CN104810514A - Preparation method for ion adulterated lithium titanate cathode material - Google Patents
Preparation method for ion adulterated lithium titanate cathode material Download PDFInfo
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- CN104810514A CN104810514A CN201510156517.4A CN201510156517A CN104810514A CN 104810514 A CN104810514 A CN 104810514A CN 201510156517 A CN201510156517 A CN 201510156517A CN 104810514 A CN104810514 A CN 104810514A
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- ball milling
- lithium titanate
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- preparation
- 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
-
- 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
-
- 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
-
- 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 for an ion adulterated lithium titanate cathode material. The preparation method mainly comprises the following steps: placing materials required into an MITR-YXQM-2L oil sealing mute planetary high-energy ball mill after mixing; ball milling for 2 h at the speed of 250 r/min; after obtaining a pasty material, carrying out vacuum drying at 80 DEG C; putting the obtained powder into an HY-MB high-temperature energy-saving muffle furnace for calcining for 16 h at 900 DEG C in the air atmosphere; reducing to room temperature along with the furnace temperature, then putting to the MITR-YXQM-2L oil sealing mute planetary high-energy ball mill, and adopting a ball milling medium with the diameter of 5 mm for ball milling for 6 h at the speed of 400 r/min, wherein the mass ratio of the ball milling medium to the material is 3:1; after ball milling, sieving the obtained powder with a 400-mesh sieve to obtain the final lithium titanate cathode material required by the electrode paste. According to the preparation method, after calcining, high-energy ball milling and sieving are carried out over again, so that the lithium titanate powder is uniform in particles, fine in particle sizes and free of agglomeration, has better dispersity, and greatly improves the electrochemical performance stability of lithium titanate.
Description
Technical field
The present invention relates to field of lithium, especially, relate to a kind of high-energy ball milling method prepares the lithium titanate anode material of ion doping method in conjunction with solid phase method.
Background technology
Along with development that is scientific and technical and information technology, developing rapidly of the portable type electronic products such as especially mobile communication, notebook computer, video camera, people, to the miniaturization of battery, lightness, high power, high-energy, useful life and environmental friendliness degree, propose more and more higher requirement.And traditional lead-acid battery, ickel-cadmium cell, Ni-MH battery etc., because useful life is short, the problem such as lower and environmental pollution of energy density strongly limit their use.Therefore need the rechargeable battery finding alternative traditional lead acid batteries and ni-cd battery, the battery of the exploitation electrode material of nontoxic pollution-free, electrolyte and battery diaphragm and environmentally safe is current battery industry top priority.And the advantage of lithium ion battery becomes strong candidate.
Current commercial lithium-ion batteries is mainly negative pole with graphitized carbon material.But carbon negative pole material exists following shortcoming: during battery overcharge, carbon negative pole material surface easily forms Li dendrite thus causes battery short circuit or blast; First charge-discharge efficiency is low; Carbon negative pole material easily reacts with electrolyte, cycle performance reduction; There is the problems such as voltage delay.Can not meet portable type electronic product and must have higher energy density to the requirement, particularly automobile power cell that battery high specific energy quantizes, lower cost and better fail safe, cause graphite cathode material being restricted at this future development.
Compared with carbon negative pole material, the Li of spinel-type
4ti
5o
12(lithium titanate) is called as zero strain material, good cycle; Discharging voltage balance, does not react with electrolyte, the advantages such as security performance is good; Compared with carbon negative pole material, lithium titanate has high lithium ion diffusion coefficient (being 2 * 10-8cm2/s), can high power charging-discharging etc.; The electromotive force of lithium titanate, than the height of pure metal lithium, not easily produces the advantages such as lithium dendrite arm.So Li in recent years
4ti
5o
12extensively studied as lithium ion battery negative material.But due to Li
4ti
5o
12electronic conductivity and the ionic conductivity of material are less, and when high current charge-discharge, capacity attenuation is very fast, therefore improve Li
4ti
5o
12high rate performance become and have problem to be solved.In order to improve its conductive capability, therefore, much research all concentrates in exploration to this material preparation process, optimization and element doping modification.
At present, Li
4ti
5o
12preparation method a lot, comprise high temperature solid phase synthesis, sol-gel process, hydrothermal solvent method, spray drying process etc.These methods have the advantage that product purity is high, heat treatment is low, but it needs to be added with organic compounds or fire retardant in preparation process, causes environmental pollution, and the production cycle is long, causes cost high, complex process, is difficult to realize large-scale production.And solid-phase synthesis prepares Li
4ti
5o
12, there is composition heterogeneity, the defect that product batches difference is large, but its method is simple, operating procedure is few, production efficiency advantages of higher, makes it in industrialization, have very large advantage.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the invention is a kind of preparation method of ion doping lithium titanate anode material, solves lithium titanate anode material conductance in prior art low, doubly forthright difference, the low density problem of lithium ion battery volumetric specific energy.
