CN107425192A - A kind of lithium titanate material, preparation method and applications - Google Patents
A kind of lithium titanate material, preparation method and applications Download PDFInfo
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- CN107425192A CN107425192A CN201710425634.5A CN201710425634A CN107425192A CN 107425192 A CN107425192 A CN 107425192A CN 201710425634 A CN201710425634 A CN 201710425634A CN 107425192 A CN107425192 A CN 107425192A
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- lithium titanate
- lithium
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- metallic element
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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 provides a kind of lithium titanate material, preparation method and applications, a kind of preparation method of lithium titanate material, its preparation method includes：By lithium acetate be lithium source with method of electrostatic spinning, the solution that isopropyl titanate is titanium source, samaric nitrate is dopant prepare fibrous lithium titanate precursor material, samarium doping lithium titanate material is made in high-temperature calcination.Technical scheme provided by the invention, the chemical property of lithium titanate material can be both improved, the high rate capability and stability of lithium titanate material can be improved again, the lithium titanate material of preparation can be as the application of negative electrode of lithium titanate battery material.
Description
Technical field
The present invention relates to secondary cell technical field of energy storage, and in particular to a kind of lithium titanate material, preparation method and its should
With.
Background technology
Energy storage technology is broadly divided into physics energy storage (such as draw water energy storage, compressed-air energy storage, flywheel energy storage), chemical energy storage
(such as lead-acid battery, redox flow batteries, sodium-sulphur battery, lithium ion battery) and Power Flow (such as superconducting magnetic energy storage, surpass
Level capacitor energy storage etc.) three major types.Lithium ion battery energy storage is a kind of various electrochemical energy storage sides of energy storage conversion efficiency highest
Formula.Lithium titanate battery has high potential (about 1.55VvsLi+), be not easy to be formed thick SEI films, charge and discharge cycles during zero strain,
The advantages that lithium metal is not easy to separate out, because it has very high security feature, it has also become the outstanding person in battery storage materials.
Electrode material and electrolyte have a direct impact to the chemical property of lithium ion battery, especially positive and negative electrode material
Material, anode material for lithium-ion batteries are generally inlaid scheme, mainly there is cobalt-lithium oxide, nickel oxide lithium and manganese oxide lithium based material
Spinel manganese lithium system；Polyanionic positive electrode has LiFePO4 and polynary nickel cobalt manganese lithium system etc..Wherein commercial value is big
Anode material for lithium-ion batteries mainly have cobalt acid lithium, ternary material system.Lithium ion battery why can successful commercialization, source
It instead of that security performance is low and the short lithium metal of cycle life in lithium intercalation compound material.Preferable negative electrode of lithium ion battery should have
The characteristics of standby following：
(1) there is good ion and electronic conductivity：The diffusion coefficient of lithium ion is big, conductance is high, is easy to quickly fill
Electric discharge；
(2) insertion of lithium and deintercalation is reversible and course of reaction in the structure change very little of material do not change even, can
To ensure good cycle performance；
(3) higher efficiency for charge-discharge and cycle life：The surface texture of material is good, can fully be contacted with electrolyte；
With higher structural stability, chemical stability and heat endurance, and do not reacted with electrolyte；
(4) Gibbs free is small in the reaction of lithium ion；
(5) it is cost-effective and green safe.
At present, in the market is carbon class material using more negative material.But because carbon negative pole material is scarce in the presence of some
Fall into, so people explore some new non-carbon negative materials, such as lithium titanate material, it is as fast charge material in many necks
It is used widely in domain.
Lithium titanate material often appears in high magnification (10C and more than) performance in use and cycle performance is bad
Situation, this is due to that the electric conductivity of lithium titanate material is very low and structural instability, causes to polarize in charge and discharge process very tight
Caused by again.And on the premise of no doping or other modifications, carbonic acid lithium material specific discharge capacity under 20C only has
80mAh/g, it greatly limit fast charge ability.
The content of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of lithium titanate material and preparation method thereof, can be effective
The high rate capability and stable circulation performance of lithium titanate material are improved, the lithium titanate material of preparation can answering as lithium titanate battery
With.
The present invention is achieved through the following technical solutions：
(1) lithium source and titanium source are added in the alcohol solvent containing inhibitor, blank sample lithium titanate precursor is made
Solution；
(2) Ti positions metallic element is added into the blank sample lithium titanate precursor solution, is made doped with Ti positions metal
The lithium titanate precursor solution of element：
(3) the lithium titanate precursor solution doped with Ti positions metallic element is stirred at a constant temperature, then uses electrostatic
Spinning equipment spinning, fibrous lithium titanate precursor material is made；
(4) fibrous lithium titanate precursor material described in high-temperature calcination, obtains the lithium titanate doped with Ti positions metallic element
Material.
