CN114031110A - Preparation and synthesis method of lithium titanate material for lithium ion battery - Google Patents
Preparation and synthesis method of lithium titanate material for lithium ion battery Download PDFInfo
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- CN114031110A CN114031110A CN202111167148.0A CN202111167148A CN114031110A CN 114031110 A CN114031110 A CN 114031110A CN 202111167148 A CN202111167148 A CN 202111167148A CN 114031110 A CN114031110 A CN 114031110A
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- lithium ion
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- 239000000463 material Substances 0.000 title claims abstract description 60
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 47
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 46
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000001308 synthesis method Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001694 spray drying Methods 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- 239000010936 titanium Substances 0.000 claims abstract description 13
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 36
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 11
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical group [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000007773 negative electrode material Substances 0.000 claims description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims 8
- 239000003792 electrolyte Substances 0.000 abstract description 6
- 238000007086 side reaction Methods 0.000 abstract description 4
- 238000005056 compaction Methods 0.000 abstract description 3
- 238000009766 low-temperature sintering Methods 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 25
- 239000002994 raw material Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- 241000219094 Vitaceae Species 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel 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
-
- 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
- C01G23/005—Alkali titanates
-
- 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
- H01M4/36—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
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation and synthesis method of a lithium titanate material for a lithium ion battery, which mainly comprises the following steps: s1, mixing the lithium source, the titanium source and water, and stirring uniformly; then spray drying is carried out until the water content of the material is below 5%; s2, sintering the material obtained in the step S1 for the first time; s3, carrying out wet ball milling on the calcined dry material, and grinding the dry material by taking water as a solvent and zirconium balls as a ball milling medium to obtain nano slurry; and S4, spray drying the nano slurry again to obtain a spherical material, carrying out secondary sintering, drying to remove water, and controlling the water content of the material to be less than 200ppm to obtain the lithium titanate material for the lithium ion battery. The lithium titanate material provided by the invention has smooth appearance, and has the advantages of improving material compaction, saving electrolyte, reducing the consumption of side reaction of the electrolyte and improving the cycle performance of a battery through low-temperature sintering.
Description
Technical Field
The invention belongs to the technical field of negative electrode materials, and particularly relates to a preparation and synthesis method of a lithium titanate material for a lithium ion battery.
Background
Under the large environment of the national great advocated development of new energy and related industries, lithium titanate becomes a research hotspot of a negative electrode material of a novel lithium ion battery due to excellent safety, ultra-long cycle performance, rapid charge and discharge and ultra-wide high/low temperature performance, and the application prospect of the lithium titanate is also expanded continuously.
At present, the preparation method of lithium titanate mainly comprises a solid-phase reaction method, a sol-gel method, a hydrothermal ion exchange synthesis method and the like. The high-temperature solid-phase synthesis method has the advantages of simple preparation process, low equipment requirement, few reaction influence factors and easiness in industrial batch production, but the particle size of the high-temperature solid-phase synthesis method is larger and is generally in a micron level; the powder material is difficult to mix, and the raw material mixing uniformity is limited; the heat treatment temperature is higher, and the energy consumption is larger. The lithium titanate prepared by the sol-gel method has high purity and controllable particle size, can realize the nanocrystallization of the material, but has long preparation period and a plurality of influencing factors in the preparation process. The hydrothermal ion exchange synthesis method has the advantages of simple operation, low synthesis temperature, changeable and controllable reaction conditions, uniform product composition and controllable particle size, but the large-scale high-temperature and high-pressure resistant reactor required in the preparation process has large design and manufacture difficulty, high manufacturing cost and difficult maintenance.
Disclosure of Invention
The invention provides a preparation and synthesis method of a lithium titanate material for a lithium ion battery, and the prepared lithium titanate material has smooth appearance and has the advantages of improving material compaction, saving electrolyte, reducing the consumption of side reaction of the electrolyte and improving the cycle performance of the battery.
The technical scheme of the invention is that a preparation and synthesis method of a lithium titanate material for a lithium ion battery comprises the following steps:
s1, mixing the lithium source, the titanium source and water, and stirring uniformly; then spray drying is carried out until the water content of the material is below 5%;
s2, sintering the material obtained in the step S1 for the first time;
s3, carrying out wet ball milling on the calcined dry material, and grinding the dry material to obtain nano slurry by taking water as a solvent and zirconia balls as a ball milling medium;
and (3) spray drying the nano slurry obtained from the S4 and the S3 again to obtain a spherical material, then carrying out secondary sintering, and finally carrying out vacuum drying at 120-180 ℃ to remove water, wherein the water content of the material is controlled to be less than 200ppm, so as to obtain the lithium titanate material for the lithium ion battery.
Further, the lithium source is LiOH H2One or more of O, lithium carbonate and lithium acetate, and the titanium source is TiO2·2H2O, and the mass ratio of the lithium source to the titanium source to the water is 2-3: 6-8: 20-25.
Furthermore, after the lithium source, the titanium source and the water in the S1 are mixed, the solid content is 20-40%, and the mixture is continuously stirred for 4-10 hours.
