CN101798117B - Method for preparing highly ordered tungsten trioxide nano-rod - Google Patents
Method for preparing highly ordered tungsten trioxide nano-rod Download PDFInfo
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- CN101798117B CN101798117B CN2010101328674A CN201010132867A CN101798117B CN 101798117 B CN101798117 B CN 101798117B CN 2010101328674 A CN2010101328674 A CN 2010101328674A CN 201010132867 A CN201010132867 A CN 201010132867A CN 101798117 B CN101798117 B CN 101798117B
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Abstract
The invention discloses a method for preparing a highly ordered tungsten trioxide nano-rod. The method comprises the following steps: mixing 0 to 50ml of deionized water and 0 to 50ml of 36.5-38 percent commercial concentrated hydrochloric acid to obtain mixed solution with total volume of 50ml; adding 0.2 to 4g of tungsten hexachloride into the mixed solution after the mixed solution is stirred for 5 minutes at normal temperature; moving the mixed solution to a 100ml high-temperature reaction kettle after the mixed solution is continuously stirred for 5 minutes; placing the conductive surface of clean conductive glass upwards in the high-temperature reaction kettle; placing the high-temperature reaction kettle in a thermostatic drying oven to perform a hydro-thermal reaction for 4 to 20 hours at constant temperature between 100 and 180 DEG C, naturally cooling the high-temperature reaction kettle; and taking the conductive glass out of the high-temperature reaction kettle, and drying the conductive glass in the drying oven after the conductive glass is washed by the deionized water. The method has the advantages of simple process and good repeatability, and the prepared tungsten trioxide nano-rod has the diameter between 80 and 100 nanometers and the length between 3 and 6 microns.
Description
Technical field
The present invention relates to a kind of preparation method of highly ordered tungsten trioxide nano-rod.
Background technology
Conductor photocatalysis and the current problem that much relates to the environment and the energy are closely bound up.Conductor photocatalysis is except being used in photochemical catalysis water providing cleaning and the Hydrogen Energy capable of circulation, and some semiconductor materials utilize sun power to degrade the organic and inorganics of pollution in the empty G﹠W.Titanium dioxide becomes current widely used high-efficiency photocatalysis material because of its stable performance and low price.Yet because the wide band gap of titanium dioxide, in fact titanium dioxide has only utilized the sub-fraction UV-light of the whole spectrum 3-5% of sun power as photochemical catalysis the time.Therefore, development of new efficiently photocatalyst material become when previous urgent and the challenge problem.With titanium dioxide contrast, tungstic oxide has littler bandgap structure, so tungstic oxide occupy a lot of advantages aspect the photochemical catalysis utilizing, and for example, can utilize most of solar spectrum, and photochemical properties is stable.
Nanorod structure has the electric transmission of raising speed, reduces electron recombination and improves the advantage of scattering of light.At present synthetic high-purity tungsten trioxide nano-rod, especially apposition growth is quite difficult on conductive glass.And, synthetic high-purity tungsten trioxide nano-rod, the industrialization aspect generally adopts chemical vapour deposition, and there is the cost height in this technology, and is unfavorable for that big area synthesizes the tungsten trioxide nano-rod material.
Summary of the invention
The object of the present invention is to provide a kind of technology simple, the preparation method of high orientation growth tungsten trioxide nano-rod on conductive glass.
Concrete steps are:
With 0-50 ml deionized water and 0-50 milliliter weight percent is the commercially available concentrated hydrochloric acid mixing of 36.5-38%, reach cumulative volume and be 50 milliliters mixed solution, after stirring 5 minutes at normal temperatures, add the tungsten hexachloride of 0.2-4 gram then, continue to stir after 5 minutes, forward in 100 milliliters the pyroreaction still; To clean clean conductive glass conducting surface then upwards is placed in the pyroreaction still; The pyroreaction still is placed in the thermostatic drying chamber, after under the 100-180 ℃ of constant temperature hydro-thermal reaction 4-20 hour, naturally cooling; At last conductive glass is taken out from the pyroreaction still, oven dry can obtain the tungsten trioxide nano-rod array that high orientation is grown on conductive glass in the loft drier with being placed on behind the deionized water rinsing.
The present invention synthesizes the tungsten trioxide nano-rod of high orientation growth on conductive glass by a kind of easy hydrothermal synthesis method, and this nanometer rod diameter is the 80-100 nanometer, and length is the 3-6 micron.This operational path is compared over generally the chemical gaseous phase depositing process that adopts, have simple, the advantage of good reproducibility.
Description of drawings
The XRD figure of the tungsten trioxide nano-rod that Fig. 1 makes for the embodiment of the invention 2.
The lateral SEM figure of the tungsten trioxide nano-rod that Fig. 2 makes for the embodiment of the invention 2.
