CN104746129A - Preparation method of immobilized single-crystal anatase TiO2 nanowire membrane layer - Google Patents
Preparation method of immobilized single-crystal anatase TiO2 nanowire membrane layer Download PDFInfo
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- CN104746129A CN104746129A CN201510092235.2A CN201510092235A CN104746129A CN 104746129 A CN104746129 A CN 104746129A CN 201510092235 A CN201510092235 A CN 201510092235A CN 104746129 A CN104746129 A CN 104746129A
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Abstract
The invention discloses a preparation method of an immobilized single-crystal anatase TiO2 nanowire membrane layer. The preparation method comprises the following steps: pre-treatment: cutting a titanium sheet with a certain thickness to a strip, then polishing the surface of the strip by using abrasive paper and washing thoroughly and drying for later use; anodic oxidation treatment: by adopting a two electrode system and taking the pre-treated titanium sheet as a positive electrode and a platinum sheet as a negative electrode, carrying out anodic oxidation treatment to obtain a anatase TiO2 nanowire membrane layer; and post-treatment: calcining the titanium sheet after anodic oxidation treatment. The immobilized single-crystal anatase TiO2 nanowire membrane layer prepared by the method disclosed by the invention can be firmly combined on a Ti substrate and has a single-crystal structure and a proper aspect ratio, so that the transmission and separation efficiency of photo electron cavities are hugely promoted, compounding of photo electron cavity pairs is reduced, and excellent photocatalytic and photoelectrochemical properties are shown. The photocatalytic material is easily separated from water, so that the photocatalytic material is conveniently recovered and recycled from water.
Description
Technical field
The present invention relates to a kind of immobilization monocrystalline anatase octahedrite TiO
2the preparation method of film with nano lines, belongs to field of nano material preparation.
Background technology
Anonizing is that a kind of conventional employing electrochemical method prepares TiO
2the method of film.Be generally employing two electrode system, using platinized platinum or platinum filament as negative electrode, titanium sheet, as anode, applies certain strength of electric field between electrodes, prepares TiO through oxidising process
2oxide membranous layer.In recent years, using anonizing to prepare maximum is TiO
2nanotube, and the length of the nanotube prepared in different electrolyte systems is different.The most frequently used electrolytic solution mainly contains hydrofluoric acid containing (HF) system, fluoride (NaF etc.) system and water-bearing organic system (as ethylene glycol etc.).Generally will, more than 500nm, in HF electrolyte system, due to the chemical dissolution speed on nanotube top, therefore cause the nanotube length of preparation limited containing the nanotube length prepared in HF electrolytic solution.And in NaF electrolyte system, because electrolytic solution is in neutral or slightly acidic, the nanotube length therefore prepared can reach several microns or tens microns.In water-bearing organic electrolytic solution, by changing the preparation parameters such as water ratio, oxidation voltage, oxidization time, pipe range can be obtained and reach hundreds of the micron even nanotube of thousands of microns.And, in organism reaction system, because the viscosity ratio of its electrolytic solution is higher, reduce the velocity of diffusion of fluorion, therefore can obtain shape matching regular uniform, show smoother nanotube.In moisture organic system electrolytic solution, preparing nanotube, the TiO of preparation can be regulated and controled by controlling the parameters such as the proportioning of organic solvent and water in anodic oxidation voltage, oxidization time, electrolytic solution
2the growth velocity of nanotube, the parameter such as length and smooth surface degree.
Summary of the invention
An object of the present invention is to provide one to prepare immobilization monocrystalline anatase octahedrite TiO
2the method of film with nano lines, immobilization monocrystalline anatase octahedrite TiO prepared by the method
2film with nano lines has good photochemical catalysis and photoelectrochemical behaviour, may be used for environmental improvement or solar cell.
The present invention is achieved through the following technical solutions, and the method comprises the following steps:
Pre-treatment: certain thickness titanium sheet is cut into strip, then with sand paper to its surface finish, and rinse dry for standby well.
Anodic oxidation treatment: adopt two electrode systems, using pretreated titanium sheet as anode, platinized platinum, as negative electrode, prepares anatase octahedrite TiO through anodic oxidation treatment
2film with nano lines.
Aftertreatment: calcine in atmosphere through anodised titanium sheet.
Further, in described anodic oxidation treatment step, electrolytic solution is be the ethylene glycol solution of 1 ~ 1.5% moisture containing volume percent, and the mass percentage content of Neutral ammonium fluoride is 0.4 ~ 0.6%.
Further, in described anodic oxidation treatment step, temperature of reaction controls at 24 ~ 26 DEG C, and the mode of boosting step by step applies voltage, and rate of pressure rise is 1V/s, and last voltage constant is at 55 ~ 65V, and the treatment time is 2 ~ 4h.
Further, in described post-processing step, calcination temperature is 400 ~ 500 DEG C, and calcine 2 ~ 3 hours, temperature rise rate is 1 DEG C/min.
