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Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles

A technology of nanoparticle and mixed valence state, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science. It can solve problems such as complex methods and large product sizes, and achieve simple synthesis steps, uniform particles, and The effect of strong near-infrared absorption ability

Inactive Publication Date: 2014-01-29
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to literature reports, there are many methods that can be used to synthesize W 18 o 49 Nanopowder, but the shape of the product is one-dimensional material, such as nanowire, nanotube, etc.
At the same time, most of the synthesis steps involve high temperature processes and the use of chemically toxic and corrosive expensive organic reagents
In recent years, the literature has reported the hydrothermal synthesis of W 18 o 49 Nanoparticles, but the synthesis method is divided into two steps, including hydrothermal synthesis and subsequent reduction treatment of the product, which is complex and the product size is large

Method used

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  • Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles
  • Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles
  • Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles

Examples

Experimental program
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Effect test

Embodiment 1

[0029] In this example, tungsten hexachloride is used as the tungsten source, the concentration is 15 mmol / L, and n-propanol is used as the reducing agent. The specific preparation steps are as follows:

[0030] After adding 50 ml of n-propanol to a 100 ml hydrothermal reaction kettle, add 0.2976 g of tungsten hexachloride powder, and stir and mix at room temperature. After the solution is completely mixed, seal the reaction kettle and place it in an oven at 200°C Crystallized for 22 h. After cooling to room temperature, centrifuge, wash with deionized water and absolute ethanol alternately, and dry in vacuum to obtain mixed valence tungsten-based nanoparticle powder. like figure 2 As shown, the sample prepared in this example is a shuttle-shaped nanoparticle with a length of about 450 nm and a diameter of about 180 nm in the middle.

Embodiment 2

[0032] In this example, tungsten ethanol (Ⅴ) was used as the tungsten source, the concentration was 4.4 mmol / L, and ethanol was used as the reducing agent. The specific preparation steps are as follows:

[0033] After adding 50ml of absolute ethanol to a 100 ml hydrothermal reaction kettle, add 0.09 g of tungsten ethoxide (Ⅴ) dropwise, and stir and mix at room temperature. 22 h. After cooling to room temperature, centrifuge, wash with deionized water and absolute ethanol in sequence, and vacuum dry to obtain mixed valence tungsten-based nanoparticle powder. like image 3 As shown, the sample prepared in this embodiment is a sheet-like nanoparticle with a length and width of about 30 nm.

Embodiment 3

[0035] In this example, tungsten ethoxide (Ⅴ) is used as the tungsten source, the concentration is 10 mmol / L, and ethanol is used as the reducing agent. The specific preparation steps are as follows:

[0036] After adding 50ml of absolute ethanol to a 100ml hydrothermal reaction kettle, add 0.2047 g of tungsten ethoxide (Ⅴ) dropwise, and stir and mix at room temperature. After the solution is completely mixed, seal the reaction kettle and place it in an oven at 200°C for crystallization 22 h. After cooling to room temperature, centrifuge, wash with deionized water and absolute ethanol in sequence, and vacuum dry to obtain mixed valence tungsten-based nanoparticle powder. like Figure 4 As shown, the samples prepared in this embodiment are spherical nanoparticles with a diameter of about 130 nm.

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Abstract

The invention relates to a method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles, belonging to the field of the preparation of inorganic oxide materials. The method comprises the steps of dissolving a tungsten source into organic straight-chain alcohol, mixing uniformly under magnetic stirring, then, transferring a solution to a reactor for crystallization reaction, and carrying out centrifugation, washing and vacuum drying on a powder sample after reaction, thereby obtaining a powder sample. According to the method, the synthesis steps are simple, and the obtained particles are uniform, are controllable in morphology and size and have excellent and stable near-infrared ray absorbing performance. According to the sample prepared by the method, the sample is a monoclinic-phase W18O49 nanocrystal, the size can be regulated and controlled between 50nm and 2,000nm, the form is uniform, the morphology can be nanowires, nanospheres, fusiform nanoparticles and columnar nanoparticles, and the chemical valence is of the coexistence of +4, +5 and +6. In addition, the sample prepared by the method has relatively strong near-infrared ray absorbing capacity.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic oxide materials, and relates to a method for preparing tungsten-based nanoparticles with adjustable appearance and size. Background technique [0002] Mixed valence tungsten-based nanoparticles, mainly reduced tungsten oxide (WO 3-x , x=0~0.375). Since tungsten ions in such compounds are in a mixed valence state (W 6+ , W 5+ and W 4+ ), so it has special electronic structure and optoelectronic properties, which also make this kind of compounds have a wide range of applications, such as field emission properties, electronic and ionic semiconductors, color-changing components, chemical, biological sensors, heat protection and bioluminescence heat treatment etc. Among the above compounds, W 18 o 49 It is the only tungsten oxide compound with low oxygen value that has been reported to exist in a pure state. According to literature reports, there are many methods that can be used to synt...

Claims

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Application Information

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IPC IPC(8): C01G41/02B82Y30/00
Inventor 刘绍琴果崇申颜美张守浩
Owner HARBIN INST OF TECH
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