CN105118978A - Preparation method of freeze-dried doped modified lithium titanate - Google Patents
Preparation method of freeze-dried doped modified lithium titanate Download PDFInfo
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- CN105118978A CN105118978A CN201510403002.XA CN201510403002A CN105118978A CN 105118978 A CN105118978 A CN 105118978A CN 201510403002 A CN201510403002 A CN 201510403002A CN 105118978 A CN105118978 A CN 105118978A
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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
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- 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
- H01M4/626—Metals
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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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Abstract
The invention relates to a preparation method of freeze-dried doped modified lithium titanate, and provides a preparation method for improving the electron conductivity, the charge and discharge performances and the cycle performances of a lithium ion battery negative material lithium titanate. The method comprises the following steps: dissolving soluble compounds of Li and Ti in distilled water, adding chitosan to an acetate acid gracial solution, and carrying out ultrasonic dissolving to form a uniform pale yellow solution; adding titanium dioxide powder and a Yb compound to the chitosan solution, and adding epichlorohydrin; and burdening according to a Ba:Sr:Co:Fe mole ratio of 0.5:0.5:0.8:0.2, adding an ethanol and water mixed liquid, premixing a double-component chelating agent with water, adding ammonia water, refrigerating at -60DEG C, putting the refrigerated material in a lyophilizer, carrying out vacuum drying, and calcining. The lithium ion secondary battery negative material, that is modified lithium titanate Ba0.5Sr0.5Co0.2Fe0.8O3 coated Li4YbpTi5-pO12, is prepared through a freeze-drying microemulsion technology, and the material has excellent rate performances, and is suitable for being used in power batteries.
Description
Technical field
The present invention relates to a kind of preparation method of battery electrode material, particularly a kind of preparation method of ion secondary battery cathode material lithium ytterbium doping vario-property lithium titanate.
Background technology
At present, the negative material of business-like lithium ion battery adopts carbon negative pole material mostly, but carbon negative pole material exists some defects: react with electrolyte in discharge process formation surface passivated membrane first, cause the consumption of electrolyte and coulombic efficiency is lower first; The electrode potential of carbon electrode and lithium metal is close, when battery overcharge, still may at carbon electrodes precipitating metal lithium, and form dendrite and cause short circuit, cause safety problem etc.
Recently, spinel type lithium titanate, as a kind of novel negative material, has " zero strain ", the advantages such as good cycle, becomes the focus of research gradually." zero strain " material-lithium titanate is 1.55V relative to the current potential of lithium metal, far above the recovery voltage of most electrolyte, the reduction of electrolyte and the generation of passivating film can be avoided, the generation of lithium metal can be stoped simultaneously, there is very excellent cycle performance and security performance.But lithium titanate is a kind of insulating material, its poorly conductive, and when high current charge-discharge, capacity attenuation is fast, high rate performance is poor, limits its application.
The present invention is directed to existing preparation Li
4ti
5o
12shortcoming, obtained the modified lithium titanate material of excellent performance by freeze drying micro emulsion legal system.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of preparation method of freeze drying doping vario-property lithium titanate, being prepared the lithium titanate anode material being applied to lithium ion battery by this method.
A preparation method for freeze drying doping vario-property lithium titanate, is characterized in that, comprise the steps:
(1) first weigh the soluble compound of Li and Ti, add distilled water and dissolve, then weigh shitosan and join in glacial acetic acid solution, ultrasonic to being dissolved as homogeneous weak yellow liquid completely;
(2) in chitosan solution, add the compound of titania powder and Yb, ultrasonic, magnetic agitation 5 minutes; Add in the solution that step (1) dissolved in chitosan solution, ultrasonic agitation 5 minutes;
(3) in step (2) solution, add certain epoxychloropropane, continuing magnetic force stirs 1 ~ 3 hour;
(4) by the soluble compound of Ba, Sr, Co and Fe, prepare burden according to mol ratio Ba:Sr:Co:Fe:=0.5:0.5:0.8:0.2, add the ethanol and water mixed liquid that prepare in advance, be stirred to and dissolve completely;
(5) by two component chelating agent and water premix, add ammoniacal liquor after mixing and all dissolve to chelating agent, then add the mixed liquor of step (4);
(6) will move in culture dish after step (5) and (3) mixing, build with preservative film, freezing at-60 DEG C, the sample freezed is put into freeze drier, vacuumize dry 24 hours, crucible put into by dried sample, calcines 8 ~ 10 hours for 500 ~ 700 DEG C under feeding tube furnace.
