CN106920958A - A kind of lithium titanate preparation method - Google Patents
A kind of lithium titanate preparation method Download PDFInfo
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- CN106920958A CN106920958A CN201510993021.2A CN201510993021A CN106920958A CN 106920958 A CN106920958 A CN 106920958A CN 201510993021 A CN201510993021 A CN 201510993021A CN 106920958 A CN106920958 A CN 106920958A
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- lithium titanate
- lithium
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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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- 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 present invention is a kind of lithium titanate preparation method, is comprised the following steps：Step 1：The fourth fat of metatitanic acid four and lithium carbonate of certain mass are weighed respectively；Step 2：In ethylene glycol it is agitating solution A by the fourth liposoluble of metatitanic acid four, lithium carbonate is dissolved in ultra-pure water for solution B；Step 3：Solution A is mixed with B solution carries out back flow reaction with the first preset temperature and the first Preset Time, then filters, and powder is vacuum dried in the second preset temperature, obtains lithium titanate precursor；Step 4：Lithium titanate precursor is baked into the lithium titanate that the second Preset Time obtains target product nano-sheet in tube furnace with the 3rd preset temperature.The present invention selects lithium carbonate (Li in lithium source selection2CO3) for lithium source ensures that crystal grain is small and be uniformly distributed and optimize Li/Ti molal weights than etc., synthesized high reversible capacity, high-purity nano-sheet lithium titanate, the features such as the nanometer sheet lithium titanate for synthesizing has high reversible capacity, long circulation life.
Description
【Technical field】
The present invention relates to technical field of lithium batteries, more particularly to a kind of lithium titanate preparation method.
【Background technology】
At present, electric automobile is gradually being promoted and will had broad prospects in future, and lithium battery is used as electronic
One of technology of automobile most critical, its performance quality influences great to vehicle.Traditional lithium ion battery is used
The carbon materials such as graphite often have that cycle life is short and the significant deficiency such as security difference as negative pole.And point is brilliant
Stone Li4Ti5012The Li that (lithium titanate) negative pole is generated in process of intercalation7Ti5O12Also it is spinel structure, it is brilliant
Born of the same parents' parameter a is varied less, and it is a kind of " zero volume strain " material that Unit cell volume only changes 0.3%；Lithium
During ion deinsertion, material Li4Ti5O12Skeleton structure be substantially stabilization, therefore Li4Ti5O12Energy
Enough avoid in charge and discharge cycles, structural damage is caused due to stretching back and forth for electrode material, so as to improve
The cycle performance and service life of electrode.Spinel-type Li4Ti5O12(lithium titanate) is because with excellent circulation
Property, the change of security, zero volume and cheap cost turn into the focus of research at present, the metatitanic acid for preparing at present
Lithium capacity typically (presses C in 160mAh/g-175mAh/gIt is theoretical=26.8nm/M is calculated) between, but it is reversible
Capacity only has 130mAh/g-150mAh/g, causes lithium titanate battery energy density low, adds nanoparticle titanium
Sour lithium granularity is difficult to control, and causes size distribution uneven, influences its electrical property.The point of common method synthesis is brilliant
Stone lithium titanate reversible capacity is low, impure phase, size distribution is unequal causes lithium titanate class battery in power electric
Pond application is limited.Therefore, synthetic method, the selection of lithium source, Li/Ti molal weights ratio, bake time control,
Size distribution etc. affects the physical and chemical performance of lithium titanate.The lithium source used by synthesis lithium titanate is lithia at present,
Cause product particle size big, high rate performance is poor；Titanium dioxide is the formation reduction metatitanic acid of its influence impurities phase of titanium source
Lithium purity has a strong impact on its big circulation performance；Irrational Li/Ti molal weights are than influence reversible capacity hair
Wave；Not strict control crystal nucleation time and temperature, cause size distribution unequal.
In consideration of it, real be necessary to provide a kind of new lithium titanate preparation method to overcome the deficiencies in the prior art.
【The content of the invention】
It is an object of the invention to provide a kind of lithium titanate preparation method with high reversible capacity.
