CN104953107A - Preparation method of lithium titanate cathode material with high tap density - Google Patents
Preparation method of lithium titanate cathode material with high tap density Download PDFInfo
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- CN104953107A CN104953107A CN201510332155.XA CN201510332155A CN104953107A CN 104953107 A CN104953107 A CN 104953107A CN 201510332155 A CN201510332155 A CN 201510332155A CN 104953107 A CN104953107 A CN 104953107A
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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
- 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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- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 discloses a preparation method of a lithium titanate cathode material with high tap density. The preparation method comprises the following steps: weighing a lithium source and a titanate source according to the mole ratio of Li to Ti being (0.80-0.85): 1, and taking deionized water as a medium; carrying out uniform stirring and spray drying; then, carrying out high-temperature calcination, wet ball-milling, secondary spray drying, secondary high-temperature sintering, and screening to obtain the lithium titanate cathode material. The lithium titanate cathode material obtained according to the preparation method has the advantages that the tap density can be improved to 1.2 g/cm<3> or above; lithium titanate particles obtained during the preparation are spherical, solid in structure and high in dispersity.
Description
Technical field
The present invention relates to the preparation method of high-tap density lithium titanate anode material, belong to electrochemical cell electrode raw material technical field.
Background technology
Since entering 21 century, the climatic environment in the whole world constantly worsens the modern society that makes day by day in short supply with petroleum resources and is faced with formidable challenges.From the angle of the sustainable development of socio-economy, traditional energy system is hampering the development of economic society gradually, and exploitation safety, clean green energy resource system are that people are used, have become the development trend of world today's using energy source.Traditional lead-acid battery, nickel-cadmium cell have been difficult to the demand meeting market because of problems such as energy density is lower, environmental pollutions, along with the progress of science and technology, particularly the develop rapidly of the industry such as electronics, communication, space flight, automobile, more and more urgent to the demand of high-energy-density, high-specific-power, long-life, the free of contamination new chemical energy.
A new generation lithium ion battery negative material Li
4ti
5o
12plurality of advantages is had: (1) structural advantage, the Li of spinel structure as high performance electrode material
4ti
5o
12at Lithium-ion embeding with in the process of deviating from, crystal structure change in volume is very little, the stability of height can be kept, be called as " zero strain " material, there is excellent cycle performance and stable discharge voltage, theoretical specific capacity is 175mAh/g, and actual specific energy can reach 160-165mAh/g, can meet long-life, high-power requirement; (2) there is relatively high electrode potential, make Li
4ti
5o
12can use in the electrolytical burning voltage interval of most liquid as electrode material, thus avoid the generation of electrolyte decomposition phenomenon or diaphragm, under full-charge state, have good thermal stability, less moisture absorption and more smooth charge and discharge platform; (3) Li
4ti
5o
12electromotive force higher than the electromotive force of pure metal lithium, not easily produce Li dendrite, for ensureing that the safety of battery provides the foundation; (4) high temperature performance is good, Li
4ti
5o
12ion battery possesses the charging and discharging capabilities at-40 ~ 55 DEG C, and the electric current that the lithium ion battery that current graphite is negative pole discharges at-20 DEG C is just very little, substantially cannot work; (5) Li
4ti
5o
12having high lithium ion diffusion coefficient (is 2 × 10
-8cm
2/ s), can high power charging-discharging.Li
4ti
5o
12development for high-capacity lithium-ion power battery presents wide space, following use electrode material Li
4ti
5o
12lithium ion battery most possibly as electrokinetic cell obtain scale application.
Lithium titanate preparation method mainly comprises high temperature solid-state method and liquid phase method, and solid phase method is fully mixed in lithium source and titanium source, high-temperature calcination synthesis lithium titanate in sintering furnace.Compared with liquid phase method, it is cheap that solid reaction process has the prices of raw and semifnished materials, and technological requirement is simple, is easy to large-scale production, is convenient to the features such as production management.But there is tap density situation on the low side in the lithium titanate material that solid phase method conventional is at present prepared, the low specific energy of battery that causes of material tap density is lower, has had a strong impact on the quality of battery.
