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Method for preparing tungstic oxide nano-sheets

A technology of nanosheets and tungsten oxide, which is applied in nanostructure manufacturing, tungsten oxide/tungsten hydroxide, nanotechnology, etc., can solve few problems, achieve uniform particle size, low cost, and easy-to-operate process

Inactive Publication Date: 2010-08-18
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Regarding the preparation of low-dimensional nano-tungsten oxide, there have been many reports on the preparation of tungsten oxide with zero-dimensional and one-dimensional nanostructures, but there are few reports on the preparation of tungsten oxide with two-dimensional nanosheet structures.

Method used

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  • Method for preparing tungstic oxide nano-sheets
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  • Method for preparing tungstic oxide nano-sheets

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Slowly add 13g of tungsten powder into the mixed solution of 80ml of hydrogen peroxide and 8ml of deionized water, stir continuously in an ice-water bath until the tungsten powder is completely dissolved, and obtain a bright yellow peroxypolytungstic acid solution after filtration; The solution was refluxed at 55°C for 6 hours to form a yellow sol; age the yellow sol at room temperature to obtain a yellow solid as a precursor; take 0.8g of the precursor and add 54ml of deionized water to dissolve and prepare a solution, and then add 5mol / l dropwise Hydrochloric acid solution to adjust the pH value to about 2, then add 1 g of polyethylene glycol with a molecular weight of 2000 and mix evenly to obtain a precursor solution; move the obtained precursor solution into a reaction kettle, react at 180°C for 20 hours, and cool naturally to room temperature. The obtained product was vacuum filtered, washed three times with ethanol and distilled water, and then dried in an oven at...

Embodiment 2

[0031] Slowly add 13g of tungsten powder into the mixed solution of 80ml of hydrogen peroxide and 8ml of deionized water, stir continuously in an ice-water bath until the tungsten powder is completely dissolved, and obtain a bright yellow peroxypolytungstic acid solution after filtration; The solution was refluxed at 50°C for 10 hours to form a yellow sol; age the yellow sol at room temperature to obtain a yellow solid as a precursor; take 0.8g of the precursor and add 54ml of deionized water to dissolve and prepare a solution, and then add 1mol / l dropwise The hydrochloric acid solution adjusted the pH value to about 1.5, then added 1 g of polyethylene glycol with a molecular weight of 20,000 and mixed evenly to obtain a precursor solution; moved the obtained precursor solution into a reaction kettle, reacted at 150°C for 24 hours, and cooled naturally to room temperature. The obtained product was vacuum filtered, washed with ethanol and distilled water for 5 times, and then dr...

Embodiment 3

[0033] Slowly add 13g of tungsten powder into the mixed solution of 80ml of hydrogen peroxide and 8ml of deionized water, stir continuously in an ice-water bath until the tungsten powder is completely dissolved, and obtain a bright yellow peroxypolytungstic acid solution after filtration; The solution was refluxed at 60°C for 5 hours to form a yellow sol; age the yellow sol at room temperature to obtain a yellow solid as a precursor; take 0.8g of the precursor and add 54ml of deionized water to dissolve and prepare a solution, and then add 3mol / l dropwise Hydrochloric acid solution to adjust the pH value to about 1.7, then add 1 g of polyethylene glycol with a molecular weight of 5000 and mix evenly to obtain a precursor solution; move the obtained precursor solution into a reaction kettle, react at 160°C for 22 hours, and cool naturally to room temperature. The obtained product was vacuum filtered, washed with ethanol and distilled water 4 times, and dried in an oven at 100°C ...

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Abstract

The invention provides a method for preparing tungstic oxide nano-sheets, comprising a precursor solution preparation part and a hydro-thermal reaction part, specifically comprising the following steps: carrying out hydrogen peroxide oxidation reaction of metal tungsten powder at the condition of low temperature water bath, back-flowing the obtained peroxy-polytungstic acid solution for 5-15h at the temperature of 50-60 DEG C, dissolving with deionized water after aging at room temperature, adjusting the pH value with hydrochloric acid or nitric acid, mixing with polyethylene glycol to obtain the precursor solution; carrying out the reaction of the precursor solution for 12-24h at the temperature of 150-180 DEG, putting the solution in a drying oven for drying through vacuum leaching, alcohol and distilled water washing after naturally cooling till room temperature so as to obtain tungstic oxide nano-sheets; compared with the prior art, the method has low cost, simple technology, easy operation, high preparation efficiency, good repeatability and convenient industrialization; the tungstic oxide nano-sheets preparaed by the method have regular shape and uniform granularity, and can be widely applied to visible light catalysis, solar battery, intelligent window, gas sensor, and the like.

Description

technical field [0001] The invention relates to the technical field of metal oxide semiconductor preparation methods, in particular to a preparation method for obtaining tungsten oxide nanosheets by using a tungsten powder peroxidation method. Background technique [0002] Tungsten oxide is an important transition metal oxide semiconductor with excellent electrochromic, photochromic, and field emission properties, and has important application prospects in the fields of solar energy utilization, intelligent display, visible light catalysis, and chemical sensing. [0003] The properties of nanomaterials are closely related to their structure, morphology and particle size. Therefore, the research on the shape control of various nanostructures has become one of the hotspots in the field of nanomaterials. The preparation methods of nanomaterials can be roughly divided into high temperature gas phase method, mechanochemical method and wet chemical method. These preparation meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/02B82B3/00
Inventor 孙喜莲曹鸿涛方燕群
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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