To achieve these goals, the present invention provides a kind of lithium titanate preparation method, comprises the following steps：
Step 1：The fourth fat of metatitanic acid four and lithium carbonate of certain mass are weighed respectively；
Step 2：In ethylene glycol it is agitating solution A by the fourth liposoluble of metatitanic acid four, lithium carbonate is dissolved in ultra-pure water is
Solution B；
Step 3：Solution A is mixed with B solution and is returned with the first preset temperature and the first Preset Time
Stream reaction, is then filtered, and powder is vacuum dried in the second preset temperature, obtains lithium titanate precursor；
Step 4：Lithium titanate precursor is baked into the second Preset Time with the 3rd preset temperature in tube furnace to obtain
The lithium titanate of target product nano-sheet.
The present invention selects lithium carbonate (Li in lithium source selection2CO3) for lithium source ensure crystal grain it is small and be uniformly distributed,
And optimize Li/Ti molal weights ratio etc., synthesized high reversible capacity, high-purity nano-sheet lithium titanate, close
The features such as there is high reversible capacity, long circulation life into the nanometer sheet lithium titanate for going out.
【Brief description of the drawings】
Fig. 1 is the X-ray monocrystalline of the lithium titanate made by preferred embodiment for the present invention lithium titanate preparation method
Diffraction pattern.
Fig. 2 is the electron scanning electricity of the lithium titanate made by preferred embodiment for the present invention lithium titanate preparation method
Mirror figure.
Fig. 3 is that the lithium titanate made by preferred embodiment for the present invention lithium titanate preparation method is further made
The curve of double curvature of button cell.
Fig. 4 is that the lithium titanate made by preferred embodiment for the present invention lithium titanate preparation method is further made
The cyclic curve of button cell.
【Specific embodiment】
In order that the purpose of the present invention, technical scheme and Advantageous Effects become apparent from understanding, below in conjunction with
The drawings and specific embodiments, the present invention will be described in further detail.It should be appreciated that this explanation
Specific embodiment described in book is not intended to limit the present invention just for the sake of explaining the present invention.
The present invention is the lithium titanate for preparing high reversible capacity, high-purity, selection lithium carbonate (Li2CO3) it is lithium
Source, the fourth fat (Ti (OC of metatitanic acid four4H9)4) for titanium source, ethylene glycol be solvent, process reaction equation：
Ti(OC4H9)4+2H2O→TiO2+4C4H9OH (1)
Li2CO3→Li2O+H2O (2)
Li2O+TiO2→Li2TiO3 (3)
2Li2TiO3+3TiO2→3Li4Ti5O12 (4)
Lithium titanate preparation method of the present invention specifically includes following steps：
Step 1：Fourth fat (Ti (the OC of metatitanic acid four of certain mass are weighed respectively4H9)4) and lithium carbonate (Li2CO3)；
In this step, the fourth fat (Ti (OC of metatitanic acid four for weighing4H9)4) and lithium carbonate (Li2CO3) molal weight ratio is
Li/Ti=0.82.
Step 2：By the fourth fat (Ti (OC of metatitanic acid four4H9)4) ethylene glycol is dissolved in for agitating solution A, by lithium carbonate
(Li2CO3) be dissolved in ultra-pure water for solution B；
Step 3：Solution A is mixed with B solution and is returned with the first preset temperature and the first Preset Time
Stream reaction, is then filtered, and powder is vacuum dried in the second preset temperature, obtains lithium titanate precursor；
In this step, the first preset temperature is 200 DEG C, and the first Preset Time is 15h (hour), and the powder is
Li2TiO3、3TiO2Mixture, second preset temperature is 105 DEG C.Back flow reaction is in organic solvent
The common method of mineral products is prepared, reaction temperature adds to solvent boiling point or so, it is ensured that the maximum of solvent
Activity and to the dissolubility of reactant.
Step 4：Lithium titanate precursor is baked into the second Preset Time with the 3rd preset temperature in tube furnace to obtain
The lithium titanate of target product nano-sheet.In this step, the 3rd preset temperature is 800 DEG C, the second Preset Time
It is 24h.
