CN101767826B - Preparation method of hexagon snow shaped WO3 nanometer disc - Google Patents
Preparation method of hexagon snow shaped WO3 nanometer disc Download PDFInfo
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- CN101767826B CN101767826B CN2009102188692A CN200910218869A CN101767826B CN 101767826 B CN101767826 B CN 101767826B CN 2009102188692 A CN2009102188692 A CN 2009102188692A CN 200910218869 A CN200910218869 A CN 200910218869A CN 101767826 B CN101767826 B CN 101767826B
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Abstract
Disclosed is a preparation method of a hexagon snow shaped WO3 nanometer disc. Firstly, tungsten powder is added into hydrogen peroxide solution, after the reaction is finished, filtrate in a beaker is collected and labeled as solution A. Deionized water is added into the solution A and the solution A is diluted to obtain solution B; the solution B is poured into a microwave hydrothermal reactor, and then is put into a MDS-8 type temperature-pressure double control microwave hydrothermal reaction machine. The temperature control mode is selected for reaction, after the reaction is finished, the solution B is cooled to the room temperature naturally. The hydrothermal reactor is opened, after the product is centrifugated, supernatant is removed and precipitate is collected, then the product is rinsed a plurality of times by using deionized water and absolute ethanol or deionized water and isopropanol, at last the product is soaked in absolute ethanol, and is dried in an electrothermal blowing dry box, then the snow shaped WO3 nanometer disc is obtained. The reaction of the invention is finished by one step, the subsequent treatment is not needed, the preparation period is short, and the process equipment is simple, the cost is low, the repeatability is high, the reaction temperature is low, the energy consumption is low and the production cost is saved.
Description
Technical field
The present invention relates to a kind of WO
3The preparation method of nanometer plate is specifically related to a kind of hexagon snow shaped WO
3The preparation method of nanometer plate.
Background technology
As a kind of transition metal oxide semiconductor material, nanometer WO
3Crystal is owing to its various crystal habit, and interesting physicochemical property are widely studied at present.Particularly have electrochromism because of it, thermochromism, gas-discoloration and photocatalytic effect have been widely used in the various fields at present, as the smart window material, solar battery apparatus, air-sensitive detector and photocatalyst etc.
Up to now, under special growth conditions, successfully synthesized WO
3Nano belt, nano wire, nanometer ball, nano cubic, nanometer flower, nanoshell, the multiple special appearance of nanometer plate or the like, but up to the present, multilayer is piled up the hexagonal flakes WO that forms
3The preparation of nanometer plate yet there are no report.
So far, traditional nanometer WO
3The crystalline preparation method mainly contains chemical Vapor deposition process, physical vaporous deposition, magnetron sputtering method, sol-gel method etc.In the aforesaid method, most apparatus expensive, complex process, consumes resources or pattern are difficult to accurate control, and gained crystal effect is undesirable.And the emerging preparation method such as the hydro-thermal of domestic rise over past ten years, solvent-thermal methods etc. are given WO
3New road has been opened up in the preparation of nanocrystal, but it also has preparation cycle long, the shortcoming that repeatability is not high.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of not only preparation cost low, and hexagon snow shaped WO simple to operate, that reaction time is short
3The preparation method of nanometer plate.
For achieving the above object, the technical solution used in the present invention is:
1) at first adding analytically pure volume fraction in beaker is 30% superoxol, and beaker placed cooling bath, slowly, gradation ground adds analytical pure, granular size is 200 purpose tungsten powders, after treating that its reaction finishes, the filtered liquid of collecting in the beaker is designated as solution A, adds the 1g tungsten powder in wherein every 5ml superoxol;
2) then, in A solution, add the deionized water dilution, make W in the solution
6+Concentration be 0.005～1mol/L, obtain solution B;
3) above-mentioned B solution is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 40%～80%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 140 ℃～220 ℃, and the reaction times is controlled at 1min-120min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is through after centrifugal, remove supernatant liquor and collecting precipitation, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol for several times then respectively, be soaked in the dehydrated alcohol at last, in electric drying oven with forced convection,, promptly get the alabastrine hexagon WO of final product at 30 ℃-120 ℃ following dry 1h-8h
3Nanometer plate.
Because the present invention adopts microwave hydrothermal technology, one step of reaction finishes, and does not have follow-up processing, and preparation cycle is short, and processing unit is simple, and cost is low, and repeatability is high, and temperature of reaction is low, energy consumption is low, saves production cost, and prepares the flakes WO that is combined by multilayer nanometer plate of growing arranged side by side
3Nanocrystal, this crystal shape rule, good dispersity, the shape homogeneous, and size is consistent.
