CN103682292B - The lithium titanate material preparation method of high-tap density - Google Patents
The lithium titanate material preparation method of high-tap density Download PDFInfo
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- CN103682292B CN103682292B CN201210334372.9A CN201210334372A CN103682292B CN 103682292 B CN103682292 B CN 103682292B CN 201210334372 A CN201210334372 A CN 201210334372A CN 103682292 B CN103682292 B CN 103682292B
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 40
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 39
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000004907 flux Effects 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000010936 titanium Substances 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- 239000001301 oxygen Substances 0.000 claims description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004327 boric acid Substances 0.000 claims description 4
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical group [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 4
- 229910021541 Vanadium(III) oxide Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 229910021538 borax Inorganic materials 0.000 claims description 2
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 2
- 239000004328 sodium tetraborate Substances 0.000 claims description 2
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 2
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 150000001721 carbon Chemical class 0.000 claims 1
- -1 lithium titanate Chemical class 0.000 claims 1
- SWAIALBIBWIKKQ-UHFFFAOYSA-N lithium titanium Chemical compound [Li].[Ti] SWAIALBIBWIKKQ-UHFFFAOYSA-N 0.000 claims 1
- 230000004048 modification Effects 0.000 claims 1
- 238000012986 modification Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 210000004027 cell Anatomy 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000010405 anode material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of lithium titanate material preparation method of high-tap density.The present invention mainly solves the problem that in current existing technology production, lithium titanate material density is little.Concrete grammar is: by lithium source, titanium source, flux and dispersant ball mill mixing by a certain percentage, low temperature presintering after dry, and after cooling, high-temperature calcination generates lithium titanate.Feature of the present invention is to add flux in batch mixing process, and in high-temperature sintering process, can make the tightr of particle contacts, reduce the interfacial tension between particle, crystal growth is grown more intact, and then improves material bodies density.The method technological process is simple, and raw material is easy to get, and the lithium titanate particle of preparation is large, tap density large, and chemical property is good.
Description
Technical field
The present invention relates to the preparation field of energy and material, particularly a kind of preparation method of lithium ionic cell cathode material lithium titanate.
Background technology
Lithium ion battery because energy density is high, have extended cycle life, the advantage such as memory-less effect, be the focus of field of batteries research and development always, be applied in fields such as portable electronics, electric automobile, energy storage and have good application prospect.At present, commercial lithium ion battery negative material generally adopts carbon negative pole material, but carbon negative pole material due to its oxidation-reduction potential and lithium electrode potential closely, during over-charging of battery, lithium ion is separated out on Carbon anode surface and is easily formed Li dendrite, may cause battery short circuit and cause safety problem, and material with carbon element can form SEI film with nonaqueous electrolytic solution that irreversible capacity is increased.And lithium titanate with spinel structure is because it is at Lithium-ion embeding with deviate from skeleton structure in process and change hardly, be a kind of " zero strain " material, and intercalation potential is higher, can not cause Li dendrite, improves the security performance of battery.Its advantage such as high security and long-life is the focus of research as Novel anode material always.
But lithium titanate also has weak point, the lithium titanate material obtained in existing research is little due to bulk density, causes battery energy density low, limits the application of lithium titanate, and therefore improving material tap density is one of lithium titanate main direction of studying.
Patent CN201010177934.4 discloses a kind of preparation method of spherical lithium titanate, and the method can improve the tap density of material, but the method has particular/special requirement to equipment, and technical process is numerous and diverse, and production cost is obviously increased.
Summary of the invention
For solving the problem, the invention provides a kind of lithium titanate material preparation method of high-tap density, the method raw material is cheap and easy to get, and make process operation simple owing to adding flux, the material property of synthesis is good.Concrete scheme is as follows:
A lithium titanate material preparation method for high-tap density, its step is as follows:
1) lithium source, titanium source, flux and dispersant are mixed, ball mill mixing 1 ~ 8h;
2) said mixture is placed in vacuum drying oven and passes into the gas that oxygen content is 0.01% ~ 21.6%, at 0 DEG C ~ 100 DEG C after drying, pre-burning 2 ~ 10h under 300 ~ 800 DEG C of oxygen content are the atmosphere of 0.01% ~ 50%;
3), after the cooling of pre-burning product, under 600 ~ 900 DEG C of oxygen content are the atmosphere of 0.01% ~ 99%, calcine 4 ~ 20h, obtain product Li
4ti
5o
12.
Wherein, Li/Ti=0.76 ~ 0.86 in step 1); Dispersant and solid content (gross mass of lithium source, titanium source and flux) mass ratio is 0.5 ~ 1.5:1; Flux content is 0.1 ~ 5wt% of titanium dioxide quality.
Wherein lithium source of the present invention is the one in lithium carbonate, lithium hydroxide or lithium nitrate; Titanium source is anatase titanium dioxide or rutile titanium dioxide; Flux is one or more mixtures in sodium tetraborate, Firebrake ZB, boric acid, lithium tetraborate, lithium hydroxide, lithium acetate, sodium carbonate, lithium carbonate, lithium fluoride or vanadic oxide; Dispersant is one or more mixtures in water, ethanol, methyl alcohol or acetone.
