CN107275612A - The carambola shape lithium titanate titanium dioxide electrodes material and preparation method and application of a kind of multilevel hierarchy - Google Patents
The carambola shape lithium titanate titanium dioxide electrodes material and preparation method and application of a kind of multilevel hierarchy Download PDFInfo
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- CN107275612A CN107275612A CN201710465319.5A CN201710465319A CN107275612A CN 107275612 A CN107275612 A CN 107275612A CN 201710465319 A CN201710465319 A CN 201710465319A CN 107275612 A CN107275612 A CN 107275612A
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- titanium dioxide
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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
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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
- H01M4/48—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
- H01M4/48—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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- 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 kind of carambola shape lithium titanate/titanium dioxide electrodes material with multilevel hierarchy and preparation method and application, chelating agent is dissolved in deionized water, and titanium source presoma is added in chelating agent solution and stirred, and instills the mother liquor that lithium salt solution obtains yellow；Mother liquor is sealed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, is handled by crystallization, washing, drying etc., obtains white solid powder；Calcining, finally gives Li4Ti5O12/TiO2Composite.It the method achieve lithium titanate and titanium dioxide effectively combined, show obvious second structure characteristic.The Li prepared4Ti5O12/TiO2Composite has the pattern of carambola shape, and average grain diameter is 2.0 5.0 microns, with secondary structure, and basic component units are the Li of high-sequential4Ti5O12And TiO2Nano flake.This method technique is simple, be easy to regulation and control, and the features such as composite of gained has high porosity, compound with regular structure has larger application value in terms of lithium ion battery electrode material field.
Description
Technical field
The invention belongs to field of composite material preparation, and in particular to a kind of carambola shape lithium titanate/titanium dioxide of multilevel hierarchy
Titanium electrode material and preparation method and application.
Background technology
New energy technology promotes the fast development of low-carbon economy, while being proposed more to the high performance battery such as lithium ion battery
High requirement.Traditional carbon negative pole material have with compatibility of electrolyte it is poor, graphite linings are easy to fall off, structural instability etc. lack
Point.Finding has higher intercalation potential, and the reliable novel cathode material for lithium ion battery of performance safety turns into grinding for people
Study carefully focus.Based on the intrinsic security of titanyl compound and with the preferable compatibility of electrolyte, including various metatitanic acid lithium salts and
Polymorphic titanium dioxide, is represented in the quasi-representative that field of lithium ion battery is considered as safety-type negative material.
Titanium dioxide（TiO2）Basic structural unit all be distortion titanyl octahedral body [TiO6], pass through different modes
Different crystal forms, including rutile, anatase, brockite etc. are connected and composed.When for lithium ion battery electrode material, it
It is stable with chemical property, the advantages of safe.Lithium titanate（Li4Ti5O12）A kind of zero strain material, lithium insertion/
Any change hardly occurs for structure in abjection, when for lithium ion battery electrode material, there is high operating voltage range
（1.0 ~ 3.0V, vs. Li/Li+）, it can be ensured that battery has more preferable security.At present to TiO2And Li4Ti5O12Electrode material
Research main carried out from following two directions：One is TiO of the design with special appearance size2And Li4Ti5O12Nano-particle,
Such as nanotube, nanosphere, nanometer rods, nanometer sheet etc., this kind of material can make Li after microsize and special construction is possessed+Diffusion path in body phase shortens, and adds Li+ The area of de-/embedding lithium and charge transfer, causes material to show more excellent
Different chemical property；Two be design with receiving/Li of differential level structure4Ti5O12/TiO2Composite.Li4Ti5O12It is used as lithium
When ion battery electrode materials are used, its usual very little of irreversible capacity, and TiO2Capacity it is higher, therefore
Li4Ti5O12And TiO2When both are effectively compound, the advantage of two kinds of materials can be combined, higher capacity is produced and relatively low
Irreversible capacity.
Notification number discloses a kind of Li for CN201210243679.8 patent4Ti5O12/ TiO2The preparation of composite
Titanyl sulfate hydrolysis is prepared TiO by method, this method first using titanyl sulfate as predecessor2Material；Then by preparation
TiO2Mix, calcined after steam treatment with LiOH, obtain Li4Ti5O12/ TiO2Composite.Notification number is
CN200710054481.4 patent discloses a kind of nanometer Li4Ti5O12/ TiO2The preparation method of compound, this method is first
By TiO2In the KOH solution for being dissolved in heat, Nano lines of potassium titanate is prepared, heating is then melted at 1000 DEG C with lithium citrate,
Prepare Li4Ti5O12/ TiO2Composite.The above-mentioned preparation process of these composites is relative complex, and technique is cumbersome；It is heavier
Want, Li4Ti5O12And TiO2Both of which fails effective combination, prepared composite without heterojunction structure, fail be in
The feature of existing multilevel hierarchy.
