CN105932238A - Preparation method of lithium ion battery negative electrode material lithium titanate coated by spherical rare earth metal oxide - Google Patents

Preparation method of lithium ion battery negative electrode material lithium titanate coated by spherical rare earth metal oxide Download PDF

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Publication number
CN105932238A
CN105932238A CN201610306543.5A CN201610306543A CN105932238A CN 105932238 A CN105932238 A CN 105932238A CN 201610306543 A CN201610306543 A CN 201610306543A CN 105932238 A CN105932238 A CN 105932238A
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preparation
earth metal
lithium
lithium titanate
spherical rare
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黄玉代
张萍
贾殿赠
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Xinjiang University
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • 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
    • 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
    • H01M4/624—Electric conductive fillers
    • 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 lithium ion battery negative electrode material lithium titanate coated by a spherical rare earth metal oxide. The method comprises the following steps: dissolving solid lithium salt and corresponding cerium salt and erbium salt into a certain amount of distilled water, adding the mixed solution in an ethanol solution containing a titanium source, stirring the solution at a room temperature, obtaining a mixed precursor through drying, and baking the precursor at a certain temperature to obtain the lithium ion battery negative electrode material Li<4>Ti<5>O<12>@CeO<2>, Li<4>Ti<5>O<12>@Er<2>O<3>. Through the adoption of the method disclosed by the invention, the problem that the Li<4>Ti<5>O<12> is bad in charging/discharging performance at a high-rate current is improved, and the method is simple in process, free from polluting environment and wide in applicable range.

