Preparation method of as-reduced ammonium tungsten bronze nanoparticles

A nanoparticle and tungsten bronze technology, which is applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of excessive sample particle size, easy decomposition, and decreased crystallization performance, and achieve uniform particle shape and synthesis steps. Simple, narrow particle size distribution effect

Active Publication Date: 2014-01-08
HARBIN INST OF TECH
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  • Summary
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the poor thermal stability of ammonium tungsten bronze, the decomposition temperature (300°C) is lower than the synthesis temperature, so the thermal reduction method cannot be used to synthesize ammonium tungsten bronze
Ammonium tungsten bronze is synthesized by pyrolysis method by ammonium paratungstate in reducing atmosphere (H 2 or H 2 and N 2 , Ar mixed gas, etc.) and thermally decomposed. In addition to the large particle size of the obtained sample, this method cannot obtain completely pure-phase ammonium tungsten bronze. The ammonium content in the sample is to

Method used

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  • Preparation method of as-reduced ammonium tungsten bronze nanoparticles
  • Preparation method of as-reduced ammonium tungsten bronze nanoparticles
  • Preparation method of as-reduced ammonium tungsten bronze nanoparticles

Examples

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Embodiment 1

[0026] Add 36ml oleic acid and 0.4g WCl to 100ml hydrothermal reaction kettle 6 After powdering, stir and mix at room temperature; after it is completely dissolved, add 4 ml of oleylamine, then seal the reaction vessel, and place it in an oven at 200 °C for 24 h to crystallize. After cooling to room temperature, it was separated by centrifugation, washed alternately with 30 mL deionized water and 30 mL absolute ethanol three times, and dried in vacuum to obtain ammonium tungsten bronze blue powder, which was a square-shaped ammonium tungsten bronze particle with an average diameter of 80nm.

Embodiment 2

[0028] Add 25ml oleic acid and 0.4g WCl to 100ml hydrothermal reaction kettle 6 After powdering, stir and mix at room temperature; after it is completely dissolved, add 15 ml of oleylamine, then seal the reaction vessel, and place it in an oven at 200 °C for 24 h to crystallize. After cooling to room temperature, centrifuge, wash with 30 mL deionized water and 30 mL absolute ethanol alternately three times, and vacuum dry to obtain ammonium tungsten bronze blue powder, which is rod-shaped ammonium tungsten bronze particles with an average diameter of 50nm. The nanorods have an average length of 350 nm.

Embodiment 3

[0030] Dissolve 0.4g of tungsten chloride in 32ml of oleic acid, stir well until it is completely dissolved, then add 8ml of oleylamine, mix until uniform, move to a supercritical reaction kettle, and crystallize at 350°C for 1 hour. After the reaction, the powder The sample was centrifuged, washed, and vacuum-dried at 60°C for 6 hours to obtain ammonium tungsten bronze blue powder, which was square ammonium tungsten bronze particles with an average diameter of 110nm.

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Abstract

The invention relates to a preparation method of as-reduced ammonium tungsten bronze nanoparticles and belongs to the field of inorganic oxide materials. Under the condition of solvothermal, organic long-chain high-boiling-point acid is used as reaction medium, an organic tungsten source and organic high-boiling-point amine are used as raw materials, and ammonium tungsten bronze nanoparticles are produced through one-step control in the non-water environment. A sample prepared by the preparation method is hexagonal ammonium tungsten bronze nano-crystal; the size of the nano-crystal is adjusted in a range of 80-500 nanometers; the form of the nano-crystal is even; the particle size distribution is narrow; chemical valence state of the nano-crystal is mixture of W6+ and W5+; the nano-crystal has rich free electrons. In addition, the sample prepared by the preparation method has high capacity of absorbing near infrared; the film containing the nanoparticles is effective in shielding 780-2500 micrometers near infrared and is highly permeable to visible light.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic oxide materials, and relates to a preparation method of reduced ammonium tungsten bronze nano powder. Background technique [0002] Tungsten bronze compounds are an important class of inorganic compounds, in which tungsten ions are represented by W 6+ , W 5+ and W 4+ Equivalent mixed valence states exist so that the overall charge of the compound is balanced. The rich crystal structure, tunnel structure and this special valence state make it have excellent properties, such as electronic and ionic conductivity, superconductivity, optical properties, etc. It is used in secondary batteries, electrochromic, near-infrared absorption and Applications such as chemical sensors have aroused extensive research interest. [0003] At present, the synthesis of tungsten bronze compounds mainly relies on wet chemical method, thermal reduction method and thermal decomposition method. The wet chemical ...

Claims

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Application Information

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IPC IPC(8): C01G41/00B82Y30/00
CPCY02P20/54
Inventor 刘绍琴果崇申颜美
Owner HARBIN INST OF TECH
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