active core-shell material that the embodiment of the present invention 1 is provided.
Fig. 3 is the X ray diffracting spectrum for the negative active core-shell material that the embodiment of the present invention 1 is provided.
Fig. 4 be the embodiment of the present invention 1 provide negative active core-shell material as negative electrode of lithium ion battery when, in the head of 2C speed
Cycle charge-discharge curve.
Fig. 5 be the embodiment of the present invention 1 provide negative active core-shell material as negative electrode of lithium ion battery when, in 2C speed
Cyclic curve.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.It is understood that this place is retouched
The specific embodiment stated is used only for explaining the present invention, rather than limitation of the invention.It also should be noted that, in order to just
Part related to the present invention rather than entire infrastructure are illustrate only in description, accompanying drawing.
Fig. 1 is refer to, 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 mixing, under stirring, by Titanium alkoxides
With alcohols solvent volume ratio 1~10:100 add Titanium alkoxides, until there is white precipitate；
S2：The solution sealing that step S1 is obtained, stands the solution for obtaining the titania microsphere containing hydration；
S3：It is 0.80~0.85 by the quantity ratio of lithium atom and titanium atom under stirring：1 contains hydration oxygen to described
Lithium acetate is added in the solution for changing titanium microballoon, wherein, the lithium atom in lithium chloride is contained in aforementioned proportion；
S4：It is 5~10 by the volume ratio of Titanium alkoxides and pyrroles under stirring:1 in the solution that step S3 is obtained
Pyrroles is added as carbon source, adding oxidant makes pyrroles's in-situ polymerization；
S5：Solvent evaporation in the solution that step S4 is obtained, obtains the lithium titanate microballoon presoma of polypyrrole cladding；
S6：By obtained lithium titanate microballoon presoma under inert gas shielding, in 700~900 DEG C of calcinings.
In step sl：The purpose for adding the lithium chloride solution is as the hydrolysis controlling agent for being Titanium alkoxides.It is preferred that,
Make the lithium chloride solution and alcohols solvent by volume 4~8:1000 mixing.The alcohols solvent can be methanol, ethanol,
Isopropanol, normal propyl alcohol, ethylene glycol or its mixing.Further, the Titanium alkoxides are isopropyl titanate or butyl titanate, purity
More than 98wt.%.It is preferred that, by the Titanium alkoxides and alcohols solvent volume ratio 3~9:100 add Titanium alkoxides.
In step s 2, solution step S1 obtained is sealed, and stands more than 10h, more than standing 20h preferably, from
And the solution of the titania microsphere containing hydration can be obtained.
In step s3, the purpose for adding excessive elemental lithium is to compensate for the volatilization of lithium during subsequent calcination.It is excellent
Choosing, be 0.85 by the quantity ratio of lithium atom and titanium atom:1 adds acetic acid into the solution of the titania microsphere containing hydration
Lithium.
In step s 4, the oxidant can be hydrogen peroxide or other can be catalyzed pyrroles polymerization material.The pyrrole
It can be 1 according to volume ratio to cough up with hydrogen peroxide:1~5 adds hydrogen peroxide.It is appreciated that the hydrogen peroxide can be single as pyrroles
The oxidant of body, makes it in 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 in the solution for controlling temperature by 40~80 DEG C to obtain step S4 evaporates.
In step s 6, described inert gas be the heating rate in nitrogen or rare gas, and calcination process be 1~
5 DEG C/min, calcination time is that soaking time is 2~10h after 2~10h, and calcining, finally with the cold cooling of stove, acquisition grey black
Negative active core-shell material.It is preferred that, can in 700~900 DEG C of temperature ranges calcine by steps, it is preferred that 700~750 DEG C,
2~12h is calcined respectively in 800~850 DEG C and 850~900 DEG C of grades, three temperature ranges, it is hereby achieved that more good
Crystallinity.
The negative active core-shell material obtained by above-mentioned preparation method includes the lithium titanate of kernel and is coated on lithium titanate
The carbon in face, and the negative active core-shell material is microspheroidal, particle diameter is between 0.5 μm~3 μm.Wherein, the lithium titanate is brilliant for point
Stone-type lithium titanate.
Embodiment 1：
0.4ml lithium chlorides (0.1M) solution is added into the ethanol that 100ml contents are 99.5wt.%, under stirring, plus
Enter 3ml isopropyl titanates, after there is white precipitate in solution, stop stirring；The solution is sealed, it is quiet to more than 20h, contained
The solution of hydrous titanium oxide microballoon；Under stirring, by lithium atom and titanium atom quantitative proportion 0.85：1 adds lithium acetate simultaneously
Fully dissolving；0.2ml pyrroles is added under stirring as carbon source, 1ml hydrogen peroxide (purity 28wt.%) is added, completes
The polymerization cladding of pyrroles；It is heated to 60 DEG C and stirs, evaporate solvent, obtains the lithium titanate microballoon presoma of polypyrrole cladding；
Above-mentioned presoma is calcined into 5h under inert gas shielding at 800 DEG C, wherein, heating rate is 5 DEG C/min, when being incubated after calcining
Between be 10h, finally with stove it is cold cooling i.e. obtain carbon coating lithium titanate microballoon.
