CN102898038A - Method for preparing vertically aligned tungsten oxide nano structural electrochromic film - Google Patents
Method for preparing vertically aligned tungsten oxide nano structural electrochromic film Download PDFInfo
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Abstract
The invention relates to a method for preparing a vertically aligned tungsten oxide nano structural electrochromic film. The method comprises the following steps of: 1) dissolving tungstic acid in a mixed solution of hydrogen peroxide and water, heating until tungstic acid is fully dissolved, and cooling to obtain transparent sol; 2) coating the obtained transparent sol on the surface of fluorine-doped tin oxide (FTO) conducting glass which is subjected to ultrasonic washing in a spinning way, and calcining to obtain the FTO conducting glass with a tungsten oxide crystal seed layer; and 3) preparing a reaction solution containing the transparent sol, hydrochloric acid, urea and solvent, immersing the obtained FTO conducting glass with the tungsten oxide crystal seed layer in a hydrothermal kettle in which the reaction solution is filled, preserving heat at the temperature of between 150 and 180 DEG C for 6 to 12 hours, naturally cooling to room temperature, washing and drying to obtain the vertically aligned tungsten oxide nano structural electrochromic film. A preparation process is simple and low in cost; by the method, the electrochromic properties such as color change speed, coloration efficiency, cycling stability and the like of the film are effectively improved; and the method has the industrial application prospect in the aspect of preparing the film on the surface of the glass.
Description
Technical field
The invention belongs to the preparation field of electrochomeric films, particularly a kind of preparation method of tungsten oxide nanometer structure electrochomeric films of vertical orientation arrangement.
Background technology
Electrochromism refers to that material produces and stablizes reversible change phenomenon under electric field action.Injection and the extraction of electronics and ion occuring under electrochemical action when material, its valence state and chemical composition are changed, thereby make the reflection and transmission performance change of material, then shows as the reversible change of color and transparency on appearance property.Electrochromic material is because of at display device, smart window, have broad application prospects and be subject to people's attention without dizzy reflective mirror, the military aspect such as false proof.Since the electrochromic effect of S.K.Deb reported first non-crystalline state oxidation tungsten film in 1969, the electrochomeric films material becomes one of focus of investigation of materials with its special performance.Wherein inorganic, metal oxide research is the most abundant, especially Tungsten oxide 99.999.
In recent years, the developmental research person along with nanotechnology wishes to improve by the electrochomeric films of constructing nanostructure its electrochromic property.S.H.Lee etc. have reported the tungsten oxide film of a kind of nano particle and nano bar-shape at Advanced Materials Vol.18 (2006) pp.763-766.J.M.Wang etc. have reported the tungsten oxide film that a kind of nanometer rod is piled up at Journal ofPhysical Chemistry C Vol.113 (2009) pp.9655-9658.Z.H.Jiao etc. have been reported to a kind of tabular tungsten oxide nanometer structural membrane of hydrothermal method preparation at Journal of Physics D:Applied Physics Vol.43 (2010) pp.285501.Although the electrochromic property of the tungsten oxide film of these nanostructures has had raising to a great extent, also there are in actual applications a lot of problems, as: (1) cycle index is few, is difficult to reach application request; (2) painted longer with bleaching time, can't be used for fast response device; (3) modulation amplitude to visible light transmissivity is lower, still can not satisfy the needs of practical application.
