CN105845924B - The preparation method of the lithium titanate nanometer sheet of Fluorin doped - Google Patents

The preparation method of the lithium titanate nanometer sheet of Fluorin doped Download PDF

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CN105845924B
CN105845924B CN201610342414.1A CN201610342414A CN105845924B CN 105845924 B CN105845924 B CN 105845924B CN 201610342414 A CN201610342414 A CN 201610342414A CN 105845924 B CN105845924 B CN 105845924B
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lithium
nanometer sheet
lithium titanate
fluorin doped
titanate
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CN105845924A (en
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陈铭
张鹏飞
吴倩卉
刁国旺
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Yangzhou 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
    • H01M4/48—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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C01G23/005—Alkali titanates
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • 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 preparation method of the lithium titanate nanometer sheet of Fluorin doped, the invention belongs to lithium-ion battery energy material production technical fields, synthesize Li by hydro-thermal method4Ti5O12Nanometer sheet can significantly increase the contact area of material and electrode, and then can be improved the chemical property of material.The doping of fluorine atom makes fluorine atom that lattice oxygen atom in part be replaced to form Ti-F key, in order to guarantee the charge conservation of material, has part Ti since the introducing of F makes the charge disequilibrium of material according to charge conservation4+It is converted into Ti3+, to increase the electric conductivity of material.It is adulterated by F, the uniform product appearance of acquirement, better crystallinity degree, large specific surface area, chemical property is significantly improved under high magnification.