The technical solution adopted in the present invention is: a kind of lithium titanate anode material preparation method of ion doping, it comprises the steps:
1), by lithium carbonate: anatase titanium dioxide: the elemental lithium (Li) in Doped ions additive: titanium elements (Ti): the mol ratio of doped chemical be 0.8-0.84: 1: 0.015-0.04 proportions material stand-by;
2), stand-by by 25% weighing pure water of the total weight of the material of step 1);
3), by step 1) and 2) material mixing after put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing, ball milling 2h under the speed of 250r/min, obtains the material of paste;
4), the material of step 3) gained paste is obtained the powder of presoma 80 DEG C of vacuumizes;
5), by step 4) gained powder put into HY-MB high-temperature energy-conservation Muffle furnace, 900 DEG C of roastings 16 hours, are down to room temperature with furnace temperature afterwards, obtain Li in air atmosphere
4ti
(5-x)y
xoi
2or Li
4ti
5y
xoi
2-xpowder;
6), the powder obtained is put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing, the ball-milling medium of diameter 5mm and the mass ratio of material is adopted to be 3:1, ball milling 6h under the speed of 400r/min, the powder obtained after ball milling sieves the lithium titanate anode material obtained needed for final electrode slurry through 400 mesh sieve.
Wherein step 3) is 0.1MPa 80 DEG C of vacuum degrees.
Described Doped ions is cation or anion is magnesium oxide (Mg2+), nickel sesquioxide (Ni3+), chrome green (Cr3+), alundum (Al2O3) (Al3+), tin oxide (Sn2+), lithium bromide (Br
1-), lithium fluoride (F
1-) in one.
Compared with prior art, the invention has the beneficial effects as follows: (1) the present invention adopts high-energy ball milling method to carry out micronization processes to raw material before the synthesis, for lithium carbonate and titanium dioxide provide the chance of solid phase reaction, the generation of impurity can be reduced;
(2) the present invention after firing, again carries out high-energy ball milling, screening, makes that the particle of lithium titanate powdery is homogeneous, granularity is tiny, soilless sticking, has good dispersiveness, improve the stability of lithium titanate chemical property greatly;
(3) present invention process is simple, and without the need to adopting Buchholz protection in production process, can react at ambient pressure, production cost is low, the favorable reproducibility of different batches product, is applicable to large-scale industrial production;
(4) the present invention can not produce various pernicious gas in sintering process, pollution-free, is very beneficial for environmental protection;
(5) lithium titanate anode material conductance in prior art is solved low, doubly forthright difference, the low density problem of lithium ion battery volumetric specific energy.
Embodiment
Below in conjunction with embodiment, most preferred embodiment of the present invention is described in detail.
Embodiment one: its Li: Ti:Mg mol ratio of doped with Mg 2+ is the preparation of 0.80:1:0.04 lithium titanate
(1) 295.560 grams of Li are taken
2cO
3, 798.700 grams of sharp ore deposit type TiO
2, 16.000 grams of MgO are stand-by;
(2) pure water taking 277.565 grams is stand-by;
(3) put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing by after the mixing of the raw material of step (1) and (2), under the speed of 250r/min, ball milling 2h obtains the material of paste;
(4) by the vacuum drying chamber dry 10h of the plaster material of step (3) at 80 DEG C, the powder of presoma is obtained;
(5) precursor powder of step (4) is put into industrial Muffle furnace, the lower 900 DEG C of roastings of air atmosphere 16 hours, are down to room temperature with furnace temperature, obtain Li
4-xmg
xti
5oi
2powder;
(6) powder that step (5) obtains is put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing, adopt the ball-milling medium of diameter 5mm and the mass ratio of material to be 3:1 ball milling 6h under the speed of 400r/min, the powder obtained after ball milling sieves the powder obtained needed for final electrode slurry through 400 mesh sieve.
Its Li: Ti:Ni mol ratio of embodiment two: Ni doped 3+ is the preparation of the lithium titanate of 0.84:1:0.03
(1) 310.338 grams of Li are taken
2cO
3, 798.700 grams of sharp ore deposit type TiO
2, 49.626 grams of Ni
2o
3stand-by;
(2) pure water taking 285.972 grams is stand-by;
(3) put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing by after the mixing of the raw material of step (1) and (2), under the speed of 250r/min, ball milling 2h obtains the material of paste;
(4) by the vacuum drying chamber dry 10h of the plaster material of step (3) at 80 DEG C, the powder of presoma is obtained;
(5) precursor powder of step (4) is put into industrial Muffle furnace, the lower 900 DEG C of roastings of air atmosphere 16 hours, are down to room temperature with furnace temperature, obtain Li
4ni
xti
(5-x)o
12powder;
(6) powder that step (5) obtains is put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing, adopt the ball-milling medium of diameter 5mm and the mass ratio of material to be 3:1 ball milling 6h under the speed of 400r/min, the powder obtained after ball milling sieves the powder obtained needed for final electrode slurry through 400 mesh sieve.