Trace it to its cause, mainly contain following two aspects: at first, these nanostructures all are the surfaces that is attached at random substrate of glass, therefore, bonding force between the Tungsten oxide 99.999 of these nanostructures and the electrically conducting transparent substrate is poor, especially the tungsten oxide nanometer structure on film top, this will inevitably affect contacting between ion and tungsten oxide nanometer structure and the substrate in the ionogen, thereby affects its electrochromism response speed; Secondly, exactly because these nanostructures of adhering at random can not be fully utilized at the suprabasil tightly packed active surface of these nanostructures that caused of electrically conducting transparent, thereby affect its coloration efficiency.Therefore, the tungsten oxide film of the nanostructure that direct growth one deck vertical orientation is arranged in the conductive glass substrate is expected to break through the technical bottleneck of existing electrochomeric films material, solve the above-mentioned problem of mentioning, for the extensive industrialization that realizes electrochomeric glass is laid a solid foundation.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of tungsten oxide nanometer structure electrochomeric films of vertical orientation arrangement, the method preparation technology is simple, cost is low, has the industry application possibility in the glass surface masking, the structure of obtained film is unique, larger electrochemical reaction active surface can be provided, effectively improve the electrochromic properties such as variable color speed, coloration efficiency and cyclical stability.
The preparation method of the tungsten oxide nanometer structure electrochomeric films that a kind of vertical orientation of the present invention is arranged comprises:
(1) wolframic acid is dissolved in the mixing solutions of hydrogen peroxide and water, is heated to 80～95 ℃, dissolve rear cooling fully until wolframic acid and obtain vitreosol;
(2) vitreosol obtained above is spun on through the FTO of supersound washing conductive glass surface, obtains the FTO conductive glass with the Tungsten oxide 99.999 crystal seed layer after the calcining;
(3) preparation contains the reaction soln of above-mentioned vitreosol, hydrochloric acid, urea and solvent, then the FTO conductive glass with the Tungsten oxide 99.999 crystal seed layer obtained above is immersed and fill in the water heating kettle of reaction soln, in 150～180 ℃ of insulations 6～12 hours, naturally cool at last room temperature, clean, oven dry namely obtains tungsten oxide nanometer structure electrochomeric films.
The volumetric molar concentration of the wolframic acid in the described step (1) is 0.05～0.1mol/L, and the volume ratio of hydrogen peroxide and water is 3:7.
Through deionized water, acetone and ethanol supersound washing, the supersound washing time is 20～30 minutes for successively in supersound washing in the described step (2).
Calcining temperature in the described step (2) is 350～500 ℃, and calcination time is 0.5～2 hour.
The amount of the reaction soln in the described step (3) accounts for 80% of water heating kettle volume, and wherein the volume ratio of hydrochloric acid, vitreosol and solvent is 1:3:12.
Solvent in the reaction soln in the described step (3) is that water, acetonitrile or volume ratio are water and the acetonitrile mixed solution of 1:1.
The concentration that adds hydrochloric acid in the reaction soln in the described step (3) is 3～6mol/L, and the mol ratio of wolframic acid is 3:50～9:25 in urea and the vitreosol.
Tungsten oxide nanometer structure in the described step (3) is nanometer rod, nano bar-shape flower or nano wire.
Cleaning in the described step (3) is that water and ethanol clean successively.
Addition by urea in the conditioned reaction solution and as the volume ratio of water and the acetonitrile of solvent, can change the pattern of nanostructure Tungsten oxide 99.999, thereby the vertical orientation of Tungsten oxide 99.999 on the FTO conductive glass of realizing nanostructure arranged, the structure of this uniqueness can improve the electrochromic properties such as variable color speed, coloration efficiency and cyclical stability effectively, is a kind of desirable electrochromism structure.
Beneficial effect
(1) preparation method of the present invention is simple, and cost is low, has the industry application possibility in the glass surface masking;
(2) nanostructure tungsten oxide film of the present invention is the surface that is grown directly upon the FTO conductive glass by hydrothermal method, and Tungsten oxide 99.999 and substrate have preferably bonding force, are conducive to electronic conduction, has also improved the electrochemical stability of film simultaneously;
(3) the present invention has realized that the tungsten oxide nanometer structure is in the suprabasil vertical orientation arrangement of FTO conductive glass, the structure of this uniqueness had both shortened the dispersion path of ion in film, its active surface can be fully utilized, thereby can effectively improve variable color speed, the coloration efficiency of film.
