CN105018919A - Preparation method for nanometer titanium dioxide thin film of strap-strap hierarchical structure - Google Patents
Preparation method for nanometer titanium dioxide thin film of strap-strap hierarchical structure Download PDFInfo
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- CN105018919A CN105018919A CN201510396329.9A CN201510396329A CN105018919A CN 105018919 A CN105018919 A CN 105018919A CN 201510396329 A CN201510396329 A CN 201510396329A CN 105018919 A CN105018919 A CN 105018919A
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Abstract
The invention discloses a preparation method for a nanometer titanium dioxide thin film of a strap-strap hierarchical structure. The method mainly includes the steps that titanyl sulfate, glycine and nitric acid are mixed in deionized water and then dried and decomposed, and amorphous metal complex is obtained; the amorphous metal complex reacts with a hydrogen peroxide solution, and upper-layer clean liquid is taken as a precursor solution; and a metal titanium plate where acid pickling is performed is submerged in a sodium hydroxide solution, the nanometer strap thin film is submerged in the precursor solution to react for 3-12 h after acid pickling and heat treatment, samples where reaction ends are washed through deionized water, dried and subjected to heat treatment, and the nanometer titanium dioxide thin film of the strap-strap hierarchical structure is obtained. According to the method, an alkali heat nanometer strap array is directly placed into the precursor solution to have a reaction so that the nanometer titanium dioxide thin film of the strap-strap hierarchical structure can be obtained, and reproducibility is good. The strap-strap hierarchical structure is unique, the specific area is high, and the method can be applied in the fields of photocatalysis, photoelectric conversion, lithium ion battery cathodes, gas sensors and the like.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide nano-film, particularly relate to the preparation method of one " band-band " hierarchy nano-titanium dioxide film.
Background technology
TiO
2be a kind of very important multifunctional semiconductor material, in fields such as photoelectric conversion, photochemical catalysis, lithium ion battery negative, gas sensors, all there is potential application prospect.The performance of functional materials and its microstructure with become to be grouped into closely related.One dimension Nano structure can strengthen transferring charge; Two-dimensional nanostructure has thinner thickness, can shorten electric charge diffusion length therein.The beltlike nanostructures with one fixed width and long-width ratio to a certain extent in conjunction with the advantage of monodimension nanometer material and two-dimension nano materials, can become a kind of important function nano material.
Conventional TiO
2nano belt structural integrity, has smooth surface, easily causes the compound of current carrier, and its photocatalysis performance can be caused not ideal enough.
Summary of the invention
The object of this invention is to provide the preparation method of one " band-band " hierarchy nano-titanium dioxide film, the titanium dioxide nano-film specific surface area that the method obtains is large, and photocatalysis performance is good.
The method of preparation of the present invention " band-band " hierarchy nano-titanium dioxide film, its step is as follows:
1) with deionized water, titanyl sulfate and glycine are dissolved respectively, mix with nitric acid again, the amount ratio of nitric acid and glycine is 0.34mL/g, the amount ratio of titanyl sulfate and glycine is 0.5-1g/g, above-mentioned mixed solution loading crucible is heated to decomposition at 400 DEG C complete, obtains amorphous metal complex compound; Be the H of 30% by above-mentioned amorphous metal complex compound and mass concentration
2o
2solution mixes, and every gram of amorphous metal complex compound uses 20 ~ 800mL H
2o
2solution, reacts 72h, gets supernatant liquid as precursor liquid at room temperature to 80 DEG C;
2) by mass concentration be 50 ~ 55% hydrofluoric acid, mass concentration be 65 ~ 68% nitric acid and deionized water by volume 1:3:6 mix, obtain pickle solution;
3) configuring volumetric molar concentration is 5mol/L NaOH solution, by pickling metal titanium plate step 2) after the pickle solution pickling of gained, use deionized water ultrasonic cleaning clean again, put into above-mentioned NaOH solution, be placed in autoclave, solution is no more than 80% of reactor volume, in 180 DEG C of alkali thermal response 24 h, obtains sodium titanate nano belt; Sample is taken out to be placed in the hydrochloric acid soln of volumetric molar concentration 0.1 mol/L and carries out ion-exchange, obtain metatitanic acid nano belt; Again sample is calcined 1 h at 450 DEG C, obtain titanium dioxide nano-belts;
4) by the titanium dioxide nano-belts that step 3) is obtained, be immersed in the obtained precursor liquid of step 1), at 60 ~ 90 DEG C, react 3 ~ 12h, reacted sample deionized water rinsing, drying, at 400-600 DEG C of insulation 1-3 h, obtains " band-band " hierarchy nano-titanium dioxide film.