Description of drawings
Fig. 1 is the WO of example 1 preparation
3Nanometer plate X-ray diffraction (XRD) collection of illustrative plates;
Fig. 2 is the WO of example 1 preparation
3The scanning electron microscope of nanometer plate (SEM) photo;
Fig. 3 is the WO of example 2 preparations
3The scanning electron microscope of nanometer plate (SEM) photo;
Fig. 4 is the WO of example 2 preparations
3The scanning electron microscope of nanometer plate (SEM) photo.
Embodiment
Embodiment 1:1) at first, the analytically pure volume fraction of adding 20ml is 30% superoxol in beaker, and beaker placed cooling bath, slowly, gradation ground adds the 4g analytical pure, granular size is 200 purpose tungsten powders, after treating that its reaction finishes, the filtered liquid of collecting in the beaker is designated as solution A;
2) then, in A solution, add the deionized water dilution, make W in the solution
6+Concentration be 0.1mol/L, obtain solution B;
3) above-mentioned B solution is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 60%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 180 ℃, and the reaction times is controlled at 60min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is through after centrifugal, remove supernatant liquor and collecting precipitation, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol for several times then respectively, be soaked in the dehydrated alcohol at last, in electric drying oven with forced convection,, promptly get the alabastrine hexagon WO of final product at 40 ℃ of following dry 7h
3Nanometer plate.
The sample of gained with Japanese D/max2000PCX-x ray diffractometer x analytic sample of science, is found that product is the WO that belongs to rhombic system that JCPDS is numbered 87-1203
30.33H
2O crystal (Fig. 1).This sample is observed with the JSM-6390A type scanning electronic microscope (Fig. 2) that Japanese JEOL company produces, from the prepared as can be seen typical WO of photo
3Nanocrystallinely be piled into, have the hexagon snow shaped structure of rule for the multi-layer nano dish, the about 1600nm of hexagon catercorner length of its formation, thickness is about 700nm.
Embodiment 2:1) at first, the analytically pure volume fraction of adding 20ml is 30% superoxol in beaker, and beaker placed cooling bath, slowly, gradation ground adds the 4g analytical pure, granular size is 200 purpose tungsten powders, after treating that its reaction finishes, the filtered liquid of collecting in the beaker is designated as solution A;
2) then, in A solution, add the deionized water dilution, make W in the solution
6+Concentration be 0.1mol/L, obtain solution B;
3) above-mentioned B solution is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 60%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 140 ℃, and the reaction times is controlled at 120min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is through after centrifugal, remove supernatant liquor and collecting precipitation, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol for several times then respectively, be soaked in the dehydrated alcohol at last, in electric drying oven with forced convection,, promptly get the alabastrine hexagon WO of final product at 40 ℃ of following dry 7h
3Nanometer plate.
The gained sample is observed with the JSM-6390A type scanning electronic microscope (Fig. 3,4) that Japanese JEOL company produces, from the prepared as can be seen typical WO of photo
3Nanocrystalline hexagon snow shaped structure with rule, and can observe out its center radially forms the flakes structure with the multi-layer nano dish of normal direction both direction growth formation process.
Embodiment 3:1) at first, the analytically pure volume fraction of adding 20ml is 30% superoxol in beaker, and beaker placed cooling bath, slowly, gradation ground adds the 4g analytical pure, granular size is 200 purpose tungsten powders, after treating that its reaction finishes, the filtered liquid of collecting in the beaker is designated as solution A;
2) then, in A solution, add the deionized water dilution, make W in the solution
6+Concentration be 0.03mol/L, obtain solution B;
3) above-mentioned B solution is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 50%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 200 ℃, and the reaction times is controlled at 20min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is through after centrifugal, remove supernatant liquor and collecting precipitation, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol for several times then respectively, be soaked in the dehydrated alcohol at last, in electric drying oven with forced convection,, promptly get the alabastrine hexagon WO of final product at 70 ℃ of following dry 5h
3Nanometer plate.
Embodiment 4:1) at first, the analytically pure volume fraction of adding 20ml is 30% superoxol in beaker, and beaker placed cooling bath, slowly, gradation ground adds the 4g analytical pure, granular size is 200 purpose tungsten powders, after treating that its reaction finishes, the filtered liquid of collecting in the beaker is designated as solution A;
2) then, in A solution, add the deionized water dilution, make W in the solution
6+Concentration be 0.005mol/L, obtain solution B;
3) above-mentioned B solution is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 70%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 160 ℃, and the reaction times is controlled at 100min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is through after centrifugal, remove supernatant liquor and collecting precipitation, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol for several times then respectively, be soaked in the dehydrated alcohol at last, in electric drying oven with forced convection,, promptly get the alabastrine hexagon WO of final product at 100 ℃ of following dry 3h
3Nanometer plate.
