Method for preparing nanometer electrode material Li4Ti5O12/Rutile-TiO2 by compound solvent thermal process
A nano-electrode and composite solvent technology, applied in battery electrodes, nanotechnology, nanotechnology, etc., to achieve low viscosity, good solvent thermal critical reaction conditions, and reduce losses
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Embodiment 1
[0036] (1) Dissolve 2.5mL of tetrabutyl titanate in 35mL of diethylene glycol and water mixed solution (2.5:1 by volume), and magnetically stir for 1 hour to make it evenly mixed to obtain a mixed solution;
[0037] (2) 0.268g LiOH·H 2 O was dissolved in 15mL of deionized water, and ultrasonically vibrated for half an hour to completely dissolve the lithium hydroxide to obtain an aqueous solution of lithium hydroxide;
[0038] (3) Add lithium hydroxide aqueous solution to the mixed solution obtained in step (1) drop by drop, after stirring for 5 hours, transfer the reaction solution to a 100mL stainless steel autoclave, and keep it at 180°C for 36 hours, and obtain a white precipitate after solvent heat treatment ; After being washed by centrifugation for 5 times and dried in an oven at 80°C, the precursor was obtained;
[0039] (4) Put the obtained precursor in a muffle furnace, calcinate in air atmosphere at 550-600°C for 6 hours, cool naturally to room temperature, and gri...
Embodiment 2
[0041] (1) Dissolve 2.5mL of tetrabutyl titanate in 35mL of diethylene glycol and water mixed solution (2.5:1 by volume), and magnetically stir for 1 hour to make it evenly mixed to obtain a mixed solution;
[0042] (2) 0.268g LiOH·H 2 O was dissolved in 15mL of deionized water, and ultrasonically vibrated for half an hour to completely dissolve the lithium hydroxide to obtain an aqueous solution of lithium hydroxide;
[0043] (3) Add lithium hydroxide aqueous solution to the mixed solution obtained in step (1) drop by drop, after stirring for 5 hours, transfer the reaction solution to a 100mL stainless steel autoclave, and keep it at 180°C for 36 hours, and obtain a white precipitate after solvent heat treatment ; After being washed by centrifugation for 5 times and dried in an oven at 80°C, the precursor was obtained;
[0044] (4) Place the obtained precursor in a muffle furnace, calcinate at 650-700°C for 6 hours in an air atmosphere, cool naturally to room temperature, an...
Embodiment 3
[0046] The nanometer electrode material LTO / TO-R that embodiment 1 and 2 obtains carries out XRD diffraction analysis and scanning electron microscope (SEM) morphology analysis, and the result is as follows figure 1 , image 3 shown.
[0047] figure 1 The XRD diffraction analysis spectrum of LTO / TO-R at different temperatures shows that the diffraction peaks of the samples calcined at 650-700°C ( figure 1 (b)) is consistent with LTO, TO-R standard cards; and the sample after calcining at 550-600 ° C is analyzed by XRD diffraction spectrum ( figure 1 (a) shows that in addition to the diffraction peaks of LTO and TO-R, anatase TiO also appeared 2 (TO-A) impurity peak; figure 1 In (a) and figure 1 The comparison in (b) shows that the XRD diffraction peaks of the sample LTO / TO-R calcined at 650-700°C are sharper, and the purity and crystallinity are higher.
[0048] Depend on image 3 (b) It can be seen that the target product LTO / TO-R obtained after calcination at 650-700°...
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