The content of the invention
The shortcoming for failing effectively to be combined for lithium titanate and titanic oxide material, a kind of multistage knot of patented invention of the present invention
The carambola shape lithium titanate/titanium dioxide electrodes material and preparation method and application of structure.The present invention is by titanium source, lithium salts and chelating
Agent is mixed according to a certain percentage, and Li is realized in water heating kettle4Ti5O12And TiO2Effective self assembly, so as to be formed with multistage knot
The carambola shape Li of structure4Ti5O12/TiO2Composite.When use as lithium ion battery electrode material, the material is combined
Li4Ti5O12And TiO2The advantage of material, can show that higher capacity and preferable high rate performance, be a kind of to have that have much should
With the Li of prospect4Ti5O12/TiO2Composite.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of preparation method of carambola shape lithium titanate/titanium dioxide electrodes material of multilevel hierarchy, the lithium titanate/titanium dioxide
For Li4Ti5O12/TiO2, it is characterised in that comprise the following steps that：
A, weigh a certain amount of chelating agent and be dissolved in deionized water, form homogeneous chelating agent solution；
B, titanium source presoma is slowly added into above-mentioned chelating agent solution system according to a certain percentage, made by stirring before titanium source
Drive body to be dissolved in chelating agent solution, being then slowly dropped under certain density lithium salt solution, stirring is well mixed lithium salts, obtains
To the mother liquor of yellow；
C, above-mentioned yellow mother is sealed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, by the crystallization of certain time, washing, dry
It is dry to wait processing, obtain white solid powder；Crystallization temperature is 120 ~ 140 DEG C, and crystallization time is 15 ~ 20 hours；
D, this white solid powder is placed in 500 ~ 700 DEG C at a temperature of calcine, heating rate control is with 3 DEG C/min, most
Li is obtained eventually4Ti5O12/TiO2Composite.
Described chelating agent is one kind in hydrogen peroxide, ethylene glycol, glycerine.
Described titanium source presoma is one in positive four butyl ester of metatitanic acid, tetraisopropyl titanate, titanyl sulfate, titanium tetrachloride
Kind.
Described lithium source presoma is one kind in lithium hydroxide, lithium nitrate, lithium citrate.
Li and Ti mole mixture ratio is controlled 0.05 ~ 0.20 in described step b.
Crystallization temperature control is at 120 ~ 140 DEG C in described step c, preferably 130 DEG C；Crystallization time is 15 ~ 20 hours,
Preferably 18 hours.
Carambola shape lithium titanate/titanium dioxide electrodes material of a kind of multilevel hierarchy, it is characterised in that according to any of the above-described institute
The method of stating is prepared；Described material shows obvious second structure characteristic, and its primary structure composition is ultra-thin
Li4Ti5O12And TiO2Nanometer sheet；Secondary structure composition is high-sequential, and average grain diameter is 2-5 microns of carambola shape microballoon, it
It is by Li4Ti5O12And TiO2One-level nanometer sheet constituted.
A kind of carambola shape lithium titanate of multilevel hierarchy/application of the titanium dioxide electrodes material in lithium ion battery.
The present invention prepares the Li with multilevel hierarchy using simple one step hydro thermal method4Ti5O12/TiO2Composite, by
In the addition of chelating agent so that hydrolysis will not occur at room temperature for positive four butyl ester of titanium source presoma such as metatitanic acid, titanyl sulfate,
Can stably it exist in solution.Under hydrothermal conditions, water occurs for the titanium source predecessor such as positive four butyl ester of metatitanic acid, titanyl sulfate
Solution, a part of hydrolysate is titanium dioxide nanoplate, and the hydrolysate of another part continues to react with lithium hydroxide,
Generate lithium titanate nanometer sheet.In the presence of chelating agent, mutual accumulation and the influence of titanium dioxide and lithium titanate nanometer sheet, finally
Form the Li with two grades of carambola shape structures4Ti5O12/TiO2Composite.