Description

The preparation method of the lithium titanate nanometer sheet of Fluorin doped
Technical field
The invention belongs to lithium-ion battery energy material production technical fields.
Background technique
With the aggravation of global energy crisis and environmental pollution, the development and application of new energy are imperative.Energy storage at present What field was widely used is secondary cell, lithium ion battery as one such, had extended cycle life with it, specific capacity is big, The many advantages such as memory-less effect and operating voltage height, no pollution to the environment are widely used in mobile phone, digital camera, laptop computer Etc. in all kinds of Miniature Portable Units.Nowadays various commercialized lithium ion battery negative materials be all based on Carbon materials, But carbon does the lithium ion battery of cathode that there is drawbacks in application, for example, Li dendrite is easily precipitated when overcharge, causes electricity Pond short circuit, influences the security performance of lithium battery；Easily formed SEI film and cause first charge-discharge efficiency lower, irreversible capacity compared with Greatly；The platform voltage of carbon material is lower (close to lithium metal), and easily causes the decomposition of electrolyte；Lithium ion be embedded in, Volume change is larger during abjection, and cyclical stability difference is to bring security risk.In order to solve the lithium battery that carbon does cathode Defect, safe and reliable lithium ion battery negative material development is critically important.In recent years, various negative electrode materials are in basic research side Face has also obtained a degree of development, such as lithium titanate material, tin-based material, silica-base material, metal oxide materials nitride Material etc..
Lithium titanate (Li4Ti5O12, LTO) and as the negative electrode material of lithium ion battery a kind of receive more and more researchs And concern, there is huge researching value and application prospect as lithium-ion-power cell.Li4Ti5O12The electricity of opposite lithium electrode Position is 1.55 V, and theoretical specific capacity is 175 mAh/g, is reported in a large amount of document, the actual specific capacity of the material has reached 150 ~170 mAh/g.Li4Ti5O12Electron conduction is poor, but has preferable Li+Ionic conductivity, as external Li+Ion insertion When into spinel structure, with Li+The increase of ion embedded quantity, Li4Ti5O12It is good that electric conductivity is gradually transformed by insulator Good Li7Ti5O12, the Li that generates in process of intercalation7Ti5O12Crystal structure and Li4Ti5O12Identical is also spinel structure. Li4Ti5O12Potential it is higher than pure metal lithium, be not likely to produce lithium dendrite arm, for ensure lithium battery safety provide the foundation, Li4Ti5O12As lithium ion battery negative material, in charge and discharge, the insertion and deintercalation of lithium ion to the structure of material almost It does not influence, is kind of " a zero strain material ", Li4Ti5O12These advantages of material decide it as negative electrode of lithium ion battery material Material has a good application prospect.
Conductive capability is an important physical properties of solid material, and measurement index is conductivity.Li4Ti5O12It is one The material that kind almost insulate, leading to it, capacity attenuation is fast under high magnification, and performance is poor.Li simultaneously4Ti5O12Granular size and electricity Solution liquid contact area is also an important factor for influencing its high rate capability.
Summary of the invention
It is an object of the invention to propose a kind of lithium ion battery negative material --- the lithium titanate nanometer sheet of Fluorin doped Preparation method.
The technical scheme is that: by Lithium hydroxide monohydrate, butyl titanate, lithium fluoride and dehydrated alcohol in dry ring It after being sufficiently mixed under border, adds deionized water and is vigorously stirred 0.5h, be subsequently placed in 180 in polytetrafluoroethylene (PTFE) stainless steel cauldron DEG C hydro-thermal reaction 36h, obtains Fluorin doped lithium titanate predecessor；By the predecessor in tube furnace, calcined under argon atmosphere Obtain the lithium titanate nanometer sheet (F-Li of doping fluorine4Ti5O12NSs, F-LTO NSs).
The present invention synthesizes Li by hydro-thermal method4Ti5O12Nanometer sheet can significantly increase the contact surface of material and electrode Product, and then can be improved the chemical property of material.The doping of fluorine atom makes fluorine atom that lattice oxygen atom in part be replaced to form Ti- F key, according to charge conservation, since the introducing of F has the charge disequilibrium of material in order to guarantee the charge conservation of material Part Ti4+It is converted into Ti3+, to increase the electric conductivity of material.It is adulterated by F, the uniform product appearance of acquirement, crystallinity Good, large specific surface area, chemical property is significantly improved under high magnification.
Further, the mass ratio that feeds intake of Lithium hydroxide monohydrate of the present invention, butyl titanate and lithium fluoride is 1: 0.60~0.9: 0.005~0.015.Because lithium titanate predecessor, during calcining, lithium source has different degrees of loss, Therefore Lithium hydroxide monohydrate should be excessive, so as to synthesize pure lithium titanate.The amount addition of lithium fluoride is excessive, can make flake lithium titanate Surface area reduce, reduced with the contact area of electrolyte, the performance of battery caused to decline；Too small, meeting is added in the amount of lithium fluoride So that F is replaced part O reduction, reduces insulation Ti4+It is converted into well conducting Ti3+Quantity, cause the performance of battery poor； Suitable lithium fluoride, which is added, can either make F replace part O, make the Ti that insulate4+It is converted into well conducting Ti3+, and lithium titanate can be made Laminated structure is kept, increases the contact area of lithium titanate material and electrolyte, and then improve chemical property.
The hydrothermal temperature in polytetrafluoroethylene (PTFE) stainless steel cauldron is 150~220 DEG C, the reaction time 12~ 48h.Temperature is lower than 150 DEG C, cannot get reaction product；Temperature is higher than 220 DEG C, reaches the limit of hydro-thermal reaction, therefore selects hydro-thermal Reaction temperature is 150~220 DEG C.
