CN104810515A - Preparation method of doped Li4Ti5O12 anode material - Google Patents
Preparation method of doped Li4Ti5O12 anode material Download PDFInfo
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- CN104810515A CN104810515A CN201510174894.0A CN201510174894A CN104810515A CN 104810515 A CN104810515 A CN 104810515A CN 201510174894 A CN201510174894 A CN 201510174894A CN 104810515 A CN104810515 A CN 104810515A
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- lithium
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- lithium titanate
- titanic acid
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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
- 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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 relates to the technical field of preparation of lithium ion battery electrode materials, and particularly discloses a preparation method of a doped Li4Ti5O12 anode material. According to the method, a Li source, nano-silica and glucose in certain material ratio are added to a ball mill and subjected to ball-milling with absolute ethyl alcohol as a medium, then a product is subjected to spray-drying and calcined under the condition of inert atmosphere, and a product is subjected to ball-milling and sieving to obtain the doped Li4Ti5O12 anode material. The doped Li4Ti5O12 anode material shows excellent electrochemical performance when applied to a lithium ion battery anode material. The preparation process is simple, and the prepared anode material has high reversible capacity, high-rate cycle performance and excellent rate charge and discharge performance.
Description
Technical field
The present invention relates to the preparing technical field of lithium ion battery electrode material, be specifically related to a kind of preparation method of doped titanic acid lithium titanate cathode material.
Background technology
Be widely used in mobile phone at present, it is large that lithium ion battery in the electronic products such as notebook computer has specific energy, specific power is high, self discharge is little, good and the quickly-chargeable of cycle characteristics and efficiency is high, operating temperature range is wide, the advantages such as non-environmental-pollution, lithium ion battery used in the market, substantially be all be negative pole with material with carbon element, but material with carbon element is negative pole also has some to be difficult to the weakness overcome in actual applications, such as, react with electrolyte in discharge process formation surface passivated membrane first, cause the consumption of electrolyte and coulombic efficiency is lower first, the current potential of carbon electrode and the current potential of lithium metal very close, when the battery is overcharged, the easy precipitating metal lithium of carbon electrodes, thus may short circuit be caused, and then cause battery explosion.In order to solve the safety problem of lithium battery, people have done large quantifier elimination.Spinel Li4Ti5O12 is as a kind of novel ion secondary battery cathode material lithium, compared with other business-like material, advantages such as having good cycle, do not react with electrolyte, security performance is high, charge and discharge platform is steady is one of the most excellent lithium ion battery negative material received much concern in recent years.
Lithium titanate (Li4Ti5O12) is a kind of " zero strain " material, and in lithium ion deintercalation and telescopiny, corresponding contraction and expansion does not occur its lattice, so material structure is highly stable, cycle performance is also better.Lithium titanate charge and discharge platform is greatly about about 1.55V, and theoretical specific capacity is 175mAh/g, and actual specific capacity can reach 165mAh/g, and capacity contribution concentrates on land regions.In addition, lithium titanate, compared with commercial carbon negative pole material, has larger diffusion coefficient under normal temperature, usually have better chemical property and fail safe.But lithium titanate poorly conductive, under high magnification environment, special capacity fade is rapid, and adulterating coated is improve the most effective means of its performance.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of brand-new lithium titanate lithium ion battery negative material.
Lithium salts, nano titanium oxide and silicon dioxide, glucose are first passed through wet ball grinding spraying dry by the present invention by a certain percentage, then calcine under inert atmosphere conditions, after ball milling screening, namely obtain lithium ion battery negative material with the cooled just sample of stove.Abundant raw material source of the present invention, preparation technology is simple, the negative material excellent conductivity prepared, and reversible capacity is high, and cycle performance is excellent.
Object of the present invention is achieved particular by following technical scheme, the preparation method of a kind of preparation method of doped titanic acid lithium titanate cathode material, and step is as follows:
(1) joining in ball mill by lithium source, nano titanium oxide and silicon dioxide, glucose according to certain material ratio, take absolute ethyl alcohol as medium ball milling 3 ~ 24 hours;
(2) by gained slurry spraying dry after ball milling, powder mixture material is obtained;
(3) gained powder mixture material is warming up to 800 ~ 900 DEG C from room temperature with the speed of 5 ~ 20 DEG C/min under an inert atmosphere, and keeps 1 ~ 3h hour, after cooling, obtain the lithium titanate composite material head product adulterated;
(4) by head product ball-milling treatment 1 ~ 4 hour in ball mill, after crossing 200 mesh sieves, the lithium titanate composite anode material of this law rice doping vario-property is namely obtained.