It the method achieve Li4Ti5O12And TiO2Effectively combine, it is special that prepared material shows obvious secondary structure
Levy.Its primary structure composition is ultra-thin Li4Ti5O12And TiO2Nanometer sheet；Secondary structure composition is high-sequential, average grain
Footpath is 2-5 microns of carambola shape microballoon, and it is by Li4Ti5O12And TiO2One-level nanometer sheet constituted. Li4Ti5O12/
TiO2The synthetic method of composite is prepared by hydro-thermal approach one-step method, and technique is simple, it is easy to regulate and control, respectively by titanium
Source presoma, lithium salts, chelating agent are effectively mixed, and are obtained product by hydro-thermal and calcining approach, are realized special appearance
Li4Ti5O12/TiO2The controllable preparation of electrode material.The features such as composite of gained has high porosity, compound with regular structure.
Brief description of the drawings
Fig. 1 is the Li that the embodiment of the present invention 1 is synthesized4Ti5O12/TiO2The XRD of composite.
Fig. 2 is the Li that the embodiment of the present invention 1 is synthesized4Ti5O12/TiO2The SEM figures of composite.
Embodiment
The present embodiment is implemented lower premised on technical solution of the present invention, gives detailed embodiment and specific
Operating process, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1：
0.5 mol/L lithium hydroxide solution is prepared first, is stayed with standby.Then 10 mL hydrogen peroxide reagent is weighed, is added to
In 100 mL deionized water, homogeneous solution is formed.The previously prepared hydrogen-oxygens of 150 mL are added dropwise into above-mentioned hydrogen peroxide solution
Change lithium solution, stir 30min, be then slowly added dropwise again under positive four butyl ester of 4.14 g metatitanic acids, strong agitation, it is seen that the color of solution
Yellow is progressively changed into from white；Above-mentioned yellow solution is sealed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, at a temperature of 130 DEG C
After crystallization 18 hours, by filtering, carrying out washing treatment, the powder of white is obtained；By heating speed of this white powder according to 3 DEG C/min
Rate is warming up to 500 DEG C and calcined 3 hours, may finally obtain the Li with multilevel hierarchy4Ti5O12/TiO2Composite.Fig. 1 is institute
The Li of preparation4Ti5O12/TiO2The XRD of composite, it corresponds to Li4Ti5O12And TiO2Crystal formation characteristic peak, it was confirmed that institute
The material of preparation is the compound of lithium titanate and titanium dioxide.Fig. 2 is prepared Li4Ti5O12/TiO2The SEM figures of composite
（a, b）, from figure, it can be seen that it shows the architectural feature of carambola shape, possess multilevel hierarchy.Wherein, primary structure composition is
Ultra-thin Li4Ti5O12And TiO2Nanometer sheet；Secondary structure composition is high-sequential, and the carambola shape of 2-5 microns of average grain diameter is micro-
Ball, it is by Li4Ti5O12And TiO2One-level nanometer sheet constituted.
Embodiment 2：
0.5 mol/L lithium hydroxide solution is prepared first, is stayed with standby.Then 10 mL hydrogen peroxide reagent is weighed, is added to
In 100 mL deionized water, homogeneous solution is formed.The previously prepared hydrogen-oxygens of 150 mL are added dropwise into above-mentioned hydrogen peroxide solution
Change lithium solution, stir 30min, be then slowly added dropwise again under positive four butyl ester of 12.51 g metatitanic acids, strong agitation, it is seen that the face of solution
Color is progressively changed into yellow from white；Above-mentioned yellow solution is sealed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, in 130 DEG C of temperature
Lower crystallization, by filtering, carrying out washing treatment, obtains the powder of white after 18 hours；By heating of this white powder according to 3 DEG C/min
Speed is warming up to 500 DEG C and calcined 3 hours, may finally obtain the Li with multilevel hierarchy4Ti5O12/TiO2Composite.
Embodiment 3：
0.5 mol/L lithium nitrate solution is prepared first, is stayed with standby.Then the hydrogen peroxide reagent for weighing 10 mL is dissolved in 100
In mL deionized water, homogeneous solution is formed.The previously prepared lithium nitrates of 150 mL are added dropwise into above-mentioned hydrogen peroxide solution molten
Liquid, stirs 30min, is then slowly added dropwise again under 6.14 g tetraisopropyl titanates, strong agitation, the color of solution by white progressively
It is changed into yellow；Above-mentioned yellow solution is shifted and is sealed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, the crystallization at a temperature of 130 DEG C
After 18 hours, by filtering, carrying out washing treatment, the powder of white is obtained；This white powder is heated up with 3 DEG C/min heating rate
Calcined 3 hours to 500 DEG C, the Li with multilevel hierarchy may finally be obtained4Ti5O12/TiO2Composite.