The calcination temperature condition is 500~800 DEG C, and calcination time is 2~8h.Calcination temperature is lower than 500 DEG C, obtains Lithium titanate crystal form is bad, causes the performance of battery poor；When calcination temperature is higher than 800 DEG C, although the crystal form of lithium titanate is fine, It is since temperature is excessively high, flake lithium titanate thickness increases, and surface area is less, reduces with the contact area of electrolyte, leads to battery Performance decline.So 500~800 DEG C are optimum temperature range.
Detailed description of the invention
Fig. 1 is the Li of synthesis4Ti5O12The transmission electron microscope picture of nanometer sheet.
Fig. 2 is the F doping Li of synthesis4Ti5O12The transmission electron microscope picture of nanometer sheet.
Fig. 3 is the Li of synthesis4Ti5O12Nanometer sheet and F adulterate Li4Ti5O12The X-ray powder diffraction comparison diagram of nanometer sheet.
Fig. 4 is Li4Ti5O12Nanometer sheet and F adulterate Li4Ti5O12The x-ray photoelectron spectroscopy figure of nanometer sheet.
Fig. 5 is Li4Ti5O12Nanometer sheet and F adulterate Li4Ti5O12The x-ray photoelectron spectroscopy figure of nanometer sheet.
Fig. 6 is Li4Ti5O12Nanometer sheet and F adulterate Li4Ti5O12The cycle performance under different current densities of nanometer sheet Figure.
Fig. 7 is Li4Ti5O12Nanometer sheet and F adulterate Li4Ti5O12Nanometer sheet in 2Ag-1Cyclicity under current density It can figure.
Specific embodiment
One, in order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments to this hair It is bright to be described in detail.
Embodiment 1
Take 0.168 g Lithium hydroxide monohydrate, 1.7 g butyl titanates, 0.015 g lithium fluoride, 20 mL dehydrated alcohols set In the three-necked flask of 100 mL, is stirred 12 hours under dry environment, add 25mL deionized water and be vigorously stirred 0.5 h Afterwards, opalescent solution is placed in 180 DEG C of 36 h of hydro-thermal reaction in the polytetrafluoroethylene (PTFE) stainless steel cauldron of 50mL.It is heavy to take out White powder wash three times product with dehydrated alcohol in a kettle, is centrifugated, 60 DEG C of 8 h of drying obtain fluorine and mix in an oven Miscellaneous lithium titanate nanometer sheet predecessor.Predecessor is placed in argon atmosphere protection 6 h of lower 600 DEG C of calcinings in tube furnace and obtains fluorine The lithium titanate nanometer sheet of doping.
Embodiment 2
Take 0.189 g Lithium hydroxide monohydrate, 1.7 g butyl titanates, 0.010 g lithium fluoride, 20 mL dehydrated alcohols set It in the three-necked flask of 100mL, is stirred 12 hours under dry environment, adds 25 mL deionized waters and be vigorously stirred 0.5h Afterwards, opalescent solution is placed in 160 DEG C of 20 h of hydro-thermal reaction in the polytetrafluoroethylene (PTFE) stainless steel cauldron of 50mL.It is heavy to take out White powder wash three times product with dehydrated alcohol in a kettle, is centrifugated, 60 DEG C of 8 h of drying obtain fluorine and mix in an oven Miscellaneous lithium titanate nanometer sheet predecessor.Predecessor is placed in argon atmosphere protection 5 h of lower 800 DEG C of calcinings in tube furnace and obtains fluorine The lithium titanate nanometer sheet of doping.
Embodiment 3
Take 0.204 g Lithium hydroxide monohydrate, 1.7 g butyl titanates, 0.005 g lithium fluoride, 20 mL dehydrated alcohols set It in the three-necked flask of 100 mL, is stirred 12 hours under dry environment, adds 25 mL deionized waters and be vigorously stirred 0.5 After h, opalescent solution is placed in 200 DEG C of 24 h of hydro-thermal reaction in the polytetrafluoroethylene (PTFE) stainless steel cauldron of 50 mL.It takes out White powder wash three times deposition with dehydrated alcohol in a kettle, is centrifugated, 60 DEG C of dry 8h obtain fluorine and mix in an oven Miscellaneous lithium titanate nanometer sheet predecessor.Predecessor is placed in argon atmosphere protection 4 h of lower 700 DEG C of calcinings in tube furnace and obtains fluorine The lithium titanate nanometer sheet of doping.
Two, verification the verifying results:
Fig. 1 is the transmission electron microscope picture of the pure lithium titanate nanometer sheet of above each example synthesis；Fig. 2 is that the fluorine of above each example synthesis is mixed The transmission electron microscope picture of miscellaneous metatitanic acid lithium piece.Comparison diagram 1,2 is as it can be seen that product smooth in appearance prepared by each method, and pattern is uniform, nanometer About 300 nm of piece diameter, about 10 nm of thickness, better crystallinity degree.
Fig. 3 is the pure lithium titanate of preparation and the X-ray powder diffraction comparison diagram of Fluorin doped lithium titanate.Wherein, curve a generation The pure lithium titanate X-ray powder diffraction figure of table；Curve b represents Fluorin doped lithium titanate X-ray powder diffraction figure.It can from Fig. 3 Out, crystalline structure of the doping of fluorine without influence lithium titanate.
Fig. 4,5 are respectively the x-ray photoelectron spectroscopy that pure lithium titanate and Fluorin doped lithium titanate are prepared using the method for the present invention Figure.Curve a represents the x-ray photoelectron spectroscopy figure of pure lithium titanate, and curve b represents the x-ray photoelectron energy of Fluorin doped lithium titanate Spectrogram.
Three, application effect:
As shown in fig. 7, the method for the present invention to be prepared pure lithium titanate and Fluorin doped lithium titanate is assembled into filling for button cell The comparison of discharge cycle performance figure, curve a represent the charge-discharge performance figure of pure lithium titanate nanometer sheet, and curve b represents fluorine and mixes The charge-discharge performance figure of miscellaneous lithium titanate nanometer sheet.
Lithium ion battery composed by lithium titanate nanometer sheet and Fluorin doped lithium titanate nanometer sheet to the preparation of top method, warp The chemical property of detection lithium titanate battery is significantly improved than traditional Solid phase synthesis lithium titanate, Fluorin doped lithium titanate Chemical property got back further raising.And this process is simple, easy to operate, at low cost, nonhazardous, yield There is height certain potential using value can be further improved the electrification of battery by improving to battery preparation technique Learn performance.

