CN105261746A - Preparation process of lithium titanate - Google Patents
Preparation process of lithium titanate Download PDFInfo
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- CN105261746A CN105261746A CN201510678478.4A CN201510678478A CN105261746A CN 105261746 A CN105261746 A CN 105261746A CN 201510678478 A CN201510678478 A CN 201510678478A CN 105261746 A CN105261746 A CN 105261746A
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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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- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
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- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a preparation process of lithium titanate. The preparation process comprises the following steps of preparing a solvent, preparing a lithium titanate solute, transferring the solvent, the solute and titanium dioxide into a spherulitic graphite tank, and carrying out one-time ball milling, drying, smashing, one-time sintering, second-time ball milling, atomization and second-time sintering. The lithium titanate material prepared according to the method is applied to a lithium battery prepared from a cathode material, and the lithium battery is high in discharging performance and stability performance. The preparation process is simple in operation and is friendly to environment, the production cost is reduced, and industrial production is promoted.
Description
Technical field
The present invention relates to lithium battery material field, particularly, relate to a kind of preparation technology of lithium titanate.
Background technology
Along with the fast development of traffic, communication and the industrialization of information, the products such as electric automobile, notebook computer and mobile communications tool propose higher and very urgent requirement to Development of Novel chemical power source.Development of new secondary green battery has become and must need.Lithium ion battery is relative to traditional secondary battery, due to its have that energy density is high, power density is high, operating voltage is high, self-discharge rate is low, memory-less effect, have extended cycle life, the unique advantage such as pollution-free, become rapidly a kind of most important and state-of-the-art secondary cell.Having become the ideal source of the electronic installation miniaturization ands such as video camera, mobile phone, notebook computer and portable surveying instrument, is also the first-selected power supply of following light high-energy electrokinetic cell used for electric vehicle.
At present, in commercial Li-ion battery, great majority adopt carbon electrode as negative material.But because the current potential in the current potential of carbon electrode after slotting lithium and metal is very close, and most electrolyte is unstable under this current potential, and electrolyte easily decomposes at electrode surface.So when over-charging of battery, carbon electrodes easily separates out very active lithium metal, form the dendrite of lithium, the danger that barrier film causes short circuit may be pierced through, and the thermal runaway that high temperature is, affect the security performance of battery.Researcher is also to the negative material of other many lithium-ions battery, as lithium alloy, oxide, sulfide and high molecular polymer etc. are explored, at present, these materials are all undesirable, some can not solve the hidden danger in safety, and some is then that cycle performance is too poor etc.Therefore, finding the new negative material substituting carbon electrode is, one of Main way of research at present.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation technology with high-rate discharge ability, lithium titanate that stability is good.
The present invention's adopted technical scheme that solves the problem is: the preparation technology of lithium titanate, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:1 ~ 1:5;
2), the preparation of solute: lithium carbonate is stirred into suspension-turbid liquid;
3), by step 1), rapid 2) in solvent, solute be transferred to ball grinder together with titanium dioxide;
4) a, ball milling: the material prepared in step 3) is carried out ball milling;
5), dry: the material completing ball milling in step 4) is transferred in basin, is placed in drying box;
6), broken: with mortar by broken for the lump material obtained in step 5), until there is no obvious bulk material, to be then transferred to porcelain boat;
7), once sintered: gained material in step 6) is sintered in air atmosphere;
8), secondary ball milling: polyethylene glycol, glycine are configured to solution, are transferred to together with gained material in step 7) in ball grinder and carry out ball milling;
9), atomization: the slurry of gained in step 8) is carried out atomization drying, and air inlet, air outlet temperature are set to 350 DEG C, 140 DEG C respectively, and atomization terminates rear gained powder and is transferred to porcelain boat;
10), double sintering: gained material in step 7 is sintered under nitrogen and hydrogen mixture atmosphere.
Further, polyethylene glycol, magnesium acetate be 1:2 ~ 1:3 in mass percent.
Further, Ball-milling Time 2 hours, the frequency 25Hz of a ball milling;
Further, step 5) in drying box 60 DEG C dry 12 hours.
Further, the sintering time that step 7) is once sintered 4 hours, temperature 400 DEG C.
Further, Ball-milling Time 2 hours, the frequency 25Hz of secondary ball milling.
Further, sintering time 10 hours, the temperature 800 DEG C of double sintering.
To sum up, the invention has the beneficial effects as follows:
1, of the present invention simple to operate, and environmentally friendly, reduce production cost, be easy to suitability for industrialized production.
2, the lithium titanate material that prepared by the present invention is applied to lithium battery discharge performance that positive electrode makes, stability is good.
Embodiment
Below in conjunction with embodiment, to the detailed description further of invention do, but embodiments of the present invention are not limited thereto.