Description

A kind of lithium ionic cell cathode material lithium titanate of spherical rare-earth metal-oxide cladding Preparation method
Technical field
The invention belongs to high-energy battery technical field, particularly synthesizing lithium ion battery negative material technical field.
Background technology
Lithium ion battery negative material Li4Ti5O12Almost without change in volume during Lithium-ion embeding, abjection, follow Ring good stability, is referred to as " zero strain " material.In charge and discharge process, the stability of structure, makes Li4Ti5O12Become pole and have latent The lithium ion battery electrode material of power.Li4Ti5O12Discharge platform is 1.55 V, and higher than most of organic electrolytes, it is for carbon Having the advantage in terms of safety for material, being therefore considered is very promising negative pole in terms of power-type lithium ion battery Material.
Li4Ti5O12Electronic conductivity and ionic conductance are relatively low, affect its actual chemical property, particularly high magnification Discharge performance, becomes it and realizes the biggest obstacle of industrial applications.
Control particle diameter and the pattern of material: the material of (1) nanostructured is beneficial to electrolyte permeability, accelerate electrochemical reaction, Wherein, ball shape structure tend to the most even completely, this structure can be electrode material and electrolyte contact provide effective area, add Fast lithium ion transport, improves chemical property.(2) its electronic conductivity is improved by methods such as surface clad oxides And ionic conductance, improve its discharge capacity under high current density.
At present, Li4Ti5O12Main preparation method has high temperature solid-state method, and this method is simple and convenient, and condition is easily controllable, just In realizing industrialization, but this method mainly uses mechanical process to carry out refinement and the mixing of raw material, and mixing uniformity is limited, nothing Method ensures the uniformity of granule, is easily introduced impurity, and needs to calcine the most for a long time, adds cost.Sol-gel process Equipment is simple, and process is easily controllable, and can prepare high chemical uniformity and the material of high chemical purity, but this method generally adds Enter chelating agent, the ratio between various raw material need to be regulated, the longest.Hydro-thermal method can be according to reaction temperature and response time Control the pattern of sample and structure, but this method carried out under conditions of High Temperature High Pressure, safety it cannot be guaranteed that.Coprecipitation is First preparing the cationic solution of stoichiometric proportion, add precipitant and obtain mixed precipitation presoma, filtration washing is dried and lithium Source mixed calcining, solution concentration, mixing speed, precipitation temperature, acidity and response time are close with particle diameter with the pattern of end product Cut is closed, and this method is simple to operate, and equipment is simple and direct, and the material homogeneity prepared is preferable.
Chinese patent CN104993107A, is prepared for a kind of lithium ion battery negative material Li4Ti5O12/rutile- TiO2, particularly as follows: 1) and under room temperature, by LiOH H2O is placed in ethanol, after stirring mixing, adds butyl titanate, drying condition Under, react 10-12h, obtain reactant liquor；2) in reactant liquor, add deionized water, stir 1-2min, obtain milky white solution, by institute State milky white solution and move in reactor, 170-180 DEG C of reaction 34-37h, centrifugation, collect precipitation, washing with alcohol, 70-80 DEG C vacuum drying 6-8h, obtain product presoma；3) described product presoma is placed in air atmosphere, 490-700 DEG C of calcining 6- 7h, naturally cools to room temperature, grinds, obtains target product；The lithium ion battery negative material being prepared from by the method is squama Lamellar spinel-type Li4Ti5O12/rutile-TiO2Composite, is keeping Li4Ti5O12On the premise of good characteristic, not only Realize solving the security hidden trouble of embedding lithium material with carbon element, and particular, it is important that its sclay texture further increases The specific surface area of material, and then improve the chemical property of material.
Chinese patent CN102208612A, it is provided that a kind of high-magnification lithium ion powder battery cathode TiO2Cladding Li4Ti5O12The synthetic method of composite, the method is on the basis of high-energy ball milling auxiliary solid phase reaction method, to Li4Ti5O12Table Face carries out TiN cladding in situ, and the TiAlN thin film being formed in situ inhibits Li4Ti5O12Granule is reunited in high-temperature process, from And obtain nano-scale particle, more restricted roasting, TiN is changed into TiO2Obtain final product.This method reduces Conventional solid-state method sintering Li4Ti5O12Temperature, prepare diameter of particle little, even particle size distribution, substantially increase Li4Ti5O12 The performance of negative material.This materials application, in lithium ion power cell cathode, shows the fast charging and discharging performance of excellence, 10C Multiplying power (electric discharge in 6 minutes) discharge capacity is still up to 155 mAh g−1Above.
Chinese patent CN105206815A, it is provided that a kind of carbon cladding Li4Ti5O12-TiO2The system of/Sn nano composite material Preparation Method.Wherein, Li4Ti5O12Content be 19wt%～65wt%, TiO2Content be 11wt%～57wt%, the content of Sn For 23wt%～49wt%；The content of carbon coating layer is 1wt%～24wt%.The composite that the present invention prepares plays Monodimension nanometer material Li4Ti5O12-TiO2Matrix Electrochemical lithiation process change in volume is little, metal Sn height ratio capacity and carbon cladding Layer improves the synergism such as electronic conductance and ion permeability, has shown the chemical property of excellence, at electric automobile and fast Fill the fields such as the lithium ion battery in electronic product to have broad application prospects.