Embodiment
Embodiment one:
With 25 ml deionized water and 25 milliliters of weight percents is that 36.5% commercially available concentrated hydrochloric acid mixes, and reaches cumulative volume and be 50 milliliters mixed solution; After stirring 5 minutes at normal temperatures, add the tungsten hexachloride of 0.2 gram then; Continue to stir after 5 minutes, forward 100 milliliters pyroreaction still interior (tetrafluoroethylene liner) to; The pyroreaction still is placed in the thermostatic drying chamber hydro-thermal reaction after 10 hours under 120 ℃ of constant temperature, naturally cooling; Conductive glass is taken out from the pyroreaction still, dried with being placed in the loft drier behind the deionized water rinsing, the nanometer rod diameter that is obtained is the 80-90 nanometer, and length is the 3-4 micron.
Embodiment two:
With 25 ml deionized water and 25 milliliters of weight percents is that 38% commercially available concentrated hydrochloric acid mixes, and reaches cumulative volume and be 50 milliliters mixed solution; After stirring 5 minutes at normal temperatures, add the tungsten hexachloride of 0.39 gram then; Continue to stir after 5 minutes, forward 100 milliliters pyroreaction still interior (tetrafluoroethylene liner) to; The pyroreaction still is placed in the thermostatic drying chamber hydro-thermal reaction after 20 hours under 150 ℃ of constant temperature, naturally cooling; Conductive glass is taken out from the pyroreaction still, dried with being placed in the loft drier behind the deionized water rinsing, the nanometer rod diameter that is obtained is the 90-100 nanometer, and length is the 5-6 micron.The XRD figure of the tungsten trioxide nano-rod that makes is seen Fig. 1, and the lateral SEM figure of the tungsten trioxide nano-rod that makes sees Fig. 2.
Claims (1)
1. the preparation method of a tungsten trioxide nano-rod is characterized in that concrete steps are:
With 25 ml deionized water and 25 milliliters of commercially available concentrated hydrochloric acid mixing that weight percent is 36.5-38%, reach cumulative volume and be 50 milliliters mixed solution, stir 5 minutes at normal temperatures after, add the tungsten hexachloride of 0.2-4 gram then, continue to stir after 5 minutes, forward in 100 milliliters the pyroreaction still; To clean clean conductive glass conducting surface then upwards is placed in the pyroreaction still; The pyroreaction still is placed in the thermostatic drying chamber, after under the 100-180 ℃ of constant temperature hydro-thermal reaction 4-20 hour, naturally cooling; At last conductive glass is taken out from the pyroreaction still, oven dry can obtain tungsten trioxide nano-rod in the loft drier with being placed on behind the deionized water rinsing, and this nanometer rod diameter is the 80-100 nanometer, and length is the 3-6 micron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2010101328674A CN101798117B (en) | 2010-03-24 | 2010-03-24 | Method for preparing highly ordered tungsten trioxide nano-rod |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101328674A CN101798117B (en) | 2010-03-24 | 2010-03-24 | Method for preparing highly ordered tungsten trioxide nano-rod |
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| CN101798117A CN101798117A (en) | 2010-08-11 |
| CN101798117B true CN101798117B (en) | 2011-12-07 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102012386A (en) * | 2010-10-24 | 2011-04-13 | 天津大学 | Preparation method of nitric oxide gas sensor element based on pseudodirected tungsten trioxide nano tape |
| CN103395842B (en) * | 2013-07-30 | 2015-06-17 | 浙江大学 | Tungsten trioxide nanometer array electrochromic film and preparation method thereof |
| CN104724758B (en) * | 2015-03-06 | 2017-07-07 | 华北电力大学 | A kind of WO3The preparation method of nanoscale twins material |
| CN105668637A (en) * | 2016-01-05 | 2016-06-15 | 天津大学 | Preparation method of tungsten oxide nanorod bundle structure gas-sensitive material |
| CN106082344B (en) * | 2016-06-15 | 2017-10-31 | 中国科学技术大学 | A kind of preparation method of defect state tungstic acid for the aerobic coupling of photocatalysis |
| CN109576702B (en) * | 2019-01-04 | 2020-05-22 | 西安交通大学 | Gas-phase evaporation film forming method based on solvent thermal synthesis method and synthesized film thereof |
| CN110295342B (en) * | 2019-07-18 | 2021-03-16 | 大连民族大学 | Method for preparing tungsten oxide nano rod by plasma pretreatment |
| CN111675241A (en) * | 2020-06-10 | 2020-09-18 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of tungsten dioxide nanowire array/zinc stannate nanoribbon cathode material, product and application |
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| CN1286732C (en) * | 2004-11-11 | 2006-11-29 | 北京科技大学 | Preparation for nanometer anhydrous wolframic acid powder |
| CN100473611C (en) * | 2006-10-19 | 2009-04-01 | 大连理工大学 | Tungsten oxide material with nano band array structure and preparing method thereof |
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