Embodiment 1:
The preparation technology of lithium titanate, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:1;
2), the preparation of solute: lithium carbonate is stirred into suspension-turbid liquid;
3), by step 1), rapid 2) in solvent, solute be transferred to ball grinder together with titanium dioxide;
4) a, ball milling: the material prepared in step 3) is carried out ball milling, Ball-milling Time 2 hours, frequency 25Hz;
5), dry: the material completing ball milling in step 4) is transferred in basin, be placed in 60 DEG C, drying box and dry 12 hours;
6), broken: with mortar by broken for the lump material obtained in step 5), until there is no obvious bulk material, to be then transferred to porcelain boat;
7), once sintered: gained material in step 6) to be sintered in air atmosphere, sintering time 4 hours, temperature 400 DEG C;
8), secondary ball milling: polyethylene glycol, glycine are configured to solution, are transferred to together with gained material in step 7) in ball grinder and carry out ball milling, Ball-milling Time 2 hours, frequency 25Hz;
9), atomization: the slurry of gained in step 8) is carried out atomization drying, and air inlet, air outlet temperature are set to 350 DEG C, 140 DEG C respectively, and atomization terminates rear gained powder and is transferred to porcelain boat;
10), double sintering: gained material in step 7 is sintered under nitrogen and hydrogen mixture atmosphere, sintering time 10 hours, temperature 800 DEG C.
Embodiment 2:
The preparation technology of lithium titanate, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:2;
2), the preparation of solute: lithium carbonate is stirred into suspension-turbid liquid;
3), by step 1), rapid 2) in solvent, solute be transferred to ball grinder together with titanium dioxide;
4) a, ball milling: the material prepared in step 3) is carried out ball milling, Ball-milling Time 2 hours, frequency 25Hz;
5), dry: the material completing ball milling in step 4) is transferred in basin, be placed in 60 DEG C, drying box and dry 12 hours;
6), broken: with mortar by broken for the lump material obtained in step 5), until there is no obvious bulk material, to be then transferred to porcelain boat;
7), once sintered: gained material in step 6) to be sintered in air atmosphere, sintering time 4 hours, temperature 400 DEG C;
8), secondary ball milling: polyethylene glycol, glycine are configured to solution, are transferred to together with gained material in step 7) in ball grinder and carry out ball milling, Ball-milling Time 2 hours, frequency 25Hz;
9), atomization: the slurry of gained in step 8) is carried out atomization drying, and air inlet, air outlet temperature are set to 350 DEG C, 140 DEG C respectively, and atomization terminates rear gained powder and is transferred to porcelain boat;
10), double sintering: gained material in step 7 is sintered under nitrogen and hydrogen mixture atmosphere, sintering time 10 hours, temperature 800 DEG C.
Embodiment 3:
The preparation technology of lithium titanate, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:3;
2), the preparation of solute: lithium carbonate is stirred into suspension-turbid liquid;
3), by step 1), rapid 2) in solvent, solute be transferred to ball grinder together with titanium dioxide;
4) a, ball milling: the material prepared in step 3) is carried out ball milling, Ball-milling Time 2 hours, frequency 25Hz;
5), dry: the material completing ball milling in step 4) is transferred in basin, be placed in 60 DEG C, drying box and dry 12 hours;
6), broken: with mortar by broken for the lump material obtained in step 5), until there is no obvious bulk material, to be then transferred to porcelain boat;
7), once sintered: gained material in step 6) to be sintered in air atmosphere, sintering time 4 hours, temperature 400 DEG C;
8), secondary ball milling: polyethylene glycol, glycine are configured to solution, are transferred to together with gained material in step 7) in ball grinder and carry out ball milling, Ball-milling Time 2 hours, frequency 25Hz;
9), atomization: the slurry of gained in step 8) is carried out atomization drying, and air inlet, air outlet temperature are set to 350 DEG C, 140 DEG C respectively, and atomization terminates rear gained powder and is transferred to porcelain boat;
10), double sintering: gained material in step 7 is sintered under nitrogen and hydrogen mixture atmosphere, sintering time 10 hours, temperature 800 DEG C.
Embodiment 4:
The preparation technology of lithium titanate, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:5;
2), the preparation of solute: lithium carbonate is stirred into suspension-turbid liquid;
3), by step 1), rapid 2) in solvent, solute be transferred to ball grinder together with titanium dioxide;
4) a, ball milling: the material prepared in step 3) is carried out ball milling, Ball-milling Time 2 hours, frequency 25Hz;
5), dry: the material completing ball milling in step 4) is transferred in basin, be placed in 60 DEG C, drying box and dry 12 hours;
6), broken: with mortar by broken for the lump material obtained in step 5), until there is no obvious bulk material, to be then transferred to porcelain boat;
7), once sintered: gained material in step 6) to be sintered in air atmosphere, sintering time 4 hours, temperature 400 DEG C;
8), secondary ball milling: polyethylene glycol, glycine are configured to solution, are transferred to together with gained material in step 7) in ball grinder and carry out ball milling, Ball-milling Time 2 hours, frequency 25Hz;
9), atomization: the slurry of gained in step 8) is carried out atomization drying, and air inlet, air outlet temperature are set to 350 DEG C, 140 DEG C respectively, and atomization terminates rear gained powder and is transferred to porcelain boat;
10), double sintering: gained material in step 7 is sintered under nitrogen and hydrogen mixture atmosphere, sintering time 10 hours, temperature 800 DEG C.