Sivashanmugam etc. [1] are prepared for Li with high temperature solid-state polishing4Ti5O12/ Sn nano-complex, shows Good chemical property.(S.G. A. Sivashanmugam, R. Thirunakaran, C. Nithya, S. Prema. Novel Li4Ti5O12/Sn nano-composites as anode material for lithium ion batteries. Mater. Res. Bull 2011, 46: 492-500).Ag not only possesses high electronic conductivity, and Being prone to prepared, the thermal decomposition of silver salt can obtain silver, it is not necessary to adds reducing agent or calcines in reducing atmosphere.Erdas etc. [2] use Sol-gel process is prepared for Ag/Li4Ti5O12Complex, discharge capacity is 170 mAh g when electric current density 1 C first−1。 (S.M.O. A. Erdas, D. Nalci, Me. O. Guler, H. Akbulut. Novel Ag/Li4Ti5O12 binary composite anode electrodes for high capacity Li-ion batteries. Surf. Coat. Technol 2015, 271: 136-140).Zhang etc. [3] have synthesized Li2ZrO3The Li of cladding4Ti5O12Complex. Li2ZrO3Clad is improving Li+The aspect of diffusion serves positive effect so that cladding sample shows good times Rate performance and cycle performance.( Y.L. H. Zhang, T. Wang, Y. Yang, S. J. Shi, G. Yang. Li2ZrO3-coated Li4Ti5O12 with nanoscale interface for high performance lithium- ion batteries. Appl. Surf. Sci. 2016, 368: 56-62)。
The present invention is according to Li4Ti5O12Low electronic conductivity and ionic conductance, select rare-earth oxide CeO2、 Er2O3As oxide coated, first Application is in Li4Ti5O12In negative material, synthesize Li4Ti5O12@CeO2、Li4Ti5O12@ Er2O3Covering material.
Summary of the invention
It is an object of the invention to provide a kind of simple process, environmental pollution is less, applied widely, have excellent high magnification The preparation method of the lithium titanate of the spherical rare-earth metal-oxide cladding of performance.The method be by solid-state lithium salts and corresponding cerium salt, Erbium salt is dissolved in a certain amount of distilled water, this mixed solution is added the ethanol solution containing titanium source, is stirred at room temperature latter 100 DEG C It is dried and prepares mix precursor.The roasting at a certain temperature of this presoma is i.e. obtained the metatitanic acid of rare-earth oxide cladding Lithium.
The present invention prepares the preparation of the lithium ionic cell cathode material lithium titanate of a kind of spherical rare-earth metal-oxide cladding Step is as follows:
By appropriate LiOH H2O adds in distilled water, after dissolving, adds Ce (NO3)3·6H2O or Er2(SO4)3·8H2O, will stir The solution mixed joins the ethanol solution containing titanium source, reacts, and obtains Li4Ti5O12@MO(M=Ce4+, Er3+) forerunner Body.
After the presoma of preparation is dried, by its 600 DEG C of calcining 5 h in Muffle furnace.
In Muffle furnace, naturally cool to room temperature, prepare this sample.
The method of the present invention is particularly suited for coprecipitation and prepares lithium ion battery negative material.
The present invention prepares Li4Ti5O12@CeO2For pale yellow powder, this material is spherical in shape, Li4Ti5O12@Er2O3For pink colour powder End, this material is spherical in shape.
Material electrochemical performance is preferable: Li4Ti5O12@CeO2(0.1525 g) discharge capacity first under 10 C electric current densities It is 161.9 mAh g-1, after 180 charge and discharge cycles, discharge capacity is still 152.1 mAh g-1, multiplying power under 40 C multiplying powers Capacity is 128.4 mAh g-1；Li4Ti5O12@Er2O3(0.2147 g) under 20 C electric current densities first discharge capacity be 192.1 mAh g-1, after 200 charge and discharge cycles, discharge capacity remains to be maintained at 154.3 mAh g-1, rate capability under 30 C multiplying powers Up to 183 mAh g-1(Li under 1 C4Ti5O12Theoretical capacity be 175 mAh g-1).
Advantages of the present invention:
Spherical Li is prepared in the co-precipitation of the present invention4Ti5O12@CeO2、Li4Ti5O12@Er2O3Method, improve Li4Ti5O12Greatly The problem of charge-discharge performance difference under electric current density, and have that technique is simple, environmentally safe or of low pollution, applied widely etc. Advantage.Li4Ti5O12@CeO2、Li4Ti5O12@Er2O3Excellent chemical property and easy preparation method, carry for business application Having supplied may.
Accompanying drawing explanation
Fig. 1 is prepared Li4Ti5O12@CeO2(0.1525 g) transmission electron microscope picture.Fig. 2 is prepared Li4Ti5O12@CeO2 (0.1525 g) cyclic curve under 10 C.Fig. 3 is prepared Li4Ti5O12@CeO2(0.1525 g) 0.2 C, 1 C, 2 C, 5 C, 10 C, 20 C, 30 C, the curve of double curvature of 40 C.
Fig. 4 is prepared Li4Ti5O12@Er2O3(0.2147 g) transmission electron microscope picture.Fig. 5 is prepared Li4Ti5O12@ Er2O3(0.2147 g) cyclic curve under 20 C.Fig. 6 is prepared Li4Ti5O12@Er2O3(0.2147 g) 0.5 C, 1 C, 5 C, 10 C, 20 C, the curve of double curvature of 30 C.
Detailed description of the invention
12 mL TBT are added in dehydrated alcohol and stir by the preparation of compound precursor stoichiometrically Li:Ti=4.03:5 Mix.By 1.208 g LiOH H2O and different amounts of Ce (NO3)3·6H2O、Er2(SO4)3·8H2O adds in distilled water, stirring Make it be completely dissolved, then this solution is added the butyl titanate ethanol solution being stirred continuously, stir 24 h, then do for 100 DEG C Dry prepared presoma.Ce(NO3)3·6H2O addition is respectively 0 g, 0.7624 g, 0.1525 g, 0.3050 g, 0.4574 g With 0.6099 g, Er2(SO4)3·8H2O addition is respectively 0 g, 0.1073 g, 0.2147 g, 0.3220 g, 0.4294 g With 0.5367 g.
Li4Ti5O12@CeO2、Li4Ti5O12@Er2O3Preparation be 5 DEG C/min by above-mentioned presoma with heating rate, 600 At DEG C, Muffle kiln roasting 5 hours, i.e. prepare Li4Ti5O12@CeO2、Li4Ti5O12@Er2O3Lithium ion battery negative material.
Use Li of the present invention4Ti5O12@CeO2、Li4Ti5O12@Er2O3Composite materials is as button cell material, dress Being made into button 2032 battery, button type battery carries out under 10 C under room temperature, 20 C electric current densities respectively, in 1-3 V voltage range Electrochemical property test: Li4Ti5O12@CeO2(0.1525 g) under 10 C electric current densities first discharge capacity be 161.9 mAh g-1, after 180 charge and discharge cycles, discharge capacity is still 152.1 mAh g-1, under 40 C multiplying powers, rate capability is 128.4 mAh g-1；Li4Ti5O12@Er2O3(0.2147 g) under 20 C electric current densities first discharge capacity be 192.1 mAh g-1, after 200 charge and discharge cycles, discharge capacity remains to be maintained at 154.3 mAh g-1, under 30 C multiplying powers, rate capability is up to 183 mAh g-1(Li under 1 C4Ti5O12Theoretical capacity be 175 mAh g-1).