Preferably, in the lithium titanate precursor solution doped with Ti positions metallic element, elemental lithium in the lithium source,
The mol ratio of titanium elements and Ti positions metallic element in titanium source is 4:5:0.3—0.7.
Preferably, the titanium source and lithium source are respectively isopropyl titanate and lithium acetate.
Preferably, Ti positions metallic element is samarium element.
Preferably, the titanium source and the molal volume of ethanol ratio are 3/1000mol/ml.
Preferably, the titanium source and the molal volume of inhibitor ratio are 1/700mol/ml.
Preferably, the inhibitor is acetic acid.
Preferably, fibrous lithium titanate precursor material described in the high-temperature calcination, is obtained doped with Ti positions metallic element
Lithium titanate material specifically include：Calcined at 550-650 DEG C after the fibrous lithium titanate precursor material 2h then at 700-
5h is calcined at 800 DEG C.
Preferably, the particle diameter of the lithium titanate material doped with Ti positions metallic element is 100nm~400nm.
A kind of lithium titanate material, it includes lithium source, titanium source, inhibitor and Ti positions metallic element, the lithium member in the lithium source
Element, the mol ratio of the titanium elements in titanium source and Ti positions metallic element in the ethanol solution containing inhibitor are 4：5：0.3-0.7, institute
It is samarium element to state Ti positions metallic element.
Preferably, the titanium source and mole body that the molal volume of ethanol ratio is 3/1000mol/ml, titanium source and inhibitor
Product ratio is 1/700mol/ml.
Preferably, described lithium titanate material is as the application for preparing negative electrode of lithium titanate battery material.
Compared with immediate prior art, technical scheme provided by the invention has the advantages that：
(1) technical scheme provided by the invention, lithium titanate material, and traditional solid phase method phase are prepared with method of electrostatic spinning
Than the particle diameter of the lithium titanate material of preparation slow down material agglomeration, improve metatitanic acid significantly between 100nm to 400nm
The chemical property of lithium material.
(2) technical scheme provided by the invention, in the Ti positions metallic element samarium doped element of lithium titanate material, the big titanium of support
The lattice of sour lithium material, expand the transmission path of lithium ion so that lithium titanate material fills under the high-discharge-rate under 50C
Discharge capacity rises to 108mAh/g by 17mAh/g, improves the high rate capability of lithium titanate material.
(3) technical scheme provided by the invention, to the Ti positions metallic element doping vario-property of carbonic acid lithium material, crystal is optimized
The stability of structure so that lithium titanate material charge/discharge capacity after the circle of discharge-rate 10C circulations 1000 is risen by 51mAh/g
To 106mAh/g, the cycle performance of lithium titanate material is improved.
Brief description of the drawings
Fig. 1 is that electrostatic spinning prepares lithium titanate material flow chart；
Fig. 2 is from left to right blank sample successively, according to Li:Ti:Sm=4:5:0.3=0.7 (mol ratio) samarium element is mixed
The 100k enlargement ratios SEM figures of miscellaneous lithium titanate material, Sm refer to samarium element；
Fig. 3 is blank sample and Li:Ti:Sm=4:5:The difference of the lithium titanate material of the samarium element doping of 0.5 (mol ratio) 0
Rate specific capacities comparison diagram；
Fig. 4 is blank sample and Li:Ti:Sm=4:5:The lithium titanate material of the samarium element doping of 0.5 (mol ratio) 10C,
The long cycle performance figure of 1000 circles；
Fig. 5 is that electrospinning process just spins obtained persursor material SEM figures；
Fig. 6 is lithium titanate SEM figures after persursor material sintering.
Embodiment
Embodiment 1
(the mol ratio of preparation method 1 of samarium doping lithium titanate material：Elemental lithium：Titanium elements：Samarium element=4:5:0.3)
(1) blank sample lithium titanate precursor solution is prepared：
1. 0.03mol isopropyl titanates and 0.024mol lithium acetates are added to the mixed liquor of 10mL ethanol and 21mL acetic acid
In, stirred 30 minutes in constant temperature blender with magnetic force；
2. adding 0.9g polyvinylpyrrolidone PVP, stirred 1 hour in constant temperature blender with magnetic force, obtain blank sample titanium
Sour lithium precursor solution；
(2) the lithium titanate precursor solution of samarium doping is prepared：Into blank sample lithium titanate precursor solution, solution adds
0.0018mol samaric nitrate, magnetic constant temperature power stir 1 hour.
