Preparation method for preparing phase-transition temperature adjustable pure-phase VO2 powder through one-step hydrothermal
A phase transition temperature, VO2 technology, applied in vanadium oxide and other directions, can solve the problems of inability to achieve continuous adjustment, inability to use actual production, poor process repeatability, etc., to achieve the effect of short production cycle, low cost, and breakthrough of application bottlenecks
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[0021] The embodiment of the present invention provides a one-step hydrothermal preparation of pure phase VO with adjustable phase transition temperature 2 The preparation method of powder comprises the following steps:
[0022] Step a, mix oxalic acid and deionized water at a mass ratio of 1:39, perform magnetic stirring in a water bath at a constant temperature, then add vanadium source, continue magnetic stirring in a water bath at a constant temperature, adjust the temperature of the water bath to 80-100°C, and stir at a constant temperature of 0.5 ~2h to obtain the precursor;
[0023] Step b. Put the precursor prepared in step a into the reactor, and conduct a hydrothermal reaction at 280°C for 72 hours to obtain the product;
[0024] Step c, centrifuging the product of step b, washing with a mixture of absolute ethanol and deionized water with a volume ratio of 1:2 to 1:5, and vacuum drying at 50° C. for 6 hours to obtain the target product.
[0025] In the step a, the...
Embodiment 1
[0033] Example 1 of the present invention provides a one-step hydrothermal preparation of pure phase VO with adjustable phase transition temperature 2 The preparation method of powder comprises the following steps:
[0034] a. Add 1.891g of oxalic acid to the beaker, add 75mL of deionized water, and stir magnetically in a water bath at a constant temperature of 40°C for 5 minutes. ℃, stirring at constant temperature for 0.5h to obtain the precursor;
[0035] b. Put the precursor prepared in step a into the reactor, and conduct a hydrothermal reaction at 280°C for 72 hours;
[0036] c. Centrifuge the product of step b, wash it with a mixture of absolute ethanol and deionized water with a volume ratio of 1:2, and dry it in a vacuum oven at 50°C for 6 hours to obtain impure VO in a crystalline phase 2 Powder. The X-ray diffraction (XRD) pattern of the product is as figure 1 As shown, the scanning electron microscope (SEM) pattern is as figure 2 shown.
Embodiment 2
[0038] Example 2 of the present invention provides a one-step hydrothermal preparation of pure phase VO with adjustable phase transition temperature 2 The preparation method of powder comprises the following steps:
[0039] a. Add 1.891g of oxalic acid into the beaker, add 75mL of deionized water, stir magnetically in a water bath at 40°C for 5 minutes, add 1.755g of ammonium metavanadate into the above solution, stir magnetically in a water bath at 40°C for 15min, and adjust the temperature of the water bath to 90 °C, stirring at constant temperature for 1 h to obtain the precursor;
[0040] b. Put the precursor prepared in step a into the reactor, and conduct a hydrothermal reaction at 280°C for 72 hours;
[0041]c. Centrifuge the product of step b, wash it with a mixture of absolute ethanol and deionized water with a volume ratio of 1:3, and dry it in a vacuum oven at 50°C for 6 hours, then put it in a furnace for annealing treatment, and pass Into a protective atmosphere...
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