Described lithium source is the one in lithium acetate, lithium sulfate, lithium oxalate, lithium carbonate, lithium hydroxide.。
Described nano titanium oxide is anatase titanium dioxide, particle diameter 10 ~ 20nm, purity >99%.
Described inert atmosphere conditions is nitrogen or argon gas atmosphere.
The ratio of described lithium source (in elemental lithium), nano titanium oxide amount of substance is 1:1, add silicon dioxide, the quality of glucose be respectively lithium source, both titanium dioxide quality sum 2.5% ~ 10%, 3% ~ 5%.
Described nano silicon is the preparation of vapor phase method deposition, and its particle diameter is not more than 30 nanometers.
Compared with prior art, the advantage of the inventive method and beneficial effect are:
1. add nano silicon by original position, make it enter among lithium titanate lattice, the internal structure of modified lithium titanate material, plays the effect of skeletal support simultaneously, ensures the cyclical stability of material;
2. add glucose, after high-temperature process, the carbonaceous conductive agent of glucose carbonization forming property excellence, the deficiency of lithium titanate electric conductivity can be made up, meanwhile, the microcellular structure of material with carbon element is conducive to the quick deintercalation of lithium ion, improves high rate performance and the cryogenic property of material;
3. preparation technology of the present invention is simple, cheap, and utilization doping and the material prepared by carbon modification have the plurality of advantages such as efficiency for charge-discharge is high, discharge and recharge reaction good reversibility, Stability Analysis of Structures, cycle performance are excellent.
Embodiment
Reaching object to make technological means of the present invention, creation characteristic, workflow, using method and effect is easy to understand, below in conjunction with specific embodiment, setting forth the present invention further.
Embodiment 1
A kind of preparation method of doped titanic acid lithium titanate cathode material, step is as follows: join in ball mill by lithium hydroxide, nano titanium oxide and silicon dioxide, glucose, take absolute ethyl alcohol as medium ball milling 10 hours, wherein the ratio of the amount of substance of lithium hydroxide and nano titanium oxide is 1:1, the quality of silicon dioxide, glucose be respectively lithium hydroxide, nano titanium oxide quality sum 2.5%, 3%.By gained slurry spraying dry after ball milling, obtain powder mixture material.Gained powder mixture material is pressed in a nitrogen atmosphere ramp to the 800 DEG C calcining of 10 DEG C/min from room temperature, and be incubated 3 hours, after cooling, obtain lithium titanate composite material head product.By head product ball-milling treatment 3 hours in ball mill, after crossing 200 mesh sieves, namely obtain doped titanic acid lithium titanate cathode material prepared by the present invention.
Embodiment 2
A kind of preparation method of doped titanic acid lithium titanate cathode material, step is as follows: join in ball mill by lithium hydroxide, nano titanium oxide and silicon dioxide, glucose, take absolute ethyl alcohol as medium ball milling 8 hours, wherein the ratio of the amount of substance of lithium hydroxide and nano titanium oxide is 1:1, the quality of silicon dioxide, glucose be respectively lithium hydroxide, nano titanium oxide quality sum 5%, 4%.By gained slurry spraying dry after ball milling, obtain powder mixture material.Gained powder mixture material is pressed in a nitrogen atmosphere ramp to the 900 DEG C calcining of 5 DEG C/min from room temperature, and be incubated 2 hours, after cooling, obtain lithium titanate composite material head product.By head product ball-milling treatment 4 hours in ball mill, after crossing 200 mesh sieves, namely obtain doped titanic acid lithium titanate cathode material prepared by the present invention.
Embodiment 3
A kind of preparation method of doped titanic acid lithium titanate cathode material, step is as follows: join in ball mill by lithium hydroxide, nano titanium oxide and silicon dioxide, glucose, take absolute ethyl alcohol as medium ball milling 10 hours, wherein the ratio of the amount of substance of lithium hydroxide and nano titanium oxide is 1:1, the quality of silicon dioxide, glucose be respectively lithium hydroxide, nano titanium oxide quality sum 10%, 5%.By gained slurry spraying dry after ball milling, obtain powder mixture material.Gained powder mixture material is pressed in a nitrogen atmosphere ramp to the 850 DEG C calcining of 8 DEG C/min from room temperature, and be incubated 3 hours, after cooling, obtain lithium titanate composite material head product.By head product ball-milling treatment 4 hours in ball mill, after crossing 200 mesh sieves, namely obtain doped titanic acid lithium titanate cathode material prepared by the present invention.
