Doping-free low-temperature thermally variable vo 2 Preparation method of powder material
A technology of powder materials and low-temperature heating, which is applied in the field of nano-VO2 preparation, can solve the problems of long process flow, high preparation cost, uncontrollable phase transition temperature, etc., and achieve the solution of uneven doping, high crystallinity, high The effect of added value
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[0033] Specifically, non-doped low temperature thermogenic VO 2 Method for preparing powder material, which comprises the following steps:
[0034] A, the vanadium pentoxide is mixed with deionized water, and then into the solution of the reducing agent, when the solution color from earth yellow to dark blue stop ventilation, and warm stirring, to get solution A;
[0035] B, dilute solution A to a total vanadium concentration of 0.05 ~ 0.2mol / L, and then add CTAB or PEG-400, and then add sodium hydroxide solution to adjust the solution pH to 3.8 ~ 4.0, continue to stir, to get solution B;
[0036]C, the solution B with deionized water and absolute ethanol alternate centrifugal washing, precipitation after drying, grinding, to obtain a solid powder;
[0037] D, the solid powder and ethanol solution mixed ultrasonic dispersion, first in 120 ~ 180 °C temperature insulation 1 ~ 2h, and then heated to 260 °C ~ 300 °C, continue to insulation 4 ~ 24h, after the end of the insulation, c...
Embodiment 1
[0049] Take 200mL of vanadium solution with a concentration of 1.83mol / L dilute to n(TV)=0.05mol / L, add 7.4g CTAB to stir evenly, and slowly add a concentration of 30g / L of sodium hydroxide solution drop by drop to adjust the solution pH to 3.8, the droplet acceleration rate is controlled at 0.5 mL / min, and continue stirring for 5min after the end of drop-by-drop;
[0050] After the end of stirring, it was washed 6 times with alternating centrifugation of deionized water and absolute ethanol, and the obtained precipitate product was dried in vacuo at 60 °C for 18 h, and the solid powder was ground to obtain;
[0051]Weigh 0.5g of the solid powder, add 70mL volume fraction of 50% ethanol solution in ultrasonic dispersion for 30min, and pour into a hydrothermal reactor with a volume of 100mL, insulation at a temperature of 120 °C for 2h, heating to 260 °C after the completion of heat preservation, continue to insulation for 24h, heating rate controlled at 6 °C / min, after the end of...
Embodiment 2
[0054] Take 200mL of vanadium solution with a concentration of 1.83mol / L dilute to n(TV)=0.1mol / L, add 73.2ml of PEG-400 and stir evenly, and slowly add a concentration of 40g / L of sodium hydroxide solution drop by drop to adjust the solution pH to 3.9, the drop acceleration rate is controlled at 1mL / min, and continue to stir for 15min after the end of the drop addition;
[0055] After the end of stirring, it was washed 6 times with alternating centrifugation of deionized water and absolute ethanol, and the obtained precipitate product was dried in vacuo at 60 °C for 18 h, and the solid powder was ground to obtain;
[0056] Weigh 1g of the solid powder, add 70mL of ethanol solution with a volume fraction of 50% ultrasonic dispersion for 30min, and pour into a hydrothermal reactor with a volume of 100mL, incubate at a temperature of 150 °C for 1.5h, heat up to 280 °C after the completion of insulation, continue to hold for 18h, the heating rate is controlled at 6 °C / min, after the ...
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