As mentioned above, the present invention can be realized preferably.
Claims (7)
1. the preparation technology of lithium titanate, is characterized in that, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:1 ~ 1:5;
2), the preparation of solute: lithium carbonate is stirred into suspension-turbid liquid;
3), by step 1), rapid 2) in solvent, solute be transferred to ball grinder together with titanium dioxide;
4) a, ball milling: the material prepared in step 3) is carried out ball milling;
5), dry: the material completing ball milling in step 4) is transferred in basin, is placed in drying box;
6), broken: with mortar by broken for the lump material obtained in step 5), until there is no obvious bulk material, to be then transferred to porcelain boat;
7), once sintered: gained material in step 6) is sintered in air atmosphere;
8), secondary ball milling: polyethylene glycol, glycine are configured to solution, are transferred to together with gained material in step 7) in ball grinder and carry out ball milling;
9), atomization: the slurry of gained in step 8) is carried out atomization drying, and air inlet, air outlet temperature are set to 350 DEG C, 140 DEG C respectively, and atomization terminates rear gained powder and is transferred to porcelain boat;
10), double sintering: gained material in step 7 is sintered under nitrogen and hydrogen mixture atmosphere.
2. the preparation technology of lithium titanate according to claim 1, is characterized in that, described polyethylene glycol, magnesium acetate be 1:2 ~ 1:3 in mass percent.
3. the preparation technology of lithium titanate according to claim 1, is characterized in that, the Ball-milling Time 2 hours of a described ball milling, frequency 25Hz.
4. the preparation technology of lithium titanate according to claim 1, is characterized in that, described step 5) in drying box 60 DEG C dry 12 hours.
5. the preparation technology of lithium titanate according to claim 1, is characterized in that, sintering time 4 hours, temperature 400 DEG C that described step 7) is once sintered.
6. the preparation technology of lithium titanate according to claim 1, is characterized in that, the Ball-milling Time 2 hours of described secondary ball milling, frequency 25Hz.
7., according to the preparation technology of the arbitrary described lithium titanate of claim 1 to 6, it is characterized in that, the sintering time 10 hours of described double sintering, temperature 800 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510678478.4A CN105261746A (en) | 2015-10-20 | 2015-10-20 | Preparation process of lithium titanate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510678478.4A CN105261746A (en) | 2015-10-20 | 2015-10-20 | Preparation process of lithium titanate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745223A (en) * | 2017-03-16 | 2017-05-31 | 东北大学 | Modifying titanium dioxide raw powder's production technology and modifying titanium dioxide powder |
| CN107394069A (en) * | 2017-06-09 | 2017-11-24 | 镇江宇神动力能源有限公司 | A kind of Li-ion batteries piles device |
| CN108946799A (en) * | 2018-09-26 | 2018-12-07 | 山东精工电子科技有限公司 | The method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130029228A1 (en) * | 2005-07-07 | 2013-01-31 | Hiroki Inagaki | Negative electrode active material , nonaqueous electrolyte battery, battery pack and vehicle |
| CN103474645A (en) * | 2013-09-22 | 2013-12-25 | 四川科能锂电有限公司 | Preparation method for lithium titanate |
| CN103779549A (en) * | 2012-10-18 | 2014-05-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of lithium ion batteryelectrode material nano lithium titanate with uniformly-dispersed particles |
| CN104409712A (en) * | 2014-09-19 | 2015-03-11 | 四川省有色冶金研究院有限公司 | Preparation method of carbon and nitrogen coated lithium titanate material |
-
2015
- 2015-10-20 CN CN201510678478.4A patent/CN105261746A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130029228A1 (en) * | 2005-07-07 | 2013-01-31 | Hiroki Inagaki | Negative electrode active material , nonaqueous electrolyte battery, battery pack and vehicle |
| CN103779549A (en) * | 2012-10-18 | 2014-05-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of lithium ion batteryelectrode material nano lithium titanate with uniformly-dispersed particles |
| CN103474645A (en) * | 2013-09-22 | 2013-12-25 | 四川科能锂电有限公司 | Preparation method for lithium titanate |
| CN104409712A (en) * | 2014-09-19 | 2015-03-11 | 四川省有色冶金研究院有限公司 | Preparation method of carbon and nitrogen coated lithium titanate material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745223A (en) * | 2017-03-16 | 2017-05-31 | 东北大学 | Modifying titanium dioxide raw powder's production technology and modifying titanium dioxide powder |
| CN107394069A (en) * | 2017-06-09 | 2017-11-24 | 镇江宇神动力能源有限公司 | A kind of Li-ion batteries piles device |
| CN108946799A (en) * | 2018-09-26 | 2018-12-07 | 山东精工电子科技有限公司 | The method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate |
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Application publication date: 20160120 |