Claims (6)

1. a preparation method for the lithium ionic cell cathode material lithium titanate of spherical rare-earth metal-oxide cladding, its feature exists In:
(1) by LiOH H2O adds in distilled water, and stirring makes it be completely dissolved, and then this solution add the metatitanic acid being stirred continuously Butyl ester ethanol solution, stirs 24 h, is dried (Li:Ti mol ratio is 4.03:5), obtain Li4Ti5O12Presoma;
(2) by appropriate LiOH H2O adds in distilled water, after dissolving, adds Ce (NO3)3·6H2O or Er2(SO4)3·8H2O, will The solution being stirred joins the ethanol solution containing titanium source, reacts, and obtains Li4Ti5O12@MO(M=Ce4+, Er3+) front Drive body;
(3) after the presoma prepared is dried, by its 600 DEG C of calcining 5 h in Muffle furnace;
(4) in Muffle furnace, naturally cool to room temperature, prepare this sample.
2. according to the preparation of the lithium ionic cell cathode material lithium titanate of a kind of spherical rare-earth metal-oxide cladding described in right 1 Method, it is characterised in that step 1) uses C16H36O4Ti, LiOH H2O is as raw material.
3. according to the preparation of the lithium ionic cell cathode material lithium titanate of a kind of spherical rare-earth metal-oxide cladding described in right 1 Method, it is characterised in that step 2) use C16H36O4Ti, LiOH H2O, Ce (NO3)3·6H2O or Er2(SO4)3·8H2O makees For raw material.
4. according to the preparation of the lithium ionic cell cathode material lithium titanate of a kind of spherical rare-earth metal-oxide cladding described in right 1 Method, it is characterised in that step 2) by a step Co deposited synthesis spherical structure lithium ion battery negative material Li4Ti5O12@ MO(M=Ce4+, Er3+) presoma.
5. according to the preparation of the lithium ionic cell cathode material lithium titanate of a kind of spherical rare-earth metal-oxide cladding described in right 1 Method, it is characterised in that step 3) is 600 DEG C of calcining 5 h in Muffle furnace.
6. according to the preparation of the lithium ionic cell cathode material lithium titanate of a kind of spherical rare-earth metal-oxide cladding described in right 1 Method, it is characterised in that step 4) naturally cools to room temperature in Muffle furnace, prepares this sample.
CN201610306543.5A 2016-05-11 2016-05-11 Preparation method of lithium ion battery negative electrode material lithium titanate coated by spherical rare earth metal oxide Pending CN105932238A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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CN107068995A (en) * 2017-02-15 2017-08-18 浙江大学 A kind of new precipitated oxide coated lithium ion battery positive electrode in situ and preparation method and application
CN115301411A (en) * 2022-07-20 2022-11-08 浙江菲达环保科技股份有限公司 Self-heating ash-free discharge electrode and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107068995A (en) * 2017-02-15 2017-08-18 浙江大学 A kind of new precipitated oxide coated lithium ion battery positive electrode in situ and preparation method and application
CN107068995B (en) * 2017-02-15 2019-12-27 浙江大学 In-situ precipitated oxide coated lithium ion battery positive electrode material and preparation method and application thereof
CN115301411A (en) * 2022-07-20 2022-11-08 浙江菲达环保科技股份有限公司 Self-heating ash-free discharge electrode and preparation method thereof
CN115301411B (en) * 2022-07-20 2024-03-26 浙江菲达环保科技股份有限公司 Self-heating non-ash-sticking discharge electrode and preparation method thereof

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