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Method for synthesizing W18O49 nano material through microwave assistance

A nanomaterial and microwave-assisted technology, applied in nanotechnology, tungsten oxide/tungsten hydroxide, etc., can solve the problems of high sintering temperature, low product purity, long holding time, etc., to avoid grain growth and shorten the reaction time time, fast heating effect

Inactive Publication Date: 2019-04-19
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solid-phase synthesis method has higher sintering temperature, longer holding time, and lower product purity

Method used

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  • Method for synthesizing W18O49 nano material through microwave assistance
  • Method for synthesizing W18O49 nano material through microwave assistance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Take analytically pure (NH 4 ) 10 W 12 o 41 ·5H 2 O is added in absolute ethanol and is mixed with the solution A of 0.05mol / L, and seals up with plastic wrap in time to avoid pollution;

[0026] 2) Sodium oleate and n-propylamine were added to solution A, and magnetically stirred until the solution gradually changed from yellow to blue to obtain a mixed solution B with a concentration of sodium oleate of 0.05mol / L and a concentration of n-propylamine of 0.05mol / L;

[0027] 3) Put the mixed solution B into the microwave hydrothermal reactor at a filling ratio of 40%, set the heating power to 300W with the MDS-8 microwave hydrothermal instrument, and raise the temperature in the reactor from The room temperature was raised to 150°C, and the reaction was carried out for 60 minutes;

[0028] 4) Naturally cool to room temperature after the reaction, and centrifuge and wash the final reactant with deionized water and absolute ethanol, and dry the centrifuged and wash...

Embodiment 2

[0032] 1) Take analytically pure (NH 4 ) 10 W 12 o 41 ·5H 2 O is added in isopropanol and is mixed with solution A of 0.01mol / L, and seals up with plastic wrap in time to avoid pollution;

[0033] 2) Sodium oleate and n-propylamine were added to solution A, and magnetically stirred until the solution gradually changed from yellow to blue to obtain a mixed solution B with a concentration of sodium oleate of 0.03mol / L and a concentration of n-propylamine of 0.03mol / L;

[0034] 3) Put the mixed solution B into the microwave hydrothermal reactor at a filling ratio of 30%, set the heating power to 400W with the MDS-8 microwave hydrothermal instrument, and raise the temperature in the reactor from The room temperature was raised to 160°C, and the reaction was carried out for 80 minutes;

[0035] 4) Cool down to room temperature naturally after the reaction, and centrifuge and wash the final reactant with deionized water and absolute ethanol, and dry the centrifuged and washed m...

Embodiment 3

[0038] 1) Take analytically pure (NH 4 ) 10 W 12 o 41 ·5H 2 O is added in n-butanol and is mixed with the solution A of 0.2mol / L, and seal up with fresh-keeping film in time to avoid pollution;

[0039] 2) adding sodium oleate and n-propylamine into solution A, and magnetically stirring until the solution gradually changes from yellow to blue to obtain a mixed solution B with a concentration of sodium oleate of 0.04mol / L and a concentration of n-propylamine of 0.02mol / L;

[0040] 3) Put the mixed solution B into the microwave hydrothermal reactor at a filling ratio of 40%, set the heating power to 400W with the MDS-8 microwave hydrothermal instrument, and raise the temperature in the reactor from The room temperature was raised to 140°C, and the reaction was carried out for 70 minutes;

[0041] 4) Naturally cool to room temperature after the reaction, and centrifuge and wash the final reactant with deionized water and absolute ethanol, and dry the centrifuged and washed m...

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Abstract

The invention relates to a method for synthesizing a W18O49 nano material through microwave assistance. The method comprises the steps that analytical pure (NH4)10W12O41.5H2O is added to alcohol, anda solution A is prepared; sodium oleate and n-propylamine are added to the solution A to obtain a solution B; the mixed solution B is placed in a microwave hydrothermal reaction kettle, and a microwave hydrothermal instrument is adopted for conducting a hydrothermal reaction; after the reaction is completed, the mixture is naturally cooled to the room temperature, a final reactant is centrifuged and washed through deionized water and absolute ethyl alcohol separately, and the centrifuged and washed substance is dried to obtain the pure-phase W18O49 nano material. According to the method, by adopting a microwave technology, the microwave is used as a heating tool, and compared with a traditional preparation method, stirring in the molecular level can be achieved, and the method has the advantages that the heating speed is high, heating is even, and the temperature gradient or the hysteresis effect exists. The defect is overcome that heating of a hydrothermal container is uneven, the reaction time is shortened, and the working efficiency is improved.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, in particular to a microwave-assisted synthesis of W 18 o 49 methods for nanomaterials. Background technique [0002] Tungsten oxide has a variety of existing forms and crystal structures, including the stoichiometric ratio of WO 3 and non-stoichiometric W 18 o 49 (WO 2.72 ), W 5 o 14 (WO 2.8 ), W 24 o 68 (WO 2.83 ) and W 20 o 58 (WO 2.9 ), its general chemical formula is WO 3-x (x=0~1). non-stoichiometric WO 3-x The color is yellow-green depending on the oxygen content. It is an important multifunctional n-type wide bandgap (2.5-3.6eV) semiconductor. It exhibits many unique properties and has potential applications. For example, due to tungsten oxide Due to its electrochromic, photochromic and aerochromic properties, it can be widely used in the fields of flat panel displays, smart windows and various sensors. [0003] where W 18 o 49 Has the largest number o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/02B82Y40/00
CPCB82Y40/00C01G41/02C01P2002/72C01P2004/03
Inventor 黄剑锋海国娟冯亮亮曹丽云介燕妮杨佳付常乐吴建鹏
Owner SHAANXI UNIV OF SCI & TECH
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