Embodiment three: its Li: Ti:Sn mol ratio of doping Sn2+ is the preparation of the lithium titanate of 0.82:1:0.015
(1) 302.949 grams of Li are taken
2cO
3, 798.700 grams of sharp ore deposit type TiO
2, 22.605 grams of SnO are stand-by
(2) pure water taking 279.216 grams is stand-by;
(3) put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing by after the mixing of the raw material of step (1) and (2), under the speed of 250r/min, ball milling 2h obtains the material of paste;
(4) by the plaster material of step (3) dry 10h under the vacuum drying chamber vacuum degree 0.1MPa of 80 DEG C, the powder of presoma is obtained;
(5) precursor powder of step (4) is put into industrial Muffle furnace, the lower 900 DEG C of roastings of air atmosphere 16 hours, are down to room temperature with furnace temperature, obtain Li
4ti
(5-x)sn
xoi
2powder;
(6) powder that step (5) obtains is put into the quiet planetary high-energy ball mill of the quiet planetary MITR-YXQM-2L oil sealing of the MITR-YXQM-2L oil sealing quiet planetary MITR-YXQM-2L oil sealing of quiet planetary MITR-YXQM-2L oil sealing, adopt the ball-milling medium of diameter 5mm and the mass ratio of material to be 3:1 ball milling 6h under the speed of 400r/min, the powder obtained after ball milling sieves the powder obtained needed for final electrode slurry through 400 mesh sieve.
Embodiment four: doping Br
1-its Li: Ti:Br mol ratio is the preparation of the lithium titanate of 0.80:1:0.04
(1) 295.560 grams of Li are taken
2cO
3, 798.700 grams of sharp ore deposit type TiO
2, 34.738 grams of LiBr are stand-by;
(2) pure water taking 272.250 grams is stand-by;
(3) put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing by after the mixing of the raw material of step (1) and (2), under the speed of 250r/min, ball milling 2h obtains the material of paste;
(4) by the plaster material of step (3) dry 10h under the vacuum drying chamber vacuum degree 0.1MPa of 80 DEG C, the powder of presoma is obtained;
(5) precursor powder of step (4) is put into industrial Muffle furnace, the lower 900 DEG C of roastings of air atmosphere 16 hours, are down to room temperature with furnace temperature, obtain Li
4ti
5o
l2-Xbr
xpowder;
(6) powder that step (5) obtains is put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing, adopt the ball-milling medium of diameter 5mm and the mass ratio of material to be 3:1 ball milling 6h under the speed of 400r/min, the powder obtained after ball milling sieves the powder obtained needed for final electrode slurry through 400 mesh sieve.
Embodiment five: doped F
1-its Li: Ti:F mol ratio is the preparation of the lithium titanate of 0.80:1:0.02
(1) 295.560 grams of Li are taken
2cO
3, 798.700 grams of sharp ore deposit type TiO
2, 0.519 gram of LiF be stand-by;
(2) pure water taking 273.695 grams is stand-by;
(3) put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing by after the mixing of the raw material of step (1) and (2), under the speed of 250r/min, ball milling 2h obtains the material of paste;
(4) by the plaster material of step (3) dry 10h under the vacuum drying chamber vacuum degree 0.1MPa of 80 DEG C, the powder of presoma is obtained;
(5) precursor powder of step (4) is put into industrial Muffle furnace, the lower 900 DEG C of roastings of air atmosphere 16 hours, are down to room temperature with furnace temperature, obtain Li
4ti
5o
l2-Xf
xpowder;
(6) powder that step (5) obtains is put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing, adopt the ball-milling medium of diameter 5mm and the mass ratio of material to be 3:1 ball milling 6h under the speed of 400r/min, the powder obtained after ball milling sieves the powder obtained needed for final electrode slurry through 400 mesh sieve.
Claims (3)
1. a lithium titanate anode material preparation method for ion doping, it comprises the steps:
1), by the elemental lithium (Li) in lithium carbonate, anatase titanium dioxide and Doped ions additive: titanium elements (Ti): the mol ratio of doped chemical be 0.8-0.84: 1: 0.015-0.04 proportions material stand-by;
2), stand-by by 25% weighing pure water of the total weight of the material of step 1);
3), by step 1) and 2) material mixing after put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing, ball milling 2h under the speed of 250r/min, obtains the material of paste;
4), the material of step 3) gained paste is obtained the powder of presoma 80 DEG C of vacuumizes;
5), by step 4) gained powder put into HY-MB high-temperature energy-conservation Muffle furnace, 900 DEG C of roastings 16 hours, are down to room temperature with furnace temperature afterwards, obtain Li in air atmosphere
4ti
(5-x)y
xoi
2or Li
4ti
5y
xoi
2-xpowder;
6), the powder obtained is put into the quiet planetary high-energy ball mill of MITR-YXQM-2L oil sealing, adopt the ball-milling medium of diameter 5mm and the mass ratio of material to be 3:1, the powder obtained after ball milling 6h ball milling under the speed of 400r/min sieves the lithium titanate anode material obtained needed for final electrode slurry through 400 mesh sieve.