Further, when drying in S1, air at 200-300 ℃ is adopted for drying.
Furthermore, the sintering temperature in S2 is 300-500 ℃, and the time is 10-18 h.
Furthermore, after water is added into the dry materials in the S3, the solid content is 15-30%.
Further, the diameter of the zirconium balls in the S3 is 0.25-0.4 mm, and the ball milling is carried out for 25-35 h; the specific surface area after ball milling is between 90 and 110m2Per g, particle size of the material D10 60～90nm，D50 250-300nm，D90 400～600nm，D99 650～800nm。
Further, when the spray drying is carried out in S4, the temperature is 200-300 ℃; drying to a water content of less than 7%.
Furthermore, the sintering temperature in S4 is 300-500 ℃, the sintering time is 8-15 h,
the invention also relates to a lithium titanate material for the lithium ion battery prepared by the method, and an application of the lithium titanate material as a negative electrode material for the lithium ion battery.
The invention has the following beneficial effects:
according to the invention, a lithium source, a titanium source and water are used as raw materials, and the raw materials are subjected to primary spray drying and calcination, then ball milling is carried out, and secondary spray drying and calcination are carried out, so that the prepared lithium titanate material has a smooth appearance, and has the advantages of improving material compaction, saving electrolyte, reducing the consumption of side reaction of the electrolyte and improving the cycle performance of a battery.
According to the invention, spray drying and calcination are carried out twice in sequence, and low-temperature calcination is adopted in the calcination, so that the formation of high-temperature macropores is avoided, side reactions are reduced, and the cycle performance of the material can be remarkably improved under the condition of ensuring a certain charge-discharge rate.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
Example 1:
a preparation and synthesis method of a lithium titanate material for a lithium ion battery comprises the following specific steps:
raw material mixing step (DT): adding LiOH & H into an enamel reaction vessel with a stainless steel shell and a 1-2mm inner lining2O3 Kg anatase type TiO2·2H2O8 Kg, solvent H220Kg of O, 35% of solid content, continuously stirred for 6 hours.
One spray drying Process (SD)1): introducing air at 300 deg.C into spray dryer to reduce water content of the mixed raw materials to below 5%.
Primary Calcination (CA): and calcining the mixture after spray drying at a high temperature of 300 ℃ for 12 hours. In the process, a chemical reaction is carried out to generate a lithium titanate material, the phase purity is 97 percent, and the phase purity is matched with the crystalline phase of lithium titanate; in the process, rutile phase will appear when the Ti equivalent is too much, and Li will be generated when the Li equivalent is too much2TiO3Lithium metatitanate.
Wet Ball Milling (BM): transferring the calcined dry material to a ball mill, and adding H2O as solvent, controlling solid content at 20%, zirconium ball diameter at 0.3mm, ball milling for 30h (basically 17h for forming), specific surface area 98m2Per g, particle size of the material D1080nm，D50 276nm，D90 500nm，D99 700nm。
Secondary Spray Drying (SD)2): and (3) carrying out spray drying on the slurry subjected to wet ball milling again, wherein the drying temperature is 280 ℃, the water content is dried to 7% in the process, and the material is spherical after spray drying.
Secondary sintering (Vitaceae, HK): calcining in a muffle furnace at 300 ℃ for 1h to complete the crystal grains, perfectly repairing, sintering at 300 ℃ for 10h, and performing 405 disc sintering and 4 Kg/disc sintering.
Drying to remove Water (WM): the water content of the material was less than 200ppm at a temperature of 150 ℃ under a vacuum of 100pa, taking 22h (18h heating +4h cooling).
Packaging: packaging environment 1% humidity.
Example 2: in the raw material mixing procedure, lithium carbonate is selected as a lithium source, and TiO is selected as a titanium source2·2H2The mass ratio of the lithium source to the titanium source to the water is 2:7:23, and the rest steps and parameters are the same as those of the waterExample 1.
Example 3: in the raw material mixing step, LiOH. H is added2O2.5 kg of anatase TiO2·2H2O7.5 kg, solvent H224kg of O, and continuously stirring for 8 hours; the rest of the steps and parameters were the same as in example 1.
Example 4: one spray drying Process (SD)1): introducing air at 200-220 ℃ into a spray dryer, and reducing the water content of the mixed raw materials to 4%; the rest of the steps and parameters were the same as in example 1.
Example 5: in the primary calcining process, the calcining temperature is 450-500 ℃, and the time is 10 hours; the rest of the steps and parameters were the same as in example 1.
Example 6: in the secondary calcining process, the calcining temperature is 450-500 ℃ and the time is 8 hours; the rest of the steps and parameters were the same as in example 1.
Comparative example 1: in the primary calcining process, the calcining temperature is 700 ℃ and the time is 4 hours; in the secondary calcining process, the calcining temperature is 800 ℃ and the time is 3 hours; the rest of the steps and parameters were the same as in example 1.