In view of this, the lithium titanate anode material inventing a kind of high-tap density becomes particularly important.
Summary of the invention
The object of the invention is to the defect overcoming prior art, a kind of preparation method of high-tap density lithium titanate anode material is provided, being intended to the tap density improving material by improving technical process, thus improve the energy density of battery.
To achieve these goals, the technical scheme taked of the present invention is as follows:
A preparation method for high-tap density lithium titanate anode material, its key technology is, comprises the steps:
(1) raw material mixing: the ratio being Li:Ti=0.80-0.85:1 according to the mol ratio of Li and Ti takes lithium source and titanium source respectively, is medium, stirs, obtain slurry with deionized water;
(2) spraying dry: the slurry that step (1) obtains is carried out spraying dry, the powder be uniformly mixed;
(3) high-temperature calcination: step (2) is obtained powder under 700-875 DEG C of condition, calcine 2-6h, obtain lithium titanate powder;
(4) wet ball grinding: in ball mill, take water as decentralized medium, the lithium titanate powder that step (3) obtains is dispersed into slurry, is mixed through ball milling, nano level lithium titanate slurry;
(5) secondary spraying dry: the slurry that step (4) obtains is obtained spherical micron particles by spraying dry;
(6) secondary high-temperature sintering: particle step (5) obtained is 750-850 DEG C of sintering 1-3h in revolution sintering furnace, and cooling, obtains lithium titanate material;
(7) sieve: cross 200-250 order spin vibration sieve, to obtain final product.
Further improve as the present invention, the titanium source described in described step (1) is anatase TiO
2.
Further improve as the present invention, the lithium source described in described step (1) is for being selected from LiOHH
2o, Li
2cO
3and LiNO
3in one or three kinds of mixtures.
Further improve as the present invention, described step (3) is specific as follows: be loaded into by the powder after spraying dry in SiC saggar, in air atmosphere, put into sintering furnace to calcine, holding temperature is 700-875 DEG C, temperature retention time is 2-6h, then cools, and obtains the lithium titanate powder that purity is high.
Further improve as the present invention, the average grain diameter of the micron particles in described step (5) is 5.5-11 μm.
Further improve as the present invention, described step (6) powder is 750-850 DEG C of calcining 1-3h in revolution sintering furnace, naturally cools, pass into dry air and take away moisture, obtain the lithium titanate material that moisture is less than 500ppm.
Compared with prior art, the beneficial effect acquired by the present invention is as follows:
The present invention by strictly controlling pulp furnish, obtains the powder mixed through mix and blend and spraying dry, obtain that crystal grain is complete, the lithium titanate powder of pure phase after high-temperature calcination; Again by wet ball grinding, after being ground to nano particle, through secondary spray drying granulation spheroiding particle, then through double sintering, tap density is by 0.9-1.0g/cm
3bring up to 1.2 g/cm
3above.The lithium titanate particle that this preparation method obtains is spherical, rugged construction, good dispersion.
Titanium material of the present invention is anatase TiO
2, uniform particle sizes, specific area is high, is 200-400 m
2/ g, good dispersion, has very high activity, greatly can increase by two kinds of raw-material contacts area, shortens the time of solid phase reaction, enhances productivity.
The present invention makes raw material fully mix by mix and blend and spraying dry, shortens the high temperature sintering time.
The present invention is in raw material mixing and wet ball grinding process, and decentralized medium is all deionized water, avoids the potential safety hazard used in organic system dry run.
The present invention in air atmosphere, does not need to use inert protective gas, reduces production cost in twice calcination process.
The lithium titanate that the present invention prepares has higher energy density, and half-cell first capacity reaches more than 170mAh/g, close to theoretical gram volume 175 mAh/g.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of lithium titanate material prepared by the present invention;
Fig. 2 is the scanning electron microscopic picture of lithium titanate material prepared by the present invention;
Fig. 3 is the 0.1C charging and discharging curve of lithium titanate anode material button cell prepared by the present invention.
Embodiment
Below in conjunction with embodiment, detailed further describing is carried out to the present invention.