Main feature of the present invention is:
The present invention adds flux in the feed, is sintered into lithium titanate material again after batch mixing drying, and this process is simple, is easy to operation, cost is effectively controlled.
The present invention is by adding flux, two kinds of raw materials are at high temperature made to contact better, reduce the growth temperature of crystal, shorten crystal growth time, improve tap density, sinter for a long time compared to conventional method high temperature, reduce energy consumption, decrease the loss of equipment, be easier to industrial production application.
The lithium titanate particle that the present invention prepares gained is large, and tap density is greater than 1.2g/cm
3, 0.1C charge specific capacity is greater than 160mAh/g.
On the basis of the lithium titanate prepared in the method, can also ion doping be carried out or carbon coated, can further improve the conductivity of material.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the lithium titanate prepared by the embodiment of the present invention three;
Fig. 2 is the first charge-discharge curve chart of the lithium titanate prepared by the embodiment of the present invention three.
Embodiment
Below in conjunction with embodiment, a kind of preparation method improving lithium titanate tap density of the present invention is described in more detail.But the present invention is not limited to following examples.
Embodiment one
Select lithium carbonate, anatase titanium dioxide to be raw material, lithium fluoride is flux, by Li/Ti(mol%) ratio is 0.80:1, lithium fluoride content is TiO
2the 1wt% of quality prepares burden, and take ethanol as dispersant, ethanol: solid powder (wt%)=0.7:1, and on ball mill, ball milling is after 6 hours, dry presoma pass into the gas 40 DEG C containing oxygen 21.6% in baking oven at.By presoma, under the atmosphere of oxygen content 10%, elder generation is at 500 DEG C, and high-temperature process 2 hours, is warmed up to 800 DEG C after cooling, under the atmosphere of oxygen content 21.6%, be incubated 8 hours, obtains Li after being finally down to room temperature
4ti
5o
12sample.Resulting materials granular size is homogeneous, tap density 1.20g/cm
3, and do not add flux and the lithium titanate tap density (0.78g/cm prepared under other identical conditions
3) compare, density significantly improves.With metal lithium sheet for prepare button cell to electrode, material 0.1C charge specific capacity is 165mAh/g.
Embodiment two
Select lithium nitrate, rutile titanium dioxide to be raw material, boric acid is flux, by Li/Ti(mol%) ratio is 0.82:1, boric acid content is TiO
2the 0.5wt% of quality prepares burden, and take ethanol as dispersant, ethanol: solid powder (wt%)=0.8:1 ball milling after 6 hours on ball mill, dry presoma pass into the gas 60 DEG C containing oxygen 0.1% in baking oven at.Presoma is first at 500 DEG C under the atmosphere of oxygen content 0.01%, and high-temperature process 2 hours, is warmed up to 800 DEG C and is incubated 8 hours under the atmosphere of oxygen content 99% after cooling, obtain Li after being finally down to room temperature
4ti
5o
12sample.Resulting materials particle is round and smooth, size is homogeneous, and tap density is 1.36g/cm
3, and do not add flux and the lithium titanate tap density (0.80g/cm prepared under other identical conditions
3) compare, density significantly improves.With metal lithium sheet for prepare button cell to electrode, the 0.1C charge specific capacity of material is 161mAh/g.
Embodiment three
Select lithium hydroxide, anatase titanium dioxide to be raw material, lithium tetraborate is flux, by Li/Ti(mol%) than being 0.84: lithium tetraborate content is TiO
2the 0.5wt% of quality prepares burden, and take methyl alcohol as dispersant, methyl alcohol: solid powder (wt%)=1:1 ball milling after 6 hours on ball mill, dry presoma pass into the gas 50 DEG C containing oxygen 21.6% in baking oven at.Presoma is first at 500 DEG C of temperature under the atmosphere of oxygen content 21.6%, and high-temperature process 2 hours, is warmed up to 800 DEG C and is incubated 8 hours under the atmosphere of oxygen content 0.1% after cooling, obtain Li after being finally down to room temperature
4ti
5o
12sample.Resulting materials particle is round and smooth, size is homogeneous, and tap density is 1.48g/cm
3, and do not add flux and the lithium titanate tap density (0.82g/cm prepared under other identical conditions
3) compare, density significantly improves.With metal lithium sheet for prepare button cell to electrode, the 0.1C charge specific capacity of material is 160mAh/g.