Claims (1)

1. the preparation method of the lithium titanate nanometer sheet of Fluorin doped, it is characterised in that: by Lithium hydroxide monohydrate, butyl titanate, fluorine After change lithium and dehydrated alcohol are sufficiently mixed under dry environment, add deionized water and be vigorously stirred 0.5h, be subsequently placed in poly- Hydro-thermal reaction in tetrafluoroethene stainless steel cauldron obtains Fluorin doped lithium titanate predecessor；By the predecessor in tube furnace, Calcining obtains the lithium titanate nanometer sheet of doping fluorine under argon atmosphere；
The Lithium hydroxide monohydrate, butyl titanate and lithium fluoride the mass ratio that feeds intake be 1: 0.60~0.9: 0.005~ 0.015；
The hydrothermal temperature in polytetrafluoroethylene (PTFE) stainless steel cauldron is 150~220 DEG C, 12~48h of reaction time；
The calcination temperature condition is 500~800 DEG C, and calcination time is 2~8h.
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CN106532011A (en) * 2016-12-22 2017-03-22 山东精工电子科技有限公司 Preparation method for novel lithium titanate material
CN106935831A (en) * 2017-03-31 2017-07-07 深圳市国创新能源研究院 A kind of lithium titanate anode material for suppressing flatulence and its preparation method and application
CN108288703B (en) * 2018-01-31 2021-02-05 中南大学 Preparation method and application of graphene-coated fluorine-doped lithium titanate nanowire
CN108539183B (en) * 2018-05-14 2020-09-25 山东玉皇新能源科技有限公司 Lithium titanate composite material and preparation method thereof, lithium ion battery cathode material and lithium ion battery
CN109440128B (en) * 2018-11-22 2021-02-09 成都先进金属材料产业技术研究院有限公司 Method for electrically modifying lithium titanate in molten salt
CN109473670A (en) * 2018-12-18 2019-03-15 上海纳米技术及应用国家工程研究中心有限公司 The preparation method and product of ion secondary battery cathode material lithium fluorine richness lithium titanate and application
CN112928244A (en) * 2019-12-05 2021-06-08 济南圣泉集团股份有限公司 Lithium ion battery electrode material, preparation method and battery

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