Embodiment 1:
A preparation method for high-tap density lithium titanate anode material, it comprises the steps:
(1) raw material mixing: add deionized water 200L in a mixing bowl, carry out proportioning according to the mol ratio of Li:Ti=0.81:1, take 30kg LiOHH
2o and 80kg TiO
2dispersion in deionized water, is stirred more than 2 hours, is made it fully mix.
(2) spraying dry: the powder that the slurry stirred is uniformly mixed by spraying dry.
(3) high-temperature calcination: roller-way sintering furnace is heated up according to heating curve, powder after spraying dry is loaded in SiC saggar, in air atmosphere, put into sintering furnace to calcine, heat preservation zone temperature is 850 DEG C, temperature retention time is 4h, then naturally cools, obtains the lithium titanate powder that purity is very high.
(4) wet ball grinding: lithium titanate powder, as abrasive media, adds in dispersion cylinder, then adds deionized water, be made into slurry by the zirconium oxide bead adding 0.2-1.0mm in ball mill, ball milling 5-8h, is mixed, nano level lithium titanate suspension-turbid liquid.
(5) secondary spraying dry: strict charging rate 18%, Contact Temperature 580 DEG C, outlet temperature 125 DEG C, the technological parameter such as negative pressure-150pa in tower controlling spray drying tower, obtains the spherical micron particles of about average grain diameter 10um by spraying dry by uniform slurry.
(6) secondary clacining: calcine 1.5h in revolution sintering furnace 800 DEG C, naturally cool, pass into dry air simultaneously and take away moisture, obtain the lithium titanate material that moisture is less than 500ppm.
(7) sieve: pack after crossing 200 order spin vibration sieves.
Adopt x-ray diffractometer to carry out material phase analysis to the lithium titanate powder sample prepared, the phase purity obtained is 99.17%, and diffraction pattern as shown in Figure 1.Adopt S-4800 field emission scanning electron microscope observation pattern, as shown in Figure 2, can see that material dispersion is fine, be spheric granules, through laser particle analyzer test granularity, and the lithium titanate material D of preparation
50for 9.39um, through tap density meter test, the powder tap density obtained after secondary spraying dry is 0.97g/cm
3, after secondary clacining, tap density brings up to 1.22g/cm
3.
Embodiment 2:
A preparation method for high-tap density lithium titanate anode material, it comprises the steps:
(1) raw material mixing: add deionized water 250L in a mixing bowl, take 26kg Li according to the mol ratio of Li:Ti=0.82:1
2cO
3with 80kg TiO
2dispersion in deionized water, is stirred more than 2 hours, is made it fully mix.
(2) spraying dry: the powder that the slurry stirred is uniformly mixed by spraying dry.
(3) high-temperature calcination: roller-way sintering furnace is heated up according to heating curve, powder after spraying dry is loaded in SiC saggar, in air atmosphere, put into sintering furnace to calcine, heat preservation zone temperature is 850 DEG C, temperature retention time is 4h, then naturally cools, obtains the lithium titanate powder that purity is very high.
(4) wet ball grinding: lithium titanate powder, as abrasive media, adds in dispersion cylinder, then adds deionized water, be made into slurry by the zirconium oxide bead adding 0.2-1.0mm in ball mill, ball milling 5-8h, is mixed, nano level lithium titanate suspension-turbid liquid.
(5) secondary spraying dry: strict charging rate 20%, Contact Temperature 610 DEG C, outlet temperature 125 DEG C, the technological parameter such as negative pressure-150Pa in tower controlling spray drying tower, obtains the spherical micron particles of about average grain diameter 10um by spraying dry by uniform slurry.
(6) secondary clacining: calcine 1.5h in revolution sintering furnace 800 DEG C, naturally cool, pass into dry air simultaneously and take away moisture, obtain the lithium titanate material that moisture is less than 500ppm.
(7) sieve: pack after crossing 200 order spin vibration sieves.
Device phase purity, pattern and powder tap density are suitable with embodiment 1 after testing.