(3) electrostatic spinning：
The lithium titanate precursor solution of samarium doping is placed in electrospinning device, with 2.5mL/h spinning speed, in
Spinning is carried out under 20kV voltages, and it is 13cm to keep the spacing of syringe needle and receiver in spinning process, obtains fibrous lithium titanate
Persursor material.
(4) calcine：
Fibrous lithium titanate precursor material is put in the Muffle furnace that heating rate is 2 DEG C/min and calcined, in 550
DEG C calcining 2 hours, then heat to 750 DEG C calcine 5 hours, obtain the lithium titanate material of samarium doping.
Embodiment 2
(the mol ratio of preparation method 2 of samarium doping lithium titanate material：Elemental lithium：Titanium elements：Samarium element=4:5:0.5)
(1) blank sample lithium titanate precursor solution is prepared：
1. 0.03mol isopropyl titanates and 0.024mol lithium acetates are added to the mixed liquor of 10mL ethanol and 21mL acetic acid
In, stirred 30 minutes in constant temperature blender with magnetic force；
2. adding 0.9g polyvinylpyrrolidone PVP, stirred 1 hour in constant temperature blender with magnetic force, obtain blank sample titanium
Sour lithium precursor solution；
(2) the lithium titanate precursor solution of samarium doping is prepared：Into blank sample lithium titanate precursor solution, solution adds
0.003mol samaric nitrate, magnetic constant temperature power stir 1 hour.
(3) electrostatic spinning：
The lithium titanate precursor solution of samarium doping is placed in electrospinning device, with 2.5mL/h spinning speed, in
Spinning is carried out under 20kV voltages, and it is 13cm to keep the spacing of syringe needle and receiver in spinning process, obtains fibrous lithium titanate
Persursor material.
(4) calcine：
Fibrous lithium titanate precursor material is put in the Muffle furnace that heating rate is 2 DEG C/min and calcined, in 600
DEG C calcining 2 hours, then heat to 750 DEG C calcine 5 hours, obtain the lithium titanate material of samarium doping.
Embodiment 3
(the mol ratio of preparation method 3 of samarium doping lithium titanate material：Elemental lithium：Titanium elements：Samarium element=4:5:0.7)
(1) blank sample lithium titanate precursor solution is prepared：
1. 0.03mol isopropyl titanates and 0.024mol lithium acetates are added to the mixed liquor of 10mL ethanol and 21mL acetic acid
In, stirred 30 minutes in constant temperature blender with magnetic force；
2. adding 0.9g polyvinylpyrrolidone PVP, stirred 1 hour in constant temperature blender with magnetic force, obtain blank sample titanium
Sour lithium precursor solution；
(2) the lithium titanate precursor solution of samarium doping is prepared：Into blank sample lithium titanate precursor solution, solution adds
0.0042mol samaric nitrate, magnetic constant temperature power stir 1 hour.
(3) electrostatic spinning：
The lithium titanate precursor solution of samarium doping is placed in electrospinning device, with 2.5mL/h spinning speed, in
Spinning is carried out under 20kV voltages, and it is 13cm to keep the spacing of syringe needle and receiver in spinning process, obtains fibrous lithium titanate
Persursor material.
(4) calcine：
Fibrous lithium titanate precursor material is put in the Muffle furnace that heating rate is 2 DEG C/min and calcined, in 600
DEG C calcining 2 hours, then heat to 800 DEG C calcine 5 hours, obtain the lithium titanate material of samarium doping.
The charge/discharge capacity contrast of each embodiment lithium titanate material
Table 1
Finally it should be noted that：The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, institute
The those of ordinary skill in category field with reference to above-described embodiment still can to the present invention embodiment modify or
Equivalent substitution, these are applying for this pending hair without departing from any modification of spirit and scope of the invention or equivalent substitution
Within bright claims.
Claims (11)
1. a kind of preparation method of lithium titanate material, it is characterised in that methods described comprises the steps：
(1) lithium source and titanium source are added into the alcohol solvent containing inhibitor, blank sample lithium titanate precursor solution is made；
(2) Ti positions metallic element is added into the blank sample lithium titanate precursor solution, is made doped with Ti positions metallic element
Lithium titanate precursor solution；
(3) the lithium titanate precursor solution doped with Ti positions metallic element is stirred at a constant temperature, then uses electrostatic spinning
Equipment spinning, fibrous lithium titanate precursor material is made；
(4) fibrous lithium titanate precursor material described in high-temperature calcination, obtains the lithium titanate material doped with Ti positions metallic element.
