Preparation method of VO2(M) nano powder and film through spray pyrolysis

A nano-powder, VO2 technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of long synthesis cycle and increased production cost, and achieve short synthesis cycle, low cost, The effect of simple process

Active Publication Date: 2016-08-03
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] At present, thermal cracking method (Chinese patent CN1321067C) prepares VO 2 (M) Nanopowder: After the precursor is pulverized, it needs to be pyrolyzed at 350-500°C under vacuum conditions, and finally the product vanadium dioxide is obtained; the spray pyrolysis method (US Patent US5427763) requires H 2 Only by restoring the atmosphere can we get VO 2 (M), the above method requires stricter experimental atmosphere; patent CN101391814A which discloses one-step hydrothermal

Method used

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  • Preparation method of VO2(M) nano powder and film through spray pyrolysis
  • Preparation method of VO2(M) nano powder and film through spray pyrolysis
  • Preparation method of VO2(M) nano powder and film through spray pyrolysis

Examples

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Embodiment 1

[0035] (1) Prepare an ethylene glycol solution of 0.2mol / L ammonium metavanadate and heat it to 20°C and stir for 200 minutes to obtain a transparent precursor solution; (2) Use a ceramic sheet as the substrate and heat it to 240°C with an electric constant temperature heating plate; (3) The distance from the atomizer nozzle to the substrate is adjusted to 8cm, and the carrier gas N 2 Velocity is 0.36m 3 / h, the spraying time is 300s, and VO 2 (M) Nanopowder.

[0036] figure 2 Shown is the XRD of the product prepared under this condition, indicating that the vanadium dioxide prepared by this method is M phase.

Embodiment 2

[0038] (1) Prepare ethylene glycol solution of 1mol / L ammonium metavanadate, heat to 80°C and stir for 30min, then cool to room temperature to obtain a transparent precursor solution; (2) Use a ceramic sheet as the substrate, and heat it to 260°C with an electric constant temperature heating plate ℃; (3) The distance from the atomizer nozzle to the substrate is adjusted to 15cm, and the carrier gas Ar flow rate is 1.2m 3 / h, the spraying time is 1200s, and VO 2 (M) Nanopowder.

[0039] image 3 Shown is the XRD of the product prepared under this condition, indicating that the vanadium dioxide prepared by this method is M phase.

Embodiment 3

[0041](1) Prepare an ethylene glycol solution of 0.5mol / L ammonium metavanadate, heat it at 95°C and stir for 5 minutes, and cool to room temperature to obtain a transparent precursor solution; (2) Use a ceramic sheet as the substrate and heat it to 280 ℃; (3) The distance from the atomizer nozzle to the substrate is adjusted to 10cm, and the carrier gas N 2 Velocity is 0.05m 3 / h, spraying time 720s, that is, get VO 2 (M) Nanopowder.

[0042] Figure 4 Shown is the XRD of the product prepared under this condition, indicating that the vanadium dioxide prepared by this method is M phase.

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Abstract

The invention relates to a preparation method of VO2(M) nano powder and film through spray pyrolysis. The preparation method comprises the following steps: adding ammonium meta-vanadate into a glycol solvent, heating and stirring to form a transparent and uniform precursor solution with a concentration of 0.02 to 1 mol/L finally, then atomizing the precursor into droplets by an atomizer, spraying the droplets to a heated substrate by carrier gas, decomposing precursors on the substrate, after the products deposit for a while, and collecting the products namely VO2(M) nano powder or film; wherein a doping agent is added during the preparation process of precursor so as to reduce the phase change temperature of vanadium dioxide to room temperature. The operation of the preparation method is simple, the cost is largely reduced, the synthesis period of vanadium dioxide (M) is effectively shortened, and the preparation method can be applied to large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of inorganic functional materials, in particular to a spray pyrolysis method for preparing VO 2 (M) The method of nanopowder and thin film. Background technique [0002] Vanadium dioxide is a functional material with a variety of crystal structures, and the M-phase structure of vanadium dioxide has been studied the most in recent years because it has completely reversible metal-insulator phase transition characteristics at 68 °C. At low temperature, the M phase has a monoclinic crystal structure with high transmittance to infrared light; however, at high temperature, it transforms into an R phase with a tetragonal crystal structure, which has a high reflection effect on infrared light. At the same time, the resistivity before and after the phase transition will also change by 4-5 orders of magnitude. [0003] Therefore, VO 2 The (M) phase has a good application prospect in energy-saving windows and electronic devic...

Claims

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Application Information

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IPC IPC(8): C01G31/02B82Y30/00C03C17/23
CPCB82Y30/00C01G31/02C01P2002/72C01P2004/64C03C17/23C03C2217/21
Inventor 肖秀娣徐刚曹子宜陆泫茗
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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