Description of drawings
Fig. 1 is the X-ray diffractogram of the tungsten oxide nanometer structure electrochomeric films of embodiment 1 preparation;
Fig. 2 is the stereoscan photograph of the tungsten oxide nanometer structure electrochomeric films of embodiment 1 preparation;
Fig. 3 is the tungsten oxide nanometer structure electrochomeric films light transmission rate curve under painted and bleached state respectively of embodiment 1 preparation;
Fig. 4 is electrochromism curve time response of the tungsten oxide nanometer structure electrochomeric films of embodiment 1 preparation;
Fig. 5 is the optical density (OD) difference-electric density curve of the tungsten oxide nanometer structure electrochomeric films of embodiment 1 preparation;
Fig. 6 is the stereoscan photograph of the tungsten oxide nanometer structure electrochomeric films of embodiment 2 preparations;
Fig. 7 is the stereoscan photograph of the tungsten oxide nanometer structure electrochomeric films of embodiment 3 preparations;
Fig. 8 is the stereoscan photograph of the tungsten oxide nanometer structure electrochomeric films of embodiment 1 preparation.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
The FTO conductive glass is immersed in deionized water, acetone and the ethanol separately supersound washing 20 minutes, dry for standby successively.Take by weighing in the mixing solutions that the 5g wolframic acid is dissolved in 60mL hydrogen peroxide and 140mL water, be heated to 95 ℃, dissolve rear cooling fully until wolframic acid and obtain vitreosol; Then vitreosol is spun on the FTO conductive glass surface of ultrasonic cleaning, obtained the Tungsten oxide 99.999 crystal seed layer in 0.5 hour 500 ℃ of lower calcinings.Preparation contains the reaction soln of 10.5mL vitreosol, 3.5mL hydrochloric acid (3mol/L), 1.2mmol urea, 42mL water, then the FTO conductive glass with the Tungsten oxide 99.999 crystal seed layer obtained above is immersed and fill in the water heating kettle of reaction soln, in 180 ℃ of insulations 12 hours, naturally cool at last room temperature, take out the FTO conductive glass, water and ethanol clean successively post-drying and get final product.Fig. 1 is the X-ray diffractogram of obtained film, and the reference standard X ray diffracting spectrum can be found out: this film is the Tungsten oxide 99.999 of six side's phases, and is corresponding with standard card JCPDS 85-2460.Fig. 2 is the stereoscan photograph of obtained tungsten oxide film, can find out that this film is comprised of rectangular nanometer rod.
In order to understand the electrochromic property of the prepared tungsten oxide nanometer structural membrane of above-described embodiment, the light transmission rate that we measure the tungsten oxide nanometer structural membrane that makes with three-electrode system combined with electrochemical workstation and solid ultraviolet-visible pectrophotometer changes and the electrochromism response speed, and calculates coloration efficiency.Wherein three-electrode system is: with the tungsten oxide nanometer structural membrane electrode of preparation as working electrode, take Ag/AgCl as reference electrode, take platinum filament as to electrode, take the polycarbonate solution of the lithium perchlorate of 1mol/L as ionogen.The result shows: when apply-when the side of 2V and 2V presses, the tungsten oxide nanometer structural membrane mazarine and transparent between reversible change; As shown in Figure 3, the transmittance of this film has obvious variation at 400～900nm wave band, has reached 62% at λ=632nm place; The electrochromic effect time of tungsten oxide nanometer structural membrane and coloration efficiency can be calculated respectively by Fig. 4 and Fig. 5, and calculation result is as shown in table 1.By above result as can be known, embodiment 1 prepared tungsten oxide nanometer structural membrane has good electrochromic property.