2. a kind of preparation method of lithium titanate material as claimed in claim 1, it is characterised in that described doped with Ti positions metal
In the lithium titanate precursor solution of element, titanium elements in elemental lithium, titanium source in the lithium source rub with Ti positions metallic element
You are than being 4:5:0.3-0.7.
A kind of 3. preparation method of lithium titanate material as claimed in claim 1, it is characterised in that titanium source and the lithium source difference
For isopropyl titanate and lithium acetate.
4. a kind of preparation method of lithium titanate material as claimed in claim 1, it is characterised in that Ti positions metallic element is
Samarium element.
5. a kind of preparation method of lithium titanate material as claimed in claim 1, it is characterised in that the titanium source and ethanol rub
Your volume ratio is 3/1000mol/ml, and the molal volume ratio of the titanium source and inhibitor is 1/700mol/ml.
6. a kind of preparation method of lithium titanate material as claimed in claim 5, it is characterised in that the inhibitor is acetic acid.
7. a kind of preparation method of lithium titanate material as claimed in claim 1, it is characterised in that fine described in the high-temperature calcination
Shape lithium titanate precursor material is tieed up, obtains including doped with the lithium titanate material of Ti positions metallic element：
After the fibrous lithium titanate precursor material 2h is calcined at 550-650 DEG C 5h is calcined at 700-800 DEG C.
8. a kind of preparation method of lithium titanate material as claimed in claim 1, it is characterised in that described doped with Ti positions metal
The particle diameter of the lithium titanate material of element is 100nm~400nm.
9. a kind of lithium titanate material, it is characterised in that it includes lithium source, titanium source, inhibitor and Ti positions metallic element, the lithium source
In elemental lithium, the mol ratio of the titanium elements in titanium source and Ti positions metallic element in the ethanol solution containing inhibitor be 4：5：
0.3-0.7, Ti positions metallic element are samarium element.
10. a kind of lithium titanate material as claimed in claim 9, it is characterised in that the titanium source and the molal volume of ethanol ratio
For 3/1000mol/ml, the molal volume ratio of the titanium source and inhibitor is 1/700mol/ml.
11. application of the lithium titanate material as described in claim 1-10 any one as negative electrode of lithium titanate battery material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109637767A (en) * | 2018-12-18 | 2019-04-16 | 浙江中杭新材料科技有限公司 | A kind of sintering method of neodymium iron boron magnetic body |
| CN111793856A (en) * | 2020-06-10 | 2020-10-20 | 齐鲁工业大学 | Cu-Br-doped lithium titanate nanofiber material and preparation method and application thereof |
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| CN102820460A (en) * | 2012-08-20 | 2012-12-12 | 上海交通大学 | Electrostatic spinning method for preparing rare-earth metal doped nanometer lithium titanate |
| CN104826622A (en) * | 2014-04-10 | 2015-08-12 | 北汽福田汽车股份有限公司 | Nano titanium dioxide material supported by porous carbon nano fiber and doped with samarium, preparation method and application thereof |
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| CN102820460A (en) * | 2012-08-20 | 2012-12-12 | 上海交通大学 | Electrostatic spinning method for preparing rare-earth metal doped nanometer lithium titanate |
| CN104826622A (en) * | 2014-04-10 | 2015-08-12 | 北汽福田汽车股份有限公司 | Nano titanium dioxide material supported by porous carbon nano fiber and doped with samarium, preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109637767A (en) * | 2018-12-18 | 2019-04-16 | 浙江中杭新材料科技有限公司 | A kind of sintering method of neodymium iron boron magnetic body |
| CN109637767B (en) * | 2018-12-18 | 2020-08-21 | 浙江中杭新材料科技有限公司 | Sintering method of neodymium iron boron magnet |
| CN111793856A (en) * | 2020-06-10 | 2020-10-20 | 齐鲁工业大学 | Cu-Br-doped lithium titanate nanofiber material and preparation method and application thereof |
| CN111793856B (en) * | 2020-06-10 | 2022-09-27 | 齐鲁工业大学 | Cu-Br-doped lithium titanate nanofiber material and preparation method and application thereof |
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