Described lithium titanate material is Ba
0.5sr
0.5co
0.2fe
0.8o
3coated Li
4yb
pti
5-po
12, 0.1 < p≤0.2 in formula, 0.01 < Ba:Li≤0.1.
Described Yb compound is ytterbium nitrate or ytterbium oxide.
The lithium titanate anode material adopting method of the present invention to prepare shows certain mesoporous characteristic, and this lithium titanate anode material has excellent large rate discharge characteristic.
Accompanying drawing explanation
Fig. 1 is the TEM figure of the embodiment of the present invention 1 product.
Embodiment
Below embodiments of the invention are elaborated: the present embodiment is implemented under premised on technical solution of the present invention, give detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1: weigh 3.915g lithium formate, the distilled water adding 10ml dissolves, the shitosan weighing 1.2575g again adds in the glacial acetic acid solution of 42ml, ultrasonic to being dissolved as homogeneous weak yellow liquid completely, the ytterbium nitrate of 4.432g titania powder and 0.0862g is added in chitosan solution, ultrasonic, magnetic agitation 5 minutes, in chitosan solution, add the lithium acetate solution dissolved, stir 5 minutes, adding the epoxychloropropane of 0.4ml in above-mentioned solution, continuing magnetic force stirs 1h, separately take the barium nitrate of 0.1307g, the strontium nitrate of 0.1058, the ferric nitrate of 0.0582g cobalt nitrate and 0.1935g is prepared burden, be dissolved in the mixing easily of 30 milliliters of ethanol and 3 ml waters, be stirred to dissolving, again 0.2g ethylenediamine tetra-acetic acid and 0.3g citric acid are added in metal ion solution mixed in advance, add ammoniacal liquor and regulate pH value to 8, to be transferred in culture dish after this solution and solution mixing and stirring above, build with preservative film, freezing at-60 DEG C, the sample freezed is put into freeze drier, vacuumize, dry 24h, obtain in spongiform white pigmented samples, 8h is calcined at sample being put into 700 DEG C, formula stove, be prepared into end product.
Embodiment 2: weigh 3.6517g lithium carbonate, the distilled water adding 10ml dissolves, the shitosan weighing 1.4281g again adds in the glacial acetic acid solution of 100ml, ultrasonic to being dissolved as homogeneous weak yellow liquid completely, the ytterbium nitrate of 3.468g titania powder and 0.1181g is added in chitosan solution, ultrasonic, magnetic agitation 5 minutes, in chitosan solution, add the lithium acetate solution dissolved, stir 5 minutes, adding the epoxychloropropane of 0.7ml in above-mentioned solution, continuing magnetic force stirs 3h, separately take the barium nitrate of 0.1531g, the strontium nitrate of 0.1482, the ferric nitrate of 0.0582g cobalt nitrate and 0.1935g is prepared burden, be dissolved in the mixing easily of 30 milliliters of ethanol and 3 ml waters, be stirred to dissolving, again 0.2g ethylenediamine tetra-acetic acid and 0.4g citric acid are added in metal ion solution mixed in advance, add ammoniacal liquor and regulate pH value to 8, to be transferred in culture dish after this solution and solution mixing and stirring above, build with preservative film, freezing at-60 DEG C, the sample freezed is put into freeze drier, vacuumize, dry 24h, obtain in spongiform white pigmented samples, 10h is calcined at sample being put into 600 DEG C, formula stove, be prepared into end product.