Embodiment 4
A kind of preparation method of doped titanic acid lithium titanate cathode material, step is as follows: join in ball mill by lithium hydroxide, nano titanium oxide and silicon dioxide, glucose, take absolute ethyl alcohol as medium ball milling 10 hours, wherein the ratio of the amount of substance of lithium hydroxide and nano titanium oxide is 1:1, the quality of silicon dioxide, glucose be respectively lithium hydroxide, nano titanium oxide quality sum 6%, 4%.By gained slurry spraying dry after ball milling, obtain powder mixture material.Gained powder mixture material is pressed in a nitrogen atmosphere ramp to the 850 DEG C calcining of 15 DEG C/min from room temperature, and be incubated 2.5 hours, after cooling, obtain lithium titanate composite material head product.By head product ball-milling treatment 2.5 hours in ball mill, after crossing 200 mesh sieves, namely obtain doped titanic acid lithium titanate cathode material prepared by the present invention.
Comparative example 1
Being that 1:1 joins in ball mill by lithium hydroxide, nano titanium oxide by the ratio of amount of substance, take absolute ethyl alcohol as medium ball milling 1 hour.By gained slurry spraying dry after ball milling, obtain powder mixture material.Gained powder mixture material is pressed under an argon atmosphere ramp to the 800 DEG C calcining of 10 DEG C/min from room temperature, and be incubated 3 hours, after cooling, obtain lithium titanate head product.By head product ball-milling treatment 4 hours in ball mill, after crossing 200 mesh sieves, namely obtain lithium titanate material.
Respectively the lithium ion battery negative material that embodiment 1 ~ 4 and comparative example 1 obtain is made half-cell and carry out chemical property mensuration, half-cell assembly method is as follows: be 80wt%:15wt%:5wt% mixing in mass ratio by testing sample, S P, conductive black and polyvinylidene fluoride, mix well with N-methyl pyrrolidone, stir into thick, be coated on Copper Foil, at 80 DEG C, vacuum (-0.1MPa), drying 20 hours, is cut into the circular film that diameter is about 1cm after cooling.Half-cell adopts CR2016 type button cell to assemble in glove box, barrier film is Celgard 2400 polypropylene diaphragm, electrolyte is that (in mixed electrolytic solution, the volume ratio of EC, DEC is 1:1 with diethyl carbonate (DEC) mixed electrolytic solution for the ethylene carbonate (EC) of 1M LiPF6, in mixed electrolytic solution, LiPF6 concentration is 1M), be circular lithium sheet (diameter 1.5cm) of commercialization to electrode, be assembled into battery.Charging/discharging voltage is 1.0 ~ 2.5V, and charge-discharge velocity is 0.5C, and carry out testing to battery performance, test result is in table 1.
Table 1 is the Performance comparision of negative material in different embodiment and comparative example
More than show and describe general principle of the present invention and principal character and advantage of the present invention; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and application claims protection range is defined by appending claims and equivalent thereof.
Claims (6)
1. a preparation method for doped titanic acid lithium titanate cathode material, step is as follows:
(1) joining in ball mill by lithium source, nano titanium oxide and silicon dioxide, glucose according to certain material ratio, take absolute ethyl alcohol as medium ball milling 3 ~ 24 hours;
(2) by gained slurry spraying dry after ball milling, powder mixture material is obtained;
(3) by gained powder mixture material under an inert atmosphere from room temperature with certain heating rate to 800 ~ 900 DEG C, and keep 1 ~ 3h hour, after cooling, obtain the lithium titanate composite material head product adulterated;
(4) by head product ball-milling treatment 1 ~ 4 hour in ball mill, after crossing 200 mesh sieves, the lithium titanate composite anode material of this law rice doping vario-property is namely obtained.
2. according to the preparation method of a kind of doped titanic acid lithium titanate cathode material described in claim 1, it is characterized in that: the described lithium source of step (1) is the one in lithium acetate, lithium sulfate, lithium oxalate, lithium carbonate, lithium hydroxide.
3. according to the preparation method of a kind of doped titanic acid lithium titanate cathode material described in claim 1, it is characterized in that: the ratio of described lithium source (in elemental lithium), nano titanium oxide amount of substance is 1:1, add silicon dioxide, the quality of glucose is respectively lithium source, both titanium dioxide quality sum 2.5% ~ 10%, 3% ~ 5%.
