Solid-phase synthesis method for caesium tungsten bronze powder

A solid-phase synthesis method, cesium tungsten bronze technology, applied in tungsten compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of increasing gas source cost, increasing equipment investment, etc., achieve short reaction cycle, save gas source, The effect of simple synthesis process

CN105016392AActive Publication Date: 2015-11-04烟台佳隆纳米产业有限公司
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2015-11-04

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Abstract

The invention belongs to the technical field of metal oxide powder preparation and particularly relates to a solid-phase synthesis method for caesium tungsten bronze powder. The solid-phase synthesis method comprises the following steps of weighing a tungsten compound and cesium salt according to the W / Cs molar ratio (2-3.5):1, and mixing and grinding; placing the ground substance into a sealed vessel to react at the temperature of 750-800 DEG C for 1-2 hours; and ending the reaction to obtain the black blue caesium tungsten bronze powder with complete crystallinity, wherein the crystal phase comprises the component, namely Cs0.3WO3 or Cs0.32WO3. According to the solid-phase synthesis method, a solid raw material is adopted to directly react in a sealed vessel, inert gases or reducing gases are not needed to be introduced, and a gas generated by self-reaction is used as a protecting gas, so that the obtained powder is black blue, the air source is saved, and the cost is reduced; in addition, the synthesis process disclosed by the invention is simple, short in reaction period and suitable for industrial production.
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Description

technical field

[0001] The invention belongs to the technical field of metal oxide powder preparation, in particular to a solid phase synthesis method of cesium tungsten bronze powder. Background technique

[0002] WO 3 It has excellent performance in electrochromism, catalysis, gas sensitivity, etc. Its composite oxide - tungsten bronze, generally refers to a metal oxide with a darker metallic luster, and is usually a metal conductor or metal semiconductor, tungsten Bronze Formula A x WO 3 , However, with the different types and moles of cations—the values ​​of A and x, the structure and color of the compound will be different (J Analytical and Pyrolysis, 2000, 56:23-31). At present, there are many potassium cesium tungsten bronzes and cesium tungsten bronzes. Because of its low resistance, excellent visible light transmittance and near-infrared shielding performance, cesium tungsten bronze is widely used to prepare conductive films, and is used in transparent heat insul...

Examples

Embodiment 1

[0025] A solid phase synthesis method of cesium tungsten bronze powder, comprising the following steps:

[0026] (1) Weigh 9.6g of ammonium tungstate and 3.1g of cesium carbonate, and grind them until they are evenly mixed;

[0027] (2) Put the ground material into a closed container and put it into a muffle furnace for reaction, the reaction temperature is 800°C, and the reaction time is 1h;

[0028] (3) After the reaction, blue-black cesium tungsten bronze powder with complete crystallinity is obtained.

[0029] The cesium tungsten bronze powder prepared in this embodiment has a metallic luster and is blue-black. from figure 1 It can be seen from the figure that the cesium tungsten bronze powder has high crystallinity and the crystal phase composition is Cs 0.3 WO 3 or Cs 0.32 WO 3 .

Embodiment 2

[0031] A solid phase synthesis method of cesium tungsten bronze powder, comprising the following steps:

[0032] (1) Weigh 11.3g of tungstic acid and 3.0g of cesium hydroxide, grind them until they are evenly mixed;

[0033] (2) Put the grinding material into a closed container and put it into a muffle furnace for reaction. The reaction temperature is 800°C and the reaction time is 2 hours;

[0034] (3) After the reaction, blue-black cesium tungsten bronze powder with complete crystallinity is obtained.

[0035] The cesium tungsten bronze powder prepared in this embodiment has a metallic luster and is blue-black. from figure 2 It can be seen from the figure that the cesium tungsten bronze powder has high crystallinity and the crystal phase composition is Cs 0.3 WO 3 or Cs 0.32 WO 3 .

Embodiment 3

[0037] A solid phase synthesis method of cesium tungsten bronze powder, comprising the following steps:

[0038] (1) Weigh 14.4g of ammonium tungstate and 3.7g of cesium nitrate, grind them until they are evenly mixed;

[0039] (2) Put the ground material into a high-temperature-resistant crucible, put the charged crucible into a closed stainless steel container, seal it and put it into a muffle furnace for reaction. The reaction temperature is 750°C and the reaction time is 2 hours;

[0040] (3) After the reaction, blue-black cesium tungsten bronze powder with complete crystallinity is obtained.

[0041] The cesium tungsten bronze powder prepared in this embodiment has a metallic luster and is blue-black. from image 3 It can be seen from the figure that the cesium tungsten bronze powder has high crystallinity and the crystal phase composition is Cs 0.3 WO 3 or Cs 0.32 WO 3 ;from Figure 4 It can be seen that its transmittance in the near-infrared region is low, indica...