Claims (8)
1. a kind of preparation method of carambola shape lithium titanate/titanium dioxide electrodes material of multilevel hierarchy, the lithium titanate/titanium dioxide
Titanium is Li4Ti5O12/TiO2, it is characterised in that comprise the following steps that：
A, weigh a certain amount of chelating agent and be dissolved in deionized water, form homogeneous chelating agent solution；
B, titanium source presoma is slowly added into above-mentioned chelating agent solution system according to a certain percentage, made by stirring before titanium source
Drive body to be dissolved in chelating agent solution, being then slowly dropped under certain density lithium salt solution, stirring is well mixed lithium salts, obtains
To the mother liquor of yellow；
C, above-mentioned yellow mother is sealed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, by the crystallization of certain time, washing, dry
It is dry to wait processing, obtain white solid powder；Crystallization temperature is 120 ~ 140 DEG C, and crystallization time is 15 ~ 20 hours；
D, this white solid powder is placed in 500 ~ 700 DEG C at a temperature of calcine, heating rate control is with 3 DEG C/min, most
Li is obtained eventually4Ti5O12/TiO2Composite.
2. the preparation method of carambola shape lithium titanate/titanium dioxide electrodes material of multilevel hierarchy according to claim 1, it is special
Levy and be, described chelating agent is one kind in hydrogen peroxide, ethylene glycol, glycerine.
3. the preparation method of carambola shape lithium titanate/titanium dioxide electrodes material of multilevel hierarchy according to claim 1, it is special
Levy and be, described titanium source presoma is one kind in positive four butyl ester of metatitanic acid, tetraisopropyl titanate, titanyl sulfate, titanium tetrachloride.
4. the preparation method of carambola shape lithium titanate/titanium dioxide electrodes material of multilevel hierarchy according to claim 1, it is special
Levy and be, described lithium source presoma is one kind in lithium hydroxide, lithium nitrate, lithium citrate.
5. the preparation method of carambola shape lithium titanate/titanium dioxide electrodes material of multilevel hierarchy according to claim 1, it is special
Levy and be, Li and Ti mole mixture ratio is controlled 0.05 ~ 0.20 in described step b.
6. the preparation method of carambola shape lithium titanate/titanium dioxide electrodes material of multilevel hierarchy according to claim 1, it is special
Levy and be, crystallization temperature control is at 120 ~ 140 DEG C in described step c, preferably 130 DEG C；Crystallization time is 15 ~ 20 hours, excellent
Elect as 18 hours.
7. carambola shape lithium titanate/titanium dioxide electrodes material of a kind of multilevel hierarchy, it is characterised in that according to claim 1-6
Any methods described is prepared；Described material shows obvious second structure characteristic, and its primary structure composition is super
Thin Li4Ti5O12And TiO2Nanometer sheet；Secondary structure composition is high-sequential, and average grain diameter is micro- for 2-5 microns of carambola shape
Ball, it is by Li4Ti5O12And TiO2One-level nanometer sheet constituted.
8. carambola shape lithium titanate/titanium dioxide electrodes material of multilevel hierarchy is in lithium ion battery according to claim 7
Application.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107946554A (en) * | 2017-10-26 | 2018-04-20 | 天津普兰能源科技有限公司 | A kind of preparation method of lithium battery lithium titanate anode material |
| CN110061245A (en) * | 2019-04-11 | 2019-07-26 | 武汉大学 | The preparation method of solid oxide cell electrode material |
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| CN102070186A (en) * | 2010-11-23 | 2011-05-25 | 南京航空航天大学 | Preparation method of spinel type nano lithium titanate |
| CN102169980A (en) * | 2010-02-27 | 2011-08-31 | 比亚迪股份有限公司 | Preparation method of anode active material |
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| CN102169980A (en) * | 2010-02-27 | 2011-08-31 | 比亚迪股份有限公司 | Preparation method of anode active material |
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Non-Patent Citations (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107946554A (en) * | 2017-10-26 | 2018-04-20 | 天津普兰能源科技有限公司 | A kind of preparation method of lithium battery lithium titanate anode material |
| CN110061245A (en) * | 2019-04-11 | 2019-07-26 | 武汉大学 | The preparation method of solid oxide cell electrode material |
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