4. according to the preparation method of a kind of doped titanic acid lithium titanate cathode material described in claim 1, it is characterized in that: the nano silicon described in step (1) is the preparation of vapor phase method deposition, and its particle diameter is not more than 30 nanometers.
5. according to the preparation method of a kind of doped titanic acid lithium titanate cathode material described in claim 1, it is characterized in that: step (3) described inert atmosphere conditions is nitrogen or argon gas atmosphere.
6. according to the preparation method of a kind of doped titanic acid lithium titanate cathode material described in claim 1, it is characterized in that: the speed of the intensification described in step (3) is 5 ~ 20 DEG C/min.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510174894.0A CN104810515A (en) | 2015-04-15 | 2015-04-15 | Preparation method of doped Li4Ti5O12 anode material |
| PCT/CN2015/087970 WO2016165262A1 (en) | 2015-04-15 | 2015-08-25 | Preparation method for doped lithium titanate negative electrode material |
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| CN201510174894.0A CN104810515A (en) | 2015-04-15 | 2015-04-15 | Preparation method of doped Li4Ti5O12 anode material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016165262A1 (en) * | 2015-04-15 | 2016-10-20 | 田东 | Preparation method for doped lithium titanate negative electrode material |
| CN115440967A (en) * | 2022-10-20 | 2022-12-06 | 航天锂电科技(江苏)有限公司 | Large-cylinder lithium ion power battery cathode material and preparation method thereof |
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| CN111403724B (en) * | 2020-04-21 | 2022-03-29 | 旭派电源有限公司 | Modified N, P co-doped lithium titanate negative electrode material and preparation method thereof |
| CN111747453A (en) * | 2020-05-15 | 2020-10-09 | 北方奥钛纳米技术有限公司 | Nickel-doped lithium titanate, preparation method and application thereof |
| CN112670470B (en) * | 2020-12-20 | 2022-10-11 | 复旦大学 | Lithium titanate/graphite single alkyne composite anode material and preparation method and application thereof |
| CN113201808A (en) * | 2021-04-28 | 2021-08-03 | 中南大学 | Porous fiber silicon-oxygen negative electrode composite material and preparation method thereof |
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| CN101485015A (en) * | 2006-06-05 | 2009-07-15 | T/J技术公司 | Alkali metal titanates and methods for their synthesis |
| JP4334579B2 (en) * | 2007-03-28 | 2009-09-30 | 株式会社東芝 | Anode active material for non-aqueous electrolyte battery, non-aqueous electrolyte battery, battery pack and automobile |
| WO2009028553A1 (en) * | 2007-08-30 | 2009-03-05 | Ishihara Sangyo Kaisha, Ltd. | Titanic acid compound, process for producing the titanic acid compound, electrode active material containing the titanic acid compound, and storage device using the electrode active material |
| CN104810515A (en) * | 2015-04-15 | 2015-07-29 | 田东 | Preparation method of doped Li4Ti5O12 anode material |
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- 2015-04-15 CN CN201510174894.0A patent/CN104810515A/en active Pending
- 2015-08-25 WO PCT/CN2015/087970 patent/WO2016165262A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102299311A (en) * | 2011-07-20 | 2011-12-28 | 彩虹集团公司 | Cathode active material and preparation method thereof and lithium ion secondary battery prepared by cathode active material |
| CN103296257A (en) * | 2013-06-05 | 2013-09-11 | 深圳市斯诺实业发展有限公司永丰县分公司 | Preparation method of modified lithium titanate negative material of lithium-ion battery |
| CN103326009A (en) * | 2013-06-05 | 2013-09-25 | 深圳市斯诺实业发展有限公司永丰县分公司 | Process for preparing high capacity lithium titanate anode material |
| CN103456939A (en) * | 2013-07-24 | 2013-12-18 | 湖南大学 | Method for preparing cathode material carbon-coated lithium titanate for lithium ion battery from metatitanic acid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016165262A1 (en) * | 2015-04-15 | 2016-10-20 | 田东 | Preparation method for doped lithium titanate negative electrode material |
| CN115440967A (en) * | 2022-10-20 | 2022-12-06 | 航天锂电科技(江苏)有限公司 | Large-cylinder lithium ion power battery cathode material and preparation method thereof |
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| WO2016165262A1 (en) | 2016-10-20 |
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