Method for preparing spherical titanium oxide niobate anode material in large scale by utilizing spray drying method and application thereof to lithium ion battery
A large-scale preparation and spray-drying technology, which is applied to niobium compounds, chemical instruments and methods, and battery electrodes, can solve the problem of low theoretical capacity and achieve low raw material costs, excellent high-rate charge and discharge performance, and safety performance. The effect of broad application prospects
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specific Embodiment approach 1
[0027] Specific implementation method one: disperse tetrabutyl phthalate and niobium ethoxide in equimolar ratio and dissolve in ethanol, fully stir to make it disperse evenly, then add equal volume of distilled water to mix and stir, put it in the spray drier It is sprayed at a flow rate of 10ml / min, and the nozzle temperature is 150°C. figure 1 and figure 2 That is, TiNb prepared by spray drying 2 o 7 The scanning electron microscope image of the nanosphere shows the typical spherical particles at the Chen correlation point of the material. The obtained powder is dried in an oven at 80°C to obtain a white precursor, and then the precursor is calcined in a tube furnace at 900°C in an air atmosphere to obtain spherical TiNb 2 o 7 Negative material.
specific Embodiment approach 2
[0028] Specific embodiment two: Disperse and dissolve titanium isopropoxide (isopropyl titanate) and niobium hydroxide in equal molar ratios in water, where a certain amount of oxalic acid needs to be added in advance to prevent hydrolysis at a concentration of 0.5 mol / L , fully stirred to disperse evenly, sprayed out in a spray dryer at a speed of 5ml / min, and the spraying temperature from spray drying was 180°C. The obtained powder is dried in an oven to obtain a precursor, and then the precursor is calcined in a high-temperature furnace at 1000°C in an air atmosphere to obtain spherical TiNb 2 o 7 Negative material. image 3 and Figure 4 That is the morphology of spherical TNO after calcination.
specific Embodiment approach 3
[0029] Specific embodiment three: Titanium isopropoxide (isopropyl titanate) and niobium hydroxide in equimolar ratio are dispersed and dissolved in water, wherein a certain amount of oxalic acid needs to be added in advance to prevent hydrolysis, the concentration is 0.2mol / L, Thoroughly stir it to disperse it evenly, spray it in the spray dryer at a speed of 20ml / min, the spray temperature from spray drying is 200°C, increase the flow rate and nozzle temperature to obtain the precursor material of large particles, and then Improve its tap density and the energy density of the battery. The obtained powder is dried in an oven to obtain a precursor, and then the precursor is calcined in a high-temperature furnace at 1200°C in an air atmosphere to obtain a larger volume of spherical TiNb 2 o 7 Negative material.
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