Embodiment four
Select lithium hydroxide, anatase titanium dioxide to be raw material, vanadic oxide is flux, is (mol%) 0.84: pentoxide content is TiO by Li/Ti ratio
2the 1wt% of quality prepares burden, and take acetone as dispersant, acetone: solid powder (wt%)=0.8:1 ball milling after 6 hours on ball mill, dry presoma pass into the gas 50 DEG C containing oxygen 10% in baking oven at.Presoma is first at 500 DEG C of temperature under the atmosphere of oxygen content 21.6%, and high-temperature process 2 hours, is warmed up to 750 DEG C and is incubated 8 hours under the atmosphere of oxygen content 99% after cooling, obtain Li after being finally down to room temperature
4ti
5o
12sample.Resulting materials particle is round and smooth, size is homogeneous, and tap density is 1.25g/cm
3, and do not add flux and the lithium titanate tap density (0.84g/cm prepared under other identical conditions
3) compare, density significantly improves.With metal lithium sheet for prepare button cell to electrode, the 0.1C charge specific capacity of material is 163mAh/g.
Claims (9)
1. a preparation method for the lithium titanate material of high-tap density, is characterized in that following steps:
1) lithium source, titanium source, flux and dispersant are mixed, ball mill mixing 1 ~ 8h;
2) said mixture is placed in vacuum drying oven and passes into the gas that oxygen content is 0.01% ~ 21.6%, at 0 DEG C ~ 100 DEG C after drying, pre-burning 2 ~ 10h under 300 ~ 800 DEG C of oxygen content are the atmosphere of 0.01% ~ 50%;
3), after the cooling of pre-burning product, under 600 ~ 900 DEG C of oxygen content are the atmosphere of 0.01% ~ 99%, calcine 4 ~ 20h, obtain product Li
4ti
5o
12; The tap density of this lithium titanate material is greater than 1.2g/cm
3.
2. preparation method according to claim 1, is characterized in that: described lithium source is lithium carbonate, lithium hydroxide or lithium nitrate.
3. preparation method according to claim 1, is characterized in that: described titanium source is the titanium dioxide of anatase titanium dioxide or rutile-type.
4. preparation method according to claim 1, is characterized in that: step 1) in raw material in lithium titanium mol ratio be Li/Ti=0.76 ~ 0.86.
5. preparation method according to claim 1, is characterized in that: described flux is one or more mixtures in sodium tetraborate, Firebrake ZB, boric acid, lithium tetraborate, lithium hydroxide, lithium acetate, lithium fluoride or vanadic oxide.
6. preparation method according to claim 1 or 5, is characterized in that: the content of described flux is 0.05 ~ 10wt% of titanium dioxide quality.
7. preparation method according to claim 1, is characterized in that: described dispersant and solid content mass ratio are 0.5 ~ 1.5:1.
8. the preparation method according to claim 1 or 7, is characterized in that: dispersant is one or more mixing in water, ethanol, methyl alcohol or acetone.
9. preparation method as claimed in claim 1, is characterized in that: also comprise step 4):
4) by step 3) in gained lithium titanate carry out coated modified carbon process or ion doping process further, obtain the Li of modification
4ti
5o
12.
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CN104979554B (en) * | 2014-04-02 | 2019-07-16 | 郭建 | A kind of preparation method of nickel cobalt lithium aluminate and its presoma |
CN104979552B (en) * | 2014-04-02 | 2019-07-16 | 张联齐 | A kind of preparation method of bulky grain nickel cobalt lithium aluminate |
CN107324379A (en) * | 2017-06-30 | 2017-11-07 | 江苏特丰新材料科技有限公司 | A kind of high power capacity lithium titanate material preparation method |
CN109704395A (en) * | 2018-12-28 | 2019-05-03 | 北方奥钛纳米技术有限公司 | Preparation method, lithium titanate material and the battery of lithium titanate material |
CN109904446B (en) * | 2019-02-26 | 2022-05-17 | 广东邦普循环科技有限公司 | Regenerated positive electrode material, preparation method thereof and lithium ion battery containing regenerated positive electrode material |
CN114725358B (en) * | 2022-05-07 | 2024-10-11 | 中国人民解放军陆军工程大学 | Lithium titanate graphene electrode and preparation method thereof |
CN115744972B (en) * | 2023-01-09 | 2023-05-16 | 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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CN101659442A (en) * | 2008-08-27 | 2010-03-03 | 比亚迪股份有限公司 | Spinel structure lithium titanate and preparation method and application thereof |
CN102315436A (en) * | 2011-08-10 | 2012-01-11 | 东莞市迈科科技有限公司 | A kind of preparation method of spinel lithium titanate |
CN102496705A (en) * | 2011-12-09 | 2012-06-13 | 东莞市迈科科技有限公司 | Preparation method of spinel lithium titanate |
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CN101659442A (en) * | 2008-08-27 | 2010-03-03 | 比亚迪股份有限公司 | Spinel structure lithium titanate and preparation method and application thereof |
CN102315436A (en) * | 2011-08-10 | 2012-01-11 | 东莞市迈科科技有限公司 | A kind of preparation method of spinel lithium titanate |
CN102496705A (en) * | 2011-12-09 | 2012-06-13 | 东莞市迈科科技有限公司 | Preparation method of spinel lithium titanate |
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