Method for preparing D-phase vanadium dioxide
A technology of vanadium dioxide and vanadium pentoxide, applied in vanadium oxide and other directions, can solve the problems of long hydrothermal time and difficult product purification, and achieve the effects of short reaction time, simple and easy-to-obtain raw materials, and uniform particle size.
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Embodiment 1
[0027] Prepare D-phase vanadium dioxide, the steps are as follows:
[0028] 1) Dissolve 0.91g of vanadium pentoxide in 175mL of ultrapure water, then add 2.25g of oxalic acid to the above solution, control the molar ratio of vanadium pentoxide to oxalic acid to be 1:5, and the concentration of vanadium pentoxide to be 0.028 mol / L, stirred for 15 minutes to obtain a precursor solution;
[0029] 2) Transfer the precursor solution to a 250mL micro-stirred reactor, and react at 260°C for 24 hours. After the reaction, after the reactor is cooled to room temperature, the obtained hydrothermal product is centrifuged and washed with deionized water. and absolute ethanol for 3 times, and then the centrifuged product was dried in a vacuum oven at 80° C. for 8 hours to obtain a spherical D-phase vanadium dioxide powder.
[0030] The phase and morphology of the product obtained in this example were characterized by X-ray diffraction analysis and scanning electron microscope (SEM). figur...
Embodiment 2
[0032] Prepare D-phase vanadium dioxide, the steps are as follows:
[0033] 1) Dissolve 1.82g of vanadium pentoxide in 175mL of ultrapure water, then add 3.60g of oxalic acid into the above solution, the molar ratio of vanadium pentoxide to oxalic acid is 1:4, and the concentration of vanadium pentoxide is 0.057mol / L, stirred for 15 minutes to obtain a precursor solution;
[0034] 2) Transfer the precursor solution to a 250mL micro-stirred reactor, and react at 240°C for 8 hours. After the reaction, after the reactor was cooled to room temperature, the obtained hydrothermal product was centrifuged, and deionized The water and absolute ethanol were washed three times respectively, and then the centrifuged product was vacuum-dried at 80° C. for 12 hours to obtain a spherical D-phase vanadium dioxide powder.
[0035] image 3 The scanning electron microscope image of the D-phase vanadium dioxide powder prepared for this example shows that the D-phase particles are spherical pa...
Embodiment 3
[0037] Prepare M-phase vanadium dioxide, the steps are as follows:
[0038] 1) Dissolve 1.82g of vanadium pentoxide in 175mL of ultrapure water, then add 2.7g of oxalic acid to the above solution, control the molar ratio of vanadium pentoxide to oxalic acid to 1:3, and the concentration of vanadium pentoxide to 0.057 mol / L, stirred for 15 minutes to obtain a precursor solution;
[0039] 2) Transfer the precursor solution to a 250mL micro-stirred reactor, and react at 220°C for 6h. Washing with water and absolute ethanol, and then drying the centrifuged product in a vacuum oven at 60°C for 16 hours to obtain a spherical D-phase vanadium dioxide powder;
[0040] 3) Annealing the obtained vanadium dioxide powder at a temperature of 400° C. and a vacuum degree of 300 Pa for 1 h to obtain an M-phase vanadium dioxide powder.
[0041] Figure 4 Scanning electron micrographs (SEM) of the D-phase vanadium dioxide prepared in this example before and after annealing, wherein a is befo...
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