Beneficial effect of the present invention is: the present invention, by forming surface heterogeneous medium hierarchy, not only can significantly improve film specific surface area, is conducive to improving quantum yield simultaneously, and then promotes the photocatalysis performance of film.Film of the present invention can be applicable to the fields such as photochemical catalysis, opto-electronic conversion, lithium ion battery negative, gas sensor.
Accompanying drawing explanation
Fig. 1 is " band-band " hierarchy TiO prepared by embodiment 1
2the X ray diffracting spectrum of nano thin-film;
Fig. 2 is " band-band " hierarchy TiO prepared by embodiment 1
2the scanning electronic microscope high power photo of nano thin-film;
Fig. 3 is " band-band " hierarchy nano-TiO prepared by embodiment 1
2the scanning electronic microscope macrograph of film;
Fig. 4 is " band-band " hierarchy nano-TiO prepared by embodiment 2
2the electron scanning micrograph of film;
Fig. 5 is " band-band " hierarchy nano-TiO prepared by embodiment 3
2the electron scanning micrograph of film;
Fig. 6 is " band-band " hierarchy nano-TiO prepared by embodiment 4
2the electron scanning micrograph of film;
Fig. 7 is " band-band " hierarchy nano-TiO prepared by embodiment 5
2the electron scanning micrograph of film.
Embodiment
Set forth the present invention further below in conjunction with the drawings and specific embodiments, but the present invention is not only confined to following embodiment.
embodiment 1
1) 1.25g titanyl sulfate, 0.6mL nitric acid and 1.75g glycine are added in 10mL deionized water, again the crucible that above-mentioned solution is housed is positioned in retort furnace in 400 DEG C of heating, solution, after boiling, foaming, decomposing, obtains black amorphous metal complex compound; After being ground by amorphous metal complex compound, getting 0.5g, to add 50mL mass concentration be in the superoxol of 30%, and room temperature places 72 h, gets supernatant liquid and obtains precursor liquid;
2) by mass concentration be 55% hydrofluoric acid, mass concentration be 65% nitric acid and deionized water by volume 1:3:6 ratio mix, obtain pickle solution;
3) by 2.5 × 2.5 × 0.01(cm
3) pickling metal titanium plate step 2) and gained pickle solution pickling after, use deionized water ultrasonic cleaning clean again, putting into 40mL volumetric molar concentration is 5M NaOH solution, then the polytetrafluoroethyllining lining of volume 50mL is put into, put into autoclave, be placed in 180 DEG C of alkali thermal response 24 h, obtain sodium titanate nano belt; Then in the hydrochloric acid soln of volumetric molar concentration 0.1M, carry out ion-exchange, obtain metatitanic acid nano belt, then by metatitanic acid nano belt 450 DEG C of calcining 1 h in retort furnace, obtain TiO
2nano belt film.
4) by TiO obtained for step 3)
2nano belt film, is immersed in the precursor liquid that 15mL step 1) is obtained, reacts 3 h, reacted sample deionized water rinsing at 80 DEG C, dry, at 400 DEG C of insulation 3 h.Obtain " band-band " hierarchy nano-titanium dioxide film.
Fig. 1 is the X ray diffracting spectrum of the film that this example obtains, and known through contrasting with standard card, products therefrom is Anatase TiO
2(except corresponding to TiO in figure
2outer diffraction peak is all from metal titanium substrate).Fig. 2, Fig. 3 by the electron scanning micrograph of acquisition film, can see that the film of acquisition is that in nano belt, growth has arrangement regular and the nano belt that size is less, namely film be " band-be with " hierarchy nano-titanium dioxide film.
embodiment 2
1) titanyl sulfate quality is 1.75g, and other conditions are with embodiment 1;
2) with embodiment 1;
3) with embodiment 1;
4) in precursor liquid, temperature of reaction is 60 DEG C, and other conditions are with embodiment 1.