The FTO conductive glass is immersed in deionized water, acetone and the ethanol separately supersound washing 20 minutes, dry for standby successively.Take by weighing in the mixing solutions that the 2.5g wolframic acid is dissolved in 60mL hydrogen peroxide and 140mL water, be heated to 80 ℃, dissolve rear cooling fully until wolframic acid and obtain vitreosol; Then vitreosol is spun on the FTO conductive glass surface of ultrasonic cleaning, obtained the Tungsten oxide 99.999 crystal seed layer in 2 hours 350 ℃ of lower calcinings.Preparation contains the reaction soln of 10.5mL vitreosol, 3.5mL hydrochloric acid (3mol/L), 3.6mmol urea, 42mL water, then the FTO conductive glass with the Tungsten oxide 99.999 crystal seed layer obtained above is immersed and fill in the water heating kettle of reaction soln, in 180 ℃ of insulations 12 hours, naturally cool at last room temperature, take out the FTO conductive glass, water and ethanol clean successively post-drying and get final product.Fig. 6 is the stereoscan photograph of prepared tungsten oxide film, can find out that this film surface appearance is the flower-like structure that nanometer rod forms.X-ray diffraction analysis shows, this film is comprised of the Tungsten oxide 99.999 of six side's phases.The bar-shaped colored film of tungsten oxide nanometer of preparation is carried out the electrochromic property test as working electrode, and the result is as shown in table 1, corresponding and embodiment 2 hurdles, and the electrochromic property of the bar-shaped colored film of this tungsten oxide nanometer is good not as embodiment 1 gained film.
The FTO conductive glass is immersed in deionized water, acetone and the ethanol separately supersound washing 30 minutes, dry for standby successively.Take by weighing in the mixing solutions that the 5g wolframic acid is dissolved in 60mL hydrogen peroxide and 140mL water, be heated to 95 ℃, dissolve rear cooling fully until wolframic acid and obtain vitreosol; Then vitreosol is spun on the FTO conductive glass surface of ultrasonic cleaning, obtained the Tungsten oxide 99.999 crystal seed layer in 0.5 hour 400 ℃ of lower calcinings.Preparation contains the reaction soln of 10.5mL vitreosol, 3.5mL hydrochloric acid (6mol/L), 1.2mmol urea, 21mL water, 21mL acetonitrile, then the FTO conductive glass with the Tungsten oxide 99.999 crystal seed layer obtained above is immersed and fill in the water heating kettle of reaction soln, in 180 ℃ of insulations 6 hours, naturally cool at last room temperature, take out the FTO conductive glass, water and ethanol clean successively post-drying and get final product.Fig. 7 is the stereoscan photograph of obtained tungsten oxide film, can find out that this film is comprised of columniform nanometer rod, and the diameter of nanometer rod is 80～100nm.X-ray diffraction analysis shows, this film is comprised of the Tungsten oxide 99.999 of six side's phases.The bar-shaped film of cylindrical nanometer of preparation is carried out the electrochromic property test as working electrode, the result is as shown in table 1, correspondence and embodiment 3 hurdles, the embodiment 1 gained film of comparing, the electrochromic property of the bar-shaped tungsten oxide film of this cylindrical nanometer is more superior.
Embodiment 4
The FTO conductive glass is immersed in deionized water, acetone and the ethanol separately supersound washing 30 minutes, dry for standby successively.Take by weighing in the mixing solutions that the 5g wolframic acid is dissolved in 60mL hydrogen peroxide and 140mL water, be heated to 95 ℃, dissolve rear cooling fully until wolframic acid and obtain vitreosol; Then vitreosol is spun on the FTO conductive glass surface of ultrasonic cleaning, obtained the Tungsten oxide 99.999 crystal seed layer in 0.5 hour 400 ℃ of lower calcinings.Preparation contains the reaction soln of 10.5mL vitreosol, 3.5mL hydrochloric acid (6mol/L), 1.2mmol urea, 42mL acetonitrile, then the FTO conductive glass with the Tungsten oxide 99.999 crystal seed layer obtained above is immersed and fill in the water heating kettle of reaction soln, in 150 ℃ of insulations 12 hours, naturally cool at last room temperature, take out the FTO conductive glass, water and ethanol clean successively post-drying and get final product.Fig. 8 is the stereoscan photograph of obtained tungsten oxide film, can find out that this film is comprised of tungsten oxide nano.The diameter of nano wire is 20～30nm.X-ray diffraction analysis shows, this film is comprised of the Tungsten oxide 99.999 of six side's phases.The tungsten oxide nano film of preparation is carried out the electrochromic property test as working electrode, and the result is as shown in table 1, corresponding and embodiment 4 hurdles.The electrochromic property of this tungsten oxide nano film is good not as embodiment 1, embodiment 2 and embodiment 3 gained films as can be seen from Table 1.