Data explanation：
1st, knowable to the X-ray single crystal diffraction figure of Fig. 1, with standard card contrast, only metatitanic acid crystalline lithium spreads out
Peak is penetrated, the presence at free from admixture peak shows that the product for synthesizing is pure lithium titanate；
2nd, knowable to the electron scanning Electronic Speculum map analysis of Fig. 2, product lithium titanate is nano-sheet, and thickness only has
20-50nm, it is very big to improve the specific surface of material in degree, increase the ion and electronic conductivity of material, be conducive to
The performance of capacity；
3rd, the lithium titanate of the nano-sheet of preparation is prepared into button cell, such as positive pole lithium titanate sample, lead
Electric agent acetylene black and polyvinylidene fluoride (PVDF 5130) bonding agent press 8:1:The well mixed system of 1 mass ratio
Piece, negative pole is lithium metal disk, knowable to the curve of double curvature analysis of Fig. 3, nanometer sheet lithium titanate high rate performance
It is excellent, excellent invertibity can be remain under 30C multiplying powers with big circulation；
4th, knowable to the cyclic curve analysis of Fig. 4, reversible capacity can also keep nearly 177 after 1C is circulated 110 weeks
MAh/g, and Lithium-ion embeding abjection is basically identical, illustrates that the nanometer sheet lithium titanate for synthesizing has reversible appearance high
The features such as amount, long circulation life.
The present invention is not restricted to described in specification and implementation method, therefore for the personnel of familiar field
For be easily achieved additional advantage and modification, therefore limited without departing substantially from claim and equivalency range
Universal spirit and scope in the case of, the present invention is not limited to specific details, representational sets
It is standby and shown here as the examples shown with description.
Claims (4)
1. a kind of lithium titanate preparation method, comprises the following steps：
Step 1：The fourth fat of metatitanic acid four and lithium carbonate of certain mass are weighed respectively；
Step 2：In ethylene glycol it is agitating solution A by the fourth liposoluble of metatitanic acid four, lithium carbonate is dissolved in ultra-pure water is
Solution B；
Step 3：Solution A is mixed with B solution and is returned with the first preset temperature and the first Preset Time
Stream reaction, is then filtered, and powder is vacuum dried in the second preset temperature, obtains lithium titanate precursor；
Step 4：Lithium titanate precursor is baked into the second Preset Time with the 3rd preset temperature in tube furnace to obtain
The lithium titanate of target product nano-sheet.
2. lithium titanate preparation method as claimed in claim 1, it is characterised in that：The titanium weighed in step 1
Sour four fourth fat are Li/Ti=0.82 with lithium carbonate molal weight ratio.
3. lithium titanate preparation method as claimed in claim 1, it is characterised in that：First presets in step 3
Temperature is 200 DEG C, and the first Preset Time is 15 hours, and the powder is Li2TiO3、3TiO2Mixture,
Second preset temperature is 105 DEG C.
4. battery pack as claimed in claim 1, it is characterised in that：The 3rd preset temperature is 800 in step 4
DEG C, the second Preset Time is 24 hours.
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| CN201510993021.2A CN106920958A (en) | 2015-12-27 | 2015-12-27 | A kind of lithium titanate preparation method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102130324A (en) * | 2011-01-05 | 2011-07-20 | 上海大学 | Preparation method of lithium titanate/carbon nano tube composite cathode material |
| CN102169980A (en) * | 2010-02-27 | 2011-08-31 | 比亚迪股份有限公司 | Preparation method of anode active material |
| CN104577046A (en) * | 2014-12-31 | 2015-04-29 | 江苏江大环保科技开发有限公司 | Application of graphene/lithium titanate composite |
-
2015
- 2015-12-27 CN CN201510993021.2A patent/CN106920958A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102169980A (en) * | 2010-02-27 | 2011-08-31 | 比亚迪股份有限公司 | Preparation method of anode active material |
| CN102130324A (en) * | 2011-01-05 | 2011-07-20 | 上海大学 | Preparation method of lithium titanate/carbon nano tube composite cathode material |
| CN104577046A (en) * | 2014-12-31 | 2015-04-29 | 江苏江大环保科技开发有限公司 | Application of graphene/lithium titanate composite |
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Application publication date: 20170704 |