Embodiment 3: weigh 4.153g lithium acetate, the distilled water adding 10ml dissolves, the shitosan weighing 1.0748g again adds in the glacial acetic acid solution of 50ml, ultrasonic to being dissolved as homogeneous weak yellow liquid completely, the ytterbium oxide of 3.9278g titania powder and 0.239g is added in chitosan solution, ultrasonic, magnetic agitation 5 minutes, in chitosan solution, add the lithium acetate solution dissolved, stir 5 minutes, adding the epoxychloropropane of 0.5ml in above-mentioned solution, continuing magnetic force stirs 2h, separately take the barium nitrate of 0.1307g, the strontium nitrate of 0.1058, the ferric nitrate of 0.0582g cobalt nitrate and 0.2035g is prepared burden, be dissolved in the mixing easily of 30 milliliters of ethanol and 3 ml waters, be stirred to dissolving, again 0.3g ethylenediamine tetra-acetic acid and 0.4g citric acid are added in metal ion solution mixed in advance, add ammoniacal liquor and regulate pH value to 8, to be transferred in culture dish after this solution and solution mixing and stirring above, build with preservative film, freezing at-60 DEG C, the sample freezed is put into freeze drier, vacuumize, dry 24h, obtain in spongiform white pigmented samples, 9h is calcined at sample being put into 500 DEG C, formula stove, be prepared into end product.
Embodiment 4: weigh 4.8597g lithium citrate, the distilled water adding 10ml dissolves, the shitosan weighing 1.5408g again adds in the glacial acetic acid solution of 80ml, ultrasonic to being dissolved as homogeneous weak yellow liquid completely, the ytterbium oxide of 4.551g titania powder and 0.0227g is added in chitosan solution, ultrasonic, magnetic agitation 5 minutes, in chitosan solution, add the lithium acetate solution dissolved, stir 5 minutes, adding the epoxychloropropane of 0.6ml in above-mentioned solution, continuing magnetic force stirs 1h, separately take the barium nitrate of 0.1307g, the strontium nitrate of 0.1058, the ferric nitrate of 0.0612g cobalt nitrate and 0.1935g is prepared burden, be dissolved in the mixing easily of 30 milliliters of ethanol and 3 ml waters, be stirred to dissolving, again 0.2g ethylenediamine tetra-acetic acid and 0.6g citric acid are added in metal ion solution mixed in advance, add ammoniacal liquor and regulate pH value to 8, to be transferred in culture dish after this solution and solution mixing and stirring above, build with preservative film, freezing at-60 DEG C, the sample freezed is put into freeze drier, vacuumize, dry 24h, obtain in spongiform white pigmented samples, 10h is calcined at sample being put into 700 DEG C, formula stove, be prepared into end product.
Claims (3)
1. a preparation method for freeze drying doping vario-property lithium titanate, is characterized in that, comprises the steps:
(1) first weigh the soluble compound of Li and Ti, add distilled water and dissolve, then weigh shitosan and join in glacial acetic acid solution, ultrasonic to being dissolved as homogeneous weak yellow liquid completely;
(2) in chitosan solution, add the compound of titania powder and Yb, ultrasonic, magnetic agitation 5 minutes; Add in the solution that step (1) dissolved in chitosan solution, ultrasonic agitation 5 minutes;
(3) in step (2) solution, add certain epoxychloropropane, continuing magnetic force stirs 1 ~ 3 hour;
(4) by the soluble compound of Ba, Sr, Co and Fe, prepare burden according to mol ratio Ba:Sr:Co:Fe:=0.5:0.5:0.8:0.2, add the ethanol and water mixed liquid that prepare in advance, be stirred to and dissolve completely;
(5) by two component chelating agent and water premix, add ammoniacal liquor after mixing and all dissolve to chelating agent, then add the mixed liquor of step (4);
(6) will move in culture dish after step (5) and (3) mixing, build with preservative film, freezing at-60 DEG C, the sample freezed is put into freeze drier, vacuumize dry 24 hours, crucible put into by dried sample, calcines 8 ~ 10 hours for 500 ~ 700 DEG C under feeding tube furnace.
2. the preparation method of a kind of freeze drying doping vario-property lithium titanate according to claim 1, it is characterized in that, described lithium titanate material is Ba
0.5sr
0.5co
0.2fe
0.8o
3coated Li
4yb
pti
5-po
12, 0.1 < p≤0.2 in formula, 0.01 < Ba:Li≤0.1.
3. the preparation method of a kind of freeze drying doping vario-property lithium titanate according to claim 1, it is characterized in that, described Yb compound is ytterbium nitrate or ytterbium oxide.
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Cited By (3)
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| 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 |
| CN110563031A (en) * | 2019-09-16 | 2019-12-13 | 广东工业大学 | Lithium titanate negative electrode material, preparation method thereof and battery |
| CN111092219A (en) * | 2019-12-20 | 2020-05-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of modified lithium titanate negative electrode material applied to lithium ion battery |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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