Table 1
Claims (9)
1. the preparation method of the tungsten oxide nanometer structure electrochomeric films arranged of a vertical orientation comprises:
(1) wolframic acid is dissolved in the mixing solutions of hydrogen peroxide and water, is heated to 80～95 ℃, dissolve rear cooling fully until wolframic acid and obtain vitreosol;
(2) vitreosol obtained above is spun on through the FTO of supersound washing conductive glass surface, obtains the FTO conductive glass with the Tungsten oxide 99.999 crystal seed layer after the calcining;
(3) preparation contains the reaction soln of above-mentioned vitreosol, hydrochloric acid, urea and solvent, then the FTO conductive glass with the Tungsten oxide 99.999 crystal seed layer obtained above is immersed and fill in the water heating kettle of reaction soln, in 150～180 ℃ of insulations 6～12 hours, naturally cool at last room temperature, clean, oven dry namely obtains tungsten oxide nanometer structure electrochomeric films.
2. the preparation method of the tungsten oxide nanometer structure electrochomeric films arranged of a kind of vertical orientation according to claim 1, it is characterized in that: the volumetric molar concentration of the wolframic acid in the described step (1) is 0.05～0.1mol/L, and the volume ratio of hydrogen peroxide and water is 3:7.
3. the preparation method of the tungsten oxide nanometer structure electrochomeric films arranged of a kind of vertical orientation according to claim 1, it is characterized in that: through deionized water, acetone and ethanol supersound washing, the supersound washing time is 20～30 minutes to the supersound washing in the described step (2) for successively.
4. the preparation method of the tungsten oxide nanometer structure electrochomeric films arranged of a kind of vertical orientation according to claim 1, it is characterized in that: the calcining temperature in the described step (2) is 350～500 ℃, calcination time is 0.5～2 hour.
5. the preparation method of the tungsten oxide nanometer structure electrochomeric films arranged of a kind of vertical orientation according to claim 1, it is characterized in that: the amount of the reaction soln in the described step (3) accounts for 80% of water heating kettle volume, and wherein the volume ratio of hydrochloric acid, vitreosol and solvent is 1:3:12.
6. the preparation method of the tungsten oxide nanometer structure electrochomeric films arranged of a kind of vertical orientation according to claim 1, it is characterized in that: the solvent in the reaction soln in the described step (3) is that water, acetonitrile or volume ratio are water and the acetonitrile mixed solution of 1:1.
7. the preparation method of the tungsten oxide nanometer structure electrochomeric films arranged of a kind of vertical orientation according to claim 1, it is characterized in that: the concentration that adds hydrochloric acid in the reaction soln in the described step (3) is 3～6mol/L, and the mol ratio of wolframic acid is 3:50～9:25 in urea and the vitreosol.
8. the preparation method of the tungsten oxide nanometer structure electrochomeric films arranged of a kind of vertical orientation according to claim 1, it is characterized in that: the tungsten oxide nanometer structure in the described step (3) is nanometer rod, nano bar-shape flower or nano wire.
9. the preparation method of the tungsten oxide nanometer structure electrochomeric films arranged of a kind of vertical orientation according to claim 1, it is characterized in that: the cleaning in the described step (3) is that water and ethanol clean successively.
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