Preparation method for novel lithium titanate material
A lithium titanate, a new type of technology, applied in the field of preparation of new lithium titanate materials, can solve the problems of poor ion transmission and low electronic conductivity, and achieve high specific energy, large specific surface area, and good rate performance.
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Embodiment 1
[0030] (1) First add tetrabutyl titanate and lithium nitrate into methanol according to the molar ratio of 4:5, the concentration of tetrabutyl titanate in methanol is 0.19mol / L, stir in vacuum for 7h to mix evenly (vacuum pressure is - 0.08Mpa), and then add distilled water with the same volume as methanol to make a milky white gel;
[0031] (2) Put the gel into the reaction kettle to evacuate (vacuum pressure is -0.08Mpa), carry out organic solvent-hydrothermal reaction, the reaction temperature is 150°C, the reaction time is 25h, the product is washed 4 times with methanol, and then Vacuum dry at 72°C for 3.5h (vacuum pressure is -0.08Mpa) to obtain the precursor;
[0032] (3) The precursor was then sintered at 610 °C for 1.3 h under the protection of argon to obtain flake Li 4 Ti 5 o 12 Material (99.1% pure);
[0033] (4) The Li obtained in step (3) 4 Ti 5 o 12 The material was mixed with mesophase pitch (Li 4 Ti 5 o 12 The mass ratio of material to mesophase pit...
Embodiment 2
[0036] (1) First add tetrabutyl titanate and lithium nitrate into methanol according to the molar ratio of 4:4.9, the concentration of tetrabutyl titanate in methanol is 0.2mol / L, stir in vacuum for 7h to mix evenly (vacuum pressure is -0.09 Mpa), and then add distilled water (the volume ratio of distilled water to methanol is 1:0.95) to make a milky white gel;
[0037] (2) Put the gel into the reaction kettle to vacuum (vacuum pressure is -0.09Mpa), carry out organic solvent-hydrothermal reaction, the reaction temperature is 160°C, the reaction time is 20h, the product is washed with methanol for 3 times, and then Vacuum dry at 72°C for 3.5h (vacuum pressure is -0.09Mpa) to obtain the precursor;
[0038] (3) The precursor was then sintered at 580 °C for 1.5 h under the protection of argon to obtain flake Li 4 Ti 5 o 12 Material (98.6% pure);
[0039] (4) The Li obtained in step (3) 4 Ti 5 o 12 The material was mixed with glucose (Li 4 Ti 5 o 12 The mass ratio of mat...
Embodiment 3
[0042] (1) First add tetrabutyl titanate and lithium nitrate into methanol according to the molar ratio of 4:5.1, stir in vacuum for 7 hours to mix evenly (vacuum pressure is -0.08Mpa), and then add a certain amount of distilled water to make a milky white gel glue.
[0043] (2) Put the gel into the reactor to vacuumize (vacuum pressure is -0.08Mpa), carry out organic solvent-hydrothermal reaction, the reaction temperature is 150°C, the reaction time is 23h, the product is washed with methanol 4 times, and then Dry in vacuum at 72°C for 3.5h (vacuum pressure is -0.08Mpa) to obtain the precursor.
[0044] (3) The precursor was then sintered at 620 °C for 1.0 h under the protection of argon to obtain flake Li 4 Ti 5 o 12 Material (98.5% pure);
[0045] (4) The Li obtained in step (3) 4 Ti 5 o 12 Material mixes with sucrose (mass ratio is the same as embodiment 2), adds oxalic acid (oxalic acid is the same as Li 4 Ti 5 o 12 The material mass ratio is 1:100) and mixed even...
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