Comparative example 2: in the primary calcining process, the calcining temperature is 450-500 ℃, and the time is 10 hours; in the secondary calcining process, the calcining temperature is 800 ℃ and the time is 3 hours; the rest of the steps and parameters were the same as in example 1.
Comparative example 3: in the primary calcining process, the calcining temperature is 800 ℃ and the time is 3 hours; in the secondary calcining process, the calcining temperature is 450 +/-10 ℃ and the time is 12 hours; the rest of the steps and parameters were the same as in example 1.
The lithium titanate materials obtained in examples 1-6 and comparative examples 1-3 are used for battery preparation, wherein the weight ratio of lithium titanate: SP: PVDF ratio: 94%: 3%: 3 percent; the prepared batteries were subjected to performance tests, which are specifically shown in the following table.
TABLE 1
The lithium titanate material prepared by the scheme provided by the invention is used for preparing a battery, and can greatly increase the cycle number on the basis of ensuring that the discharge rate is equivalent to or slightly reduced from that of the traditional method.
Claims (10)
1. A preparation and synthesis method of a lithium titanate material for a lithium ion battery is characterized by comprising the following steps:
s1, mixing the lithium source, the titanium source and water, and stirring uniformly; then spray drying is carried out until the water content of the material is below 5%;
s2, sintering the material obtained in the step S1 for the first time;
s3, carrying out wet ball milling on the calcined dry material, and grinding the dry material to obtain nano slurry by taking water as a solvent and zirconia balls as a ball milling medium;
and (3) spray drying the nano slurry obtained from the S4 and the S3 again to obtain a spherical material, then carrying out secondary sintering, and finally carrying out vacuum drying at 120-180 ℃ to remove water, wherein the water content of the material is controlled to be less than 200ppm, so as to obtain the lithium titanate material for the lithium ion battery.
2. The method for preparing and synthesizing the lithium titanate material for the lithium ion battery according to claim 1, wherein the method comprises the following steps: the lithium source is LiOH. H2One or more of O, lithium carbonate and lithium acetate, and the titanium source is TiO2·2H2O, and the mass ratio of the lithium source to the titanium source to the water is 2-3: 6-8: 20-25.
3. The method for preparing and synthesizing the lithium titanate material for the lithium ion battery according to claim 2, wherein the method comprises the following steps: and (8) mixing the lithium source, the titanium source and water in the S1 to obtain a solid content of 20-40%, and continuously stirring for 4-10 h.
4. The method for preparing and synthesizing the lithium titanate material for the lithium ion battery according to claim 1, wherein the method comprises the following steps: and when drying in S1, drying by adopting air at 200-300 ℃.
5. The method for preparing and synthesizing the lithium titanate material for the lithium ion battery according to claim 1, wherein the method comprises the following steps: in S2, the sintering temperature is 300-500 ℃ and the time is 10-18 h.
6. The method for preparing and synthesizing the lithium titanate material for the lithium ion battery according to claim 1, wherein the method comprises the following steps: and after water is added into the dry materials in the S3, the solid content is 15-30%.
7. The method for preparing and synthesizing the lithium titanate material for the lithium ion battery according to claim 1, wherein the method comprises the following steps: in S3, the diameter of the zirconium balls is 0.25-0.4 mm, and the ball milling is carried out for 25-35 h; the specific surface area after ball milling is between 90 and 110m2Per g, particle size of the material D10 60~90nm，D50 250-300nm，D90 400~600nm，D99 650~800nm。
8. The method for preparing and synthesizing the lithium titanate material for the lithium ion battery according to claim 1, wherein the method comprises the following steps: when the spray drying is carried out in S4, the temperature is 200-300 ℃; drying to a water content of less than 7%.
9. The method for preparing and synthesizing the lithium titanate material for the lithium ion battery according to claim 1, wherein the method comprises the following steps: the sintering temperature in S4 is 300-500 ℃, and the sintering time is 8-15 h.
10. The lithium titanate material for the lithium ion battery prepared by the method of any one of claims 1 to 9 is a negative electrode material for the lithium ion battery.
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| US20200262714A1 (en) * | 2017-09-14 | 2020-08-20 | Neomaterials Pty Ltd | Synthesis of Lithium Titanate |
| 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 |
| CN112607769A (en) * | 2020-12-18 | 2021-04-06 | 北方奥钛纳米技术有限公司 | Lithium titanate battery material, preparation method and application thereof |
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- 2021-10-03 CN CN202111167148.0A patent/CN114031110A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104953107A (en) * | 2015-06-16 | 2015-09-30 | 北方奥钛纳米技术有限公司 | Preparation method of lithium titanate cathode material with high tap density |
| US20200262714A1 (en) * | 2017-09-14 | 2020-08-20 | Neomaterials Pty Ltd | Synthesis of Lithium Titanate |
| CN108565427A (en) * | 2018-04-16 | 2018-09-21 | 合肥国轩电池材料有限公司 | A kind of preparation method of carbon/lithium titanate composite material |
| CN112607769A (en) * | 2020-12-18 | 2021-04-06 | 北方奥钛纳米技术有限公司 | Lithium titanate battery material, preparation method and application 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 |
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