Embodiment 3:
A preparation method for high-tap density lithium titanate anode material, it comprises the steps:
(1) in a mixing bowl, add deionized water 200L, take 24.5kg LiNO according to the mol ratio of Li:Ti=0.82:1
3with 80kg TiO
2dispersion in deionized water, is stirred more than 2 hours, is made it fully mix.
(2) spraying dry: the powder that the slurry stirred is uniformly mixed by spraying dry.
(3) high-temperature calcination: roller-way sintering furnace is heated up according to heating curve, powder after spraying dry is loaded in SiC saggar, in air atmosphere, put into sintering furnace to calcine, heat preservation zone temperature is 850 DEG C, temperature retention time is 4h, then naturally cools, obtains the lithium titanate powder that purity is very high.
(4) wet ball grinding: lithium titanate powder, as abrasive media, adds in dispersion cylinder, then adds deionized water, be made into slurry by the zirconium oxide bead adding 0.2-1.0mm in ball mill, ball milling 5-8h, is mixed, nano level lithium titanate suspension-turbid liquid.
(5) secondary spraying dry: strict charging rate 20%, Contact Temperature 610 DEG C, outlet temperature 125 DEG C, the technological parameter such as negative pressure-150Pa in tower controlling spray drying tower, obtains the spherical micron particles of about average grain diameter 10um by spraying dry by uniform slurry.
(6) secondary clacining: calcine 1.5h in revolution sintering furnace 800 DEG C, naturally cool, pass into dry air simultaneously and take away moisture, obtain the lithium titanate material that moisture is less than 500ppm.
(7) sieve: pack after crossing 200 order spin vibration sieves.
Device phase purity, pattern and powder tap density are suitable with embodiment 1 after testing.
Effect example 1
Mix according to the lithium titanate material prepared by embodiment 1, superconduction carbon black, binding agent mass ratio 90:5:5, thickness is become to be the electrode film of 0.10mm with wet process film device film, 120 DEG C of dry 0.5h in vacuum drying chamber, the pole piece of diameter 12 mm is cut into slicing machine, using metal lithium sheet as to electrode and reference electrode, Clgarde makes barrier film, 1.2Mol LiPF
6eMC+EC(mol ratio 4:1) solution is electrolyte, in glove box, be assembled into button cell.Fig. 3 is the charging and discharging curve of button cell under 0.1C multiplying power prepared by the lithium titanate anode material prepared, and charge and discharge platform is obvious, and gram volume is 172.58 mAh/g first.
The above execution mode is only the preferred embodiments of the present invention, and and the feasible enforcement of non-invention exhaustive.For persons skilled in the art, to any apparent change done by it under the prerequisite not deviating from the principle of the invention and spirit, all should be contemplated as falling with within claims of the present invention.
Claims (6)
1. a preparation method for high-tap density lithium titanate anode material, is characterized in that, comprises the steps:
(1) raw material mixing: the ratio being Li:Ti=0.80-0.85:1 according to the mol ratio of Li and Ti takes lithium source and titanium source respectively, is medium, stirs, obtain slurry with deionized water;
(2) spraying dry: the slurry that step (1) obtains is carried out spraying dry, the powder be uniformly mixed;
(3) high-temperature calcination: step (2) is obtained powder under 700-875 DEG C of condition, calcine 2-6h, obtain lithium titanate powder;
(4) wet ball grinding: in ball mill, take water as decentralized medium, the lithium titanate powder that step (3) obtains is dispersed into slurry, is mixed through ball milling, nano level lithium titanate slurry;
(5) secondary spraying dry: the slurry that step (4) obtains is obtained spherical micron particles by spraying dry;
(6) secondary high-temperature sintering: particle step (5) obtained is 750-850 DEG C of sintering 1-3h in revolution sintering furnace, and cooling, obtains lithium titanate material;
(7) sieve: cross 200-250 order spin vibration sieve, to obtain final product.
2. the preparation method of a kind of high-tap density lithium titanate anode material according to claim 1, is characterized in that, the titanium source described in described step (1) is anatase TiO
2.