Embodiment 5:1) at first, the analytically pure volume fraction of adding 20ml is 30% superoxol in beaker, and beaker placed cooling bath, slowly, gradation ground adds the 4g analytical pure, granular size is 200 purpose tungsten powders, after treating that its reaction finishes, the filtered liquid of collecting in the beaker is designated as solution A;
2) then, in A solution, add the deionized water dilution, make W in the solution
6+Concentration be 0.1,0.5mol/L, obtain solution B;
3) above-mentioned B solution is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 40%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 220 ℃, and the reaction times is controlled at 1min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is through after centrifugal, remove supernatant liquor and collecting precipitation, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol for several times then respectively, be soaked in the dehydrated alcohol at last, in electric drying oven with forced convection,, promptly get the alabastrine hexagon WO of final product at 30 ℃ of following dry 8h
3Nanometer plate.
Embodiment 6:1) at first, the analytically pure volume fraction of adding 20ml is 30% superoxol in beaker, and beaker placed cooling bath, slowly, gradation ground adds the 4g analytical pure, granular size is 200 purpose tungsten powders, after treating that its reaction finishes, the filtered liquid of collecting in the beaker is designated as solution A;
2) then, in A solution, add the deionized water dilution, make W in the solution
6+Concentration be 1mol/L, obtain solution B;
3) above-mentioned B solution is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 80%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 190 ℃, and the reaction times is controlled at 40min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is through after centrifugal, remove supernatant liquor and collecting precipitation, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol for several times then respectively, be soaked in the dehydrated alcohol at last, in electric drying oven with forced convection,, promptly get the alabastrine hexagon WO of final product at 120 ℃ of following dry 1h
3Nanometer plate.
Claims (1)
1. hexagon snow shaped WO
3The preparation method of nanometer plate is characterized in that:
1) at first adding analytically pure volume fraction in beaker is 30% superoxol, and beaker placed cooling bath, slowly, gradation ground adds analytical pure, granular size is 200 purpose tungsten powders, after treating that its reaction finishes, the filtered liquid of collecting in the beaker is designated as solution A, adds the 1g tungsten powder in wherein every 5ml superoxol;
2) then, in A solution, add the deionized water dilution, make W in the solution
6+Concentration be 0.005～1mol/L, obtain solution B;
3) above-mentioned B solution is poured in the microwave hydrothermal reaction kettle, compactedness is controlled at 40%～80%; Seal microwave hydrothermal reaction kettle then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 140 ℃～220 ℃, and the reaction times is controlled at 1min-120min, and reaction naturally cools to room temperature after finishing;
4) open hydrothermal reaction kettle, product is through after centrifugal, remove supernatant liquor and collecting precipitation, adopt deionized water and dehydrated alcohol or deionized water and washed with isopropyl alcohol for several times then respectively, be soaked in the dehydrated alcohol at last, in electric drying oven with forced convection,, promptly get the alabastrine hexagon WO of final product at 30 ℃-120 ℃ following dry 1h-8h
3Nanometer plate.
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|---|---|---|---|
| CN2009102188692A CN101767826B (en) | 2009-10-30 | 2009-10-30 | Preparation method of hexagon snow shaped WO3 nanometer disc |
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| CN101767826B true CN101767826B (en) | 2011-09-14 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010033005A2 (en) * | 2008-09-22 | 2010-03-25 | 한국과학기술원 | Single-crystalline metal nano-plate and method for fabricating same |
| CN103964509B (en) * | 2014-04-18 | 2015-09-30 | 陕西科技大学 | A kind of WO 30.5H 2the preparation method of the thread structural membrane of O nanometer |
| CN104934584B (en) | 2015-05-13 | 2017-04-05 | 陕西科技大学 | A kind of porous hollow shell WO3/WS2Nano material and preparation method thereof |
| CN106044858B (en) * | 2016-05-27 | 2017-11-07 | 南京理工大学 | A kind of tungsten trioxide nano band is self-assembled into the preparation method of micro-nano star |
| 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 |
| CN107055619B (en) * | 2017-03-27 | 2018-08-24 | 浙江大学 | A kind of multilevel hierarchy WO3And preparation method thereof |
| CN108859334A (en) * | 2018-06-08 | 2018-11-23 | 佛山市南海区佳妍内衣有限公司 | A kind of underwear with far-infrared functional |
| CN108855047A (en) * | 2018-08-29 | 2018-11-23 | 河南师范大学 | A kind of flower-shaped tungstic acid/graphene composite photocatalyst and preparation method thereof |
| CN109019693B (en) * | 2018-09-27 | 2020-11-17 | 青岛科技大学 | Monoclinic phase WO3Preparation method of nano cuboid and photocatalytic application thereof |
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