Method for preparing steady phase-A vanadium dioxide nanorod

A technology of vanadium dioxide and nanorods, which is applied in the field of preparation of phase A vanadium dioxide powder, can solve the problems of difficult synthesis, high synthesis temperature, and small filling ratio, and achieve good crystallinity, good ductility, and crystallinity. The effect of small particle size

Inactive Publication Date: 2012-10-31
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

Recently, Jin et al. synthesized phase A vanadium dioxide at 270 °C by hydrothermal method, and studied the effect of doping on its reversible phase transition, but phase A is an unstable phase, and the synth

Method used

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  • Method for preparing steady phase-A vanadium dioxide nanorod
  • Method for preparing steady phase-A vanadium dioxide nanorod
  • Method for preparing steady phase-A vanadium dioxide nanorod

Examples

Experimental program
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Embodiment 1

[0032] Disperse 3.64 g of vanadium pentoxide powder in 200 g of an aqueous solution of oxalic acid with a concentration of 0.1 M, and stir vigorously for 10 minutes to obtain an aqueous solution of vanadium ions with a molar concentration of 0.2 mol / L and a pH of 2.1. The above solution was added to a 250ml hydrothermal kettle, the filling ratio was 80%, the temperature was raised to 200°C, the temperature was maintained for 24 hours, synthesized through a hydrothermal reaction, slowly cooled to room temperature, centrifuged, and dried in an oven at 70°C for 24 hours to obtain The A-phase vanadium dioxide nanorods were 2.97 g, and the yield was 99%. like figure 1 The XRD spectrum shows that its crystal phase is pure A phase, such as figure 2 As shown in the TEM photo, the obtained vanadium dioxide powder is rod-shaped, and each vanadium dioxide rod is a single crystal and has a certain length and thickness. After testing, the obtained A-phase vanadium dioxide nanorods have...

Embodiment 2

[0034] 4.5 g of oxalic acid (2M) was added to 125 ml of an aqueous solution of vanadium oxychloride with a concentration of 0.005 mol / L, and vigorously stirred for 10 minutes to obtain an aqueous solution of vanadium ions with a molar concentration of 0.005 mol / L and a pH of 1.5. The above solution was added to a 250ml hydrothermal kettle, the filling ratio was 50%, the temperature was raised to 219°C, the temperature was maintained for 0 hours, synthesized through a hydrothermal reaction, then slowly cooled to room temperature, centrifuged, and dried in an oven at 70°C for 24 hours. 0.8 g of A-phase vanadium dioxide nanorods were obtained with a yield of 98%. After testing, the obtained A-phase vanadium dioxide nanorods have a diameter of 500 nm and a length of 1-6 μm. The aspect ratio is: 1:1~12:1.

Embodiment 3

[0036] 150 ml of an aqueous solution of vanadyl oxalate with a molar concentration of 0.1 mol / L was prepared, stirred vigorously for 10 minutes, and the pH was 2.6. The above solution was added to a 250ml hydrothermal kettle, the filling ratio was 60%, the temperature was raised to 200°C, the temperature was maintained for 1 hour, synthesized by hydrothermal reaction, then slowly cooled to room temperature, centrifuged, and dried in an oven at 70°C for 24 hours , 2.2 g of A-phase vanadium dioxide nanorods were obtained with a yield of 98%. After testing, the obtained A-phase vanadium dioxide nanorods have a diameter of 1 μm, a length of 30 to 50 μm, and an aspect ratio of 30:1 to 50:1.

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Abstract

The invention provides a method for preparing a steady phase-A vanadium dioxide nanorod. The method includes directly adding aqueous solution containing tetravalent vanadium ions into a hydrothermal kettle for hydrothermal reaction, and enabling the filling ratio of the hydrothermal kettle in the hydrothermal reaction process to range from 50% to 90%; heating and controlling the hydrothermal reaction temperature to range from 180 DEG C to 220 DEG C and keeping the hydrothermal reaction temperature for 0-720 hours; and cooling, centrifuging, washing and drying a compound obtained by hydrothermal reaction to prepare the steady phase-A vanadium dioxide nanorod with the length-diameter ratio ranging from 1:1 to 1000:1. The method has the advantages that special equipment is omitted, operation is simple and convenient, and yield is high.

Description

Technical field [0001] The present invention involves the preparation of the powder system in the field of chemical industry and the material field, and specially involves the preparation of stable A -phase dioxide powder. Background technique [0002] The oxide of the 多 is a complex system of multi -price and polycrystalline phase. Its crystal structure is more than 10 species, mainly including B phase, A phase, M phase, and R.At present, the most studies are M / R phase dioxide with thermal discoloration performance, which can be widely used in the fields of smart window coating, photoelectric switch, thermistor and optical information storage.Because the B phase dioxide can also receive a lot of attention because it can be used as the negative electrode material of the battery.Due to the difficulty in preparation, A -phase dioxide has not attracted enough attention and attention of technicians in the art. [0003] A-phase dip oxide 是 was originally used by Thébald (F. Thébald, J...

Claims

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Application Information

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IPC IPC(8): C01G31/02B82Y40/00
Inventor 高彦峰曹传祥戴雷陈长罗宏杰金平实
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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