3. the preparation method of a kind of high-tap density lithium titanate anode material according to claim 1, is characterized in that, the lithium source described in described step (1) is for being selected from LiOHH
2o, Li
2cO
3and LiNO
3in one or three kinds of mixtures.
4. the preparation method of a kind of high-tap density lithium titanate anode material according to any one of claim 1 ~ 3, it is characterized in that, described step (3) is specific as follows: be loaded into by the powder after spraying dry in SiC saggar, in air atmosphere, put into sintering furnace to calcine, holding temperature is 700-875 DEG C, and temperature retention time is 2-6h, then cool, obtain the lithium titanate powder that purity is high.
5. the preparation method of a kind of high-tap density lithium titanate anode material according to any one of claim 1 ~ 3, is characterized in that, the average grain diameter of the micron particles in described step (5) is 5.5-11.0 μm.
6. the preparation method of a kind of high-tap density lithium titanate anode material according to any one of claim 1 ~ 3, it is characterized in that, described step (6) powder is 750-850 DEG C of calcining 1-3h in revolution sintering furnace, naturally cool, pass into dry air and take away moisture, obtain the lithium titanate material that moisture is less than 500ppm.
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CN108281653A (en) * | 2017-12-12 | 2018-07-13 | 合肥国轩高科动力能源有限公司 | A kind of negative electrode of lithium ion battery nodularization hard carbon material and preparation method thereof |
CN108550843A (en) * | 2018-05-24 | 2018-09-18 | 北方奥钛纳米技术有限公司 | Preparation method, nickel-cobalt-manganese ternary material, anode material for lithium-ion batteries and the lithium ion battery of nickel-cobalt-manganese ternary material |
CN109273705A (en) * | 2018-08-29 | 2019-01-25 | 昆明理工大学 | A kind of preparation method of lithium titanate anode material for lithium ion battery |
CN109336169A (en) * | 2018-09-29 | 2019-02-15 | 南京大学射阳高新技术研究院 | A kind of controllable synthesis method of lithium titanate micron-size spherical secondary structure and its application |
CN109659517A (en) * | 2018-11-29 | 2019-04-19 | 郑州中科新兴产业技术研究院 | A kind of preparation method of high-performance lithium titanate composite material |
CN109728293A (en) * | 2017-10-31 | 2019-05-07 | 北方奥钛纳米技术有限公司 | The preparation method of metatitanic acid lithium doping nickel-cobalt lithium manganate cathode material |
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CN109336169B (en) * | 2018-09-29 | 2020-10-09 | 南京大学射阳高新技术研究院 | Controllable synthesis method and application of lithium titanate micron-sized spherical secondary structure |
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CN109659517A (en) * | 2018-11-29 | 2019-04-19 | 郑州中科新兴产业技术研究院 | A kind of preparation method of high-performance lithium titanate composite material |
CN109879309A (en) * | 2019-03-14 | 2019-06-14 | 上海电气集团股份有限公司 | A kind of preparation method of high-tap density lithium titanate material |
CN110054216A (en) * | 2019-04-01 | 2019-07-26 | 北方奥钛纳米技术有限公司 | It prepares the method for lithium titanate and prepares the equipment of lithium titanate |
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CN110422875A (en) * | 2019-08-06 | 2019-11-08 | 南京兴旺新能源有限公司 | The preparation method of high-tap density high compacted density lithium titanate lithium cell cathode material |
CN110518237A (en) * | 2019-08-08 | 2019-11-29 | 河南电池研究院有限公司 | A method of preparing lithium cell anode material lithium manganate |
CN110459750A (en) * | 2019-08-21 | 2019-11-15 | 宋婷 | A kind of cathode material of lithium-ion power battery and preparation method thereof |
CN112607771A (en) * | 2020-12-22 | 2021-04-06 | 北方奥钛纳米技术有限公司 | Porous lithium titanate material, preparation method thereof, negative electrode material and lithium ion battery |
CN114031110A (en) * | 2021-10-03 | 2022-02-11 | 湖北钛时代新能源有限公司 | Preparation and synthesis method of lithium titanate material for lithium ion battery |
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