Fig. 4 by the electron scanning micrograph of acquisition film, classification nanostructure of can seeing that product has " band-band ".
embodiment 3
1) superoxol consumption is 400mL, and other conditions are with embodiment 1;
2) with embodiment 1;
3) with embodiment 1;
4) with embodiment 1.
Fig. 5 by the electron scanning micrograph of acquisition film, classification nanostructure of can seeing that product has " band-band ".
embodiment 4
1) with embodiment 1;
2) with embodiment 1;
3) with embodiment 1;
4) in precursor liquid, at 90 DEG C, the reaction times is 6 h, and other conditions are with embodiment 1.
Fig. 6 by the electron scanning micrograph of acquisition film, classification nanostructure of can seeing that product has " band-band ".
embodiment 5
1) titanyl sulfate quality is 0.875g, and other conditions are with embodiment 1;
2) with embodiment 1;
3) with embodiment 1;
4) by TiO obtained for step 3)
2nano belt film, is immersed in the precursor liquid that 30mL step 1) is obtained, reacts 12 h, reacted sample deionized water rinsing at 60 DEG C, dry, at 600 DEG C of insulation 1 h, obtains " band-band " hierarchy nano-titanium dioxide film.
Fig. 7 by the electron scanning micrograph of acquisition film, classification nanostructure of can seeing that product has " band-band ".
Claims (1)
1. the preparation method of " band-band " hierarchy nano-titanium dioxide film, is characterized in that, comprise the steps:
1) with deionized water, titanyl sulfate and glycine are dissolved respectively, mix with nitric acid again, the amount ratio of nitric acid and glycine is 0.34mL/g, the amount ratio of titanyl sulfate and glycine is 0.5-1g/g, above-mentioned mixed solution loading crucible is heated to decomposition at 400 DEG C complete, obtains amorphous metal complex compound; Be the H of 30% by above-mentioned amorphous metal complex compound and mass concentration
2o
2solution mixes, and every gram of amorphous metal complex compound uses 20 ~ 800mL H
2o
2solution, reacts 72h, gets supernatant liquid as precursor liquid at room temperature to 80 DEG C;
2) by mass concentration be 50 ~ 55% hydrofluoric acid, mass concentration be 65 ~ 68% nitric acid and deionized water by volume 1:3:6 mix, obtain pickle solution;
3) configuring volumetric molar concentration is 5mol/L NaOH solution, by pickling metal titanium plate step 2) after the pickle solution pickling of gained, use deionized water ultrasonic cleaning clean again, put into above-mentioned NaOH solution, be placed in autoclave, solution is no more than 80% of reactor volume, in 180 DEG C of alkali thermal response 24 h, obtains sodium titanate nano belt; Sample is taken out to be placed in the hydrochloric acid soln of volumetric molar concentration 0.1 mol/L and carries out ion-exchange, obtain metatitanic acid nano belt; Again sample is calcined 1 h at 450 DEG C, obtain titanium dioxide nano-belts;
4) by the titanium dioxide nano-belts that step 3) is obtained, be immersed in the obtained precursor liquid of step 1), at 60 ~ 90 DEG C, react 3 ~ 12h, reacted sample deionized water rinsing, drying, at 400-600 DEG C of insulation 1-3 h, obtains " band-band " hierarchy nano-titanium dioxide film.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105355883A (en) * | 2015-11-18 | 2016-02-24 | 海南大学 | TiN / TiO2 core-shell nanowire array and preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030348A (en) * | 2014-05-14 | 2014-09-10 | 浙江大学 | Preparation method for titanium dioxide nano-belt |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030348A (en) * | 2014-05-14 | 2014-09-10 | 浙江大学 | Preparation method for titanium dioxide nano-belt |
Non-Patent Citations (2)
| Title |
|---|
| 宋小梅: "纳米结构TiO2光电复合薄膜的协同效应", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 * |
| 文伟: "溶液燃烧合成多孔过渡金属氧化物功能粉体", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105355883A (en) * | 2015-11-18 | 2016-02-24 | 海南大学 | TiN / TiO2 core-shell nanowire array and preparation method |
| CN105355883B (en) * | 2015-11-18 | 2017-09-29 | 海南大学 | A kind of TiN/TiO2Core-shell nano linear array and preparation method thereof |
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