Fig. 2 is refer to, from the figure, it can be seen that gained lithium titanate microballoon is black, illustrates to be successfully realized carbon coating, grain
Degree is uniform, and particle diameter is between 0.5-3 μm.Fig. 3 is refer to, Fig. 3 is that the X of the carbon coating lithium titanate microballoon prepared by embodiment 1 is penetrated
Ray diffraction diagram compose, it was demonstrated that synthesis be high-purity spinel type lithium titanate negative material.Fig. 4-5 are refer to, with prepared
Carbon coating lithium titanate microballoon prepares half-cell by positive pole of lithium metal to test carbon coating lithium titanate as negative electrode of lithium ion battery
The chemical property of microballoon, at 350mA/g (2C), discharge capacity reaches more than 130mAh/g first, is discharged after 200 circulations
Capacity stills remain in 118mAh/g or so.
Embodiment 2：
Substantially the same manner as Example 1, difference is, titanium source is used as instead of butyl titanate using isopropyl titanate.
Embodiment 3
Substantially the same manner as Example 1, difference is, solvent is used as instead of ethanol using methanol.
Embodiment 4
Substantially the same manner as Example 1, difference is, solvent is used as instead of ethanol using ethylene glycol.
Embodiment 5
Substantially the same manner as Example 1, difference is, solvent is used as instead of ethanol using isopropanol.
Embodiment 6
Substantially the same manner as Example 1, difference is, solvent is used as instead of ethanol using normal propyl alcohol.
It is demonstrated experimentally that embodiment 2-6 can obtain uniformly, the negative active core-shell material of height ratio capacity and stability.
Note, above are only presently preferred embodiments of the present invention and institute's application technology principle.It will be appreciated by those skilled in the art that
The invention is not restricted to specific embodiment described here, can carry out for a person skilled in the art it is various it is obvious change,
Readjust and substitute without departing from protection scope of the present invention.Therefore, although the present invention is carried out by above example
It is described in further detail, but the present invention is not limited only to above example, without departing from the inventive concept, also
Other more equivalent embodiments can be included, and the scope of the present invention is determined by scope of the appended claims.
Claims (7)
1. a kind of preparation method of negative active core-shell material, it is characterised in that comprise the following steps：
S1：By lithium chloride solution and alcohols solvent by volume 1~10:1000 mixing, under stirring, by Titanium alkoxides and alcohol
Class solvent volume is than 1~10:100 add Titanium alkoxides, until there is white precipitate；
S2：The solution sealing that step S1 is obtained, stands the solution for obtaining the titania microsphere containing hydration；
S3：It is 0.80~0.85 by the quantity ratio of lithium atom and titanium atom under stirring：1 contains hydrous titanium oxide to described
Lithium acetate is added in the solution of microballoon, wherein, the lithium atom in lithium chloride is contained in aforementioned proportion；
S4：It is 5~10 by the volume ratio of Titanium alkoxides and pyrroles under stirring:1 adds in the solution that step S3 is obtained
Pyrroles is as carbon source, and adding oxidant makes pyrroles's in-situ polymerization；
S5：Solvent evaporation in the solution that step S4 is obtained, obtains the lithium titanate microballoon presoma of polypyrrole cladding；
S6：By obtained lithium titanate microballoon presoma under inert gas shielding, in 700~900 DEG C of calcinings.
2. the preparation method of negative active core-shell material according to claim 1, it is characterised in that the alcohols solvent is first
Alcohol, ethanol, isopropanol, normal propyl alcohol, ethylene glycol or its mixing.
3. the preparation method of negative active core-shell material according to claim 1, it is characterised in that the lithium chloride solution and alcohol
Class solvent by volume 4~8:1000 mixing.
4. the preparation method of negative active core-shell material according to claim 1, it is characterised in that the Titanium alkoxides and alcohols are molten
Agent is according to volume ratio 3~9:100 add Titanium alkoxides.
5. the preparation method of negative active core-shell material according to claim 1, it is characterised in that described inert gas is nitrogen
Heating rate in gas or rare gas, and calcination process is 1~5 DEG C/min, and calcination time is 2~10h, when being incubated after calcining
Between be 2~10h, finally with the cold cooling of stove.
6. the preparation method of negative active core-shell material according to claim 1, it is characterised in that the Titanium alkoxides are isopropanol
Titanium or butyl titanate, more than purity 98wt.%.
7. the preparation method of negative active core-shell material according to claim 1, it is characterised in that it is 40~80 DEG C to control temperature
So that the solvent evaporation in the solution that step S4 is obtained.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP3787073A4 (en) * | 2018-04-23 | 2022-05-18 | Murata Manufacturing Co., Ltd. | Lithium ion secondary battery |
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| CN106784693B (en) * | 2016-12-26 | 2020-07-24 | 上海中聚佳华电池科技有限公司 | Preparation method of nitrogen-rich nano lithium titanate electrode material with uniform carbon coating layer on surface |
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| CN102569764B (en) * | 2010-12-28 | 2015-05-20 | 清华大学 | Lithium titanate composite material, preparation method thereof and lithium ion battery |
| CN102633300A (en) * | 2011-12-07 | 2012-08-15 | 天津市贝特瑞新能源材料有限责任公司 | Carbon-coated lithium titanate cathode material as well as preparation method and applications thereof |
| CN102969492B (en) * | 2012-12-04 | 2014-11-12 | 广州有色金属研究院 | Carbon-coated doping modified lithium titanate and preparation method thereof |
| CN103456939B (en) * | 2013-07-24 | 2015-12-23 | 湖南大学 | Metatitanic acid is utilized to prepare the method for the coated lithium titanate of lithium ion battery negative material carbon |
| CN104282906B (en) * | 2014-09-19 | 2017-04-12 | 清华大学深圳研究生院 | Lithium titanate material of micro-nano structure and preparation method of lithium titanate material |
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