2. according to the lithium titanate anode material preparation method of a kind of ion doping described in claim 1, it is characterized in that, wherein step 3) is 0.1MPa 80 DEG C of vacuum degrees.
3. the lithium titanate anode material preparation method of a kind of ion doping according to claim 1 and 2, it is characterized in that, described Doped ions is cation or anion is magnesium oxide (Mg2+), nickel sesquioxide (Ni3+), chrome green (Cr3+), alundum (Al2O3) (Al3+), tin oxide (Sn2+), lithium bromide (Br
1-), lithium fluoride (F
1-) in one.
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| CN201510156517.4A CN104810514A (en) | 2015-04-03 | 2015-04-03 | Preparation method for ion adulterated lithium titanate cathode material |
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ID=53695167
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105845924A (en) * | 2016-05-23 | 2016-08-10 | 扬州大学 | Preparation method for fluorine-doping Li4Ti5O12 nanosheet |
| CN106935831A (en) * | 2017-03-31 | 2017-07-07 | 深圳市国创新能源研究院 | A kind of lithium titanate anode material for suppressing flatulence and its preparation method and application |
| CN108417785A (en) * | 2018-01-11 | 2018-08-17 | 茆胜 | Fluorine nitrogen-doped graphene coats lithium titanate composite material and preparation method thereof |
| CN109301236A (en) * | 2018-08-17 | 2019-02-01 | 中北润良新能源汽车(徐州)股份有限公司 | A kind of solid reaction process improving 1.55V lithium titanate battery capacity |
| CN109437290A (en) * | 2018-10-09 | 2019-03-08 | 深圳大学 | A kind of preparation method and lithium ion super capacitor of a lithium titanate nanobelt ball of string |
| CN110459761A (en) * | 2019-08-21 | 2019-11-15 | 宋婷 | A kind of codope lithium titanate anode material and preparation method thereof |
| CN115744972A (en) * | 2023-01-09 | 2023-03-07 | 河北格力钛新能源有限公司 | Preparation method of high-compaction lithium titanate material and high-compaction lithium titanate material |
-
2015
- 2015-04-03 CN CN201510156517.4A patent/CN104810514A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| EUH DUCK JEONG等: "Characterizations and electrochemical performance of pure and metal-doped Li4Ti5O12 for anode materials of lithium-ion batteries", 《MATERIALS RESEARCH BULLETIN》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105845924A (en) * | 2016-05-23 | 2016-08-10 | 扬州大学 | Preparation method for fluorine-doping Li4Ti5O12 nanosheet |
| CN106935831A (en) * | 2017-03-31 | 2017-07-07 | 深圳市国创新能源研究院 | A kind of lithium titanate anode material for suppressing flatulence and its preparation method and application |
| CN108417785A (en) * | 2018-01-11 | 2018-08-17 | 茆胜 | Fluorine nitrogen-doped graphene coats lithium titanate composite material and preparation method thereof |
| CN108417785B (en) * | 2018-01-11 | 2020-11-17 | 茆胜 | Fluorine-nitrogen doped graphene coated lithium titanate composite material and preparation method thereof |
| CN109301236A (en) * | 2018-08-17 | 2019-02-01 | 中北润良新能源汽车(徐州)股份有限公司 | A kind of solid reaction process improving 1.55V lithium titanate battery capacity |
| CN109437290A (en) * | 2018-10-09 | 2019-03-08 | 深圳大学 | A kind of preparation method and lithium ion super capacitor of a lithium titanate nanobelt ball of string |
| CN109437290B (en) * | 2018-10-09 | 2021-03-23 | 深圳大学 | Preparation method of lithium titanate nanoribbon coil and lithium ion supercapacitor |
| CN110459761A (en) * | 2019-08-21 | 2019-11-15 | 宋婷 | A kind of codope lithium titanate anode material and preparation method thereof |
| CN110459761B (en) * | 2019-08-21 | 2022-05-17 | 江西优灿新能源科技有限公司 | Codoped lithium titanate negative electrode material and preparation method thereof |
| CN115744972A (en) * | 2023-01-09 | 2023-03-07 | 河北格力钛新能源有限公司 | Preparation method of high-compaction lithium titanate material and high-compaction lithium titanate material |
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Application publication date: 20150729 |