Immobilization monocrystalline anatase octahedrite TiO of the present invention
2the detection scheme of film with nano lines photocatalyst result of use is: take concentration as 5mgL
-1methylene blue solution is target contaminant, gets this solution of 50ml and is placed in quartz reactor, adds the monocrystalline anatase octahedrite TiO of preparation
2after film with nano lines, stir 1h in the dark state, then, under 50W Xenon light shining, react 2h.
Beneficial effect of the present invention is: immobilization monocrystalline anatase octahedrite TiO prepared by the present invention
2film with nano lines can firmly be combined on Ti matrix, there is single crystal structure and suitable aspect ratio, facilitate transmission and the separation efficiency of photo-generate electron-hole greatly, decrease the compound that photo-generate electron-hole is right, show outstanding photochemical catalysis and photoelectrochemical behaviour.This photocatalyst material is easy to be separated from water, is conducive to recycling and reusing from water body.
Accompanying drawing explanation
Figure 1 shows that immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the stereoscan photograph of film with nano lines.
Figure 2 shows that immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the x-ray diffractogram of film with nano lines.
Figure 3 shows that immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the photoabsorption spectrogram of film with nano lines.
Figure 4 shows that immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the clearance of film with nano lines degraded 5mg/L methylene blue solution and light application time graph of a relation.
Embodiment
Hereafter will describe content of the present invention in conjunction with specific embodiments in detail.It should be noted that the combination of technical characteristic or the technical characteristic described in following embodiment should not be considered to isolated, they can mutually be combined thus be reached better technique effect.
Figure 1 shows that immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the stereoscan photograph of film with nano lines; Figure 2 shows that immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the x-ray diffractogram of film with nano lines; Figure 3 shows that immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the photoabsorption spectrogram of film with nano lines; Figure 4 shows that immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the clearance of film with nano lines degraded 5mg/L methylene blue solution and light application time graph of a relation.
Embodiment 1
Pre-treatment: it is 100mm that the thickness titanium sheet that is 0.5mm is cut into length, and width is the specification of 20mm, then, adopts 2000 order sand paper effects on surfaces repeatedly to polish, and finally, rinses well and dry for standby.
Anodic oxidation treatment: adopt two electrode systems, pretreated titanium sheet is as anode, and platinized platinum, as negative electrode, carries out anodic oxidation treatment and prepares anatase octahedrite TiO
2film with nano lines, electrolytic solution is the ethylene glycol solution containing 1% (v/v) moisture, ammonium fluoride content is 0.5% (w/w), temperature of reaction controls constant temperature 25 DEG C, the mode of boosting step by step is adopted to apply voltage, rate of pressure rise is 1V/s, and last voltage constant is at 60V, and the treatment time is 3h.
Aftertreatment: the sample after anodic oxidation treatment calcines 2h at 450 DEG C in atmosphere, and temperature rise rate is 1 DEG C/min.
Fig. 1 is immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the stereoscan photograph of film with nano lines; Fig. 2 is immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the x-ray diffractogram of film with nano lines; Fig. 3 is immobilization monocrystalline anatase octahedrite TiO prepared by embodiment 1
2the photoabsorption spectrogram of film with nano lines.
Immobilization monocrystalline anatase octahedrite TiO of the present invention
2the detection scheme of film with nano lines photocatalyst result of use is: take concentration as 5mgL
-1methylene blue solution is target contaminant, gets this solution of 50ml and is placed in quartz reactor, adds the monocrystalline anatase octahedrite TiO of preparation
2after film with nano lines, stir 1h in the dark state, then, under 50W Xenon light shining, react 2h.Fig. 4 is immobilization monocrystalline anatase octahedrite TiO prepared by the present embodiment
2the clearance of film with nano lines degraded 5mg/L methylene blue solution and light application time graph of a relation, as can be seen from the figure, along with the prolongation of light application time, the concentration of pollutent is reducing gradually.
Embodiment 2
Pre-treatment: it is 100mm that the thickness titanium sheet that is 0.5mm is cut into length, and width is the specification of 20mm, then, adopts 2000 order sand paper effects on surfaces repeatedly to polish, and finally, rinses well and dry for standby.
Anodic oxidation treatment: adopt two electrode systems, pretreated titanium sheet is anode, and platinized platinum is negative electrode, carries out anodic oxidation treatment and prepares anatase octahedrite TiO
2film with nano lines, electrolytic solution is the ethylene glycol solution containing 1.5% (v/v) moisture, ammonium fluoride content is 0.6% (w/w), temperature of reaction controls constant temperature 26 DEG C, the mode of boosting step by step is adopted to apply voltage, rate of pressure rise is 1V/s, and last voltage constant is at 65V, and the treatment time is 4h.
Aftertreatment: the sample after anodic oxidation treatment calcines 3h at 500 DEG C in atmosphere, and temperature rise rate is 1 DEG C/min.
Immobilization monocrystalline anatase octahedrite TiO of the present invention
2film with nano lines photocatalyst carries out experiment by the following method and detects: take concentration as 5mgL
-1methylene blue solution is target contaminant, gets this solution of 50ml and is placed in quartz reactor, adds the monocrystalline anatase octahedrite TiO of preparation
2after film with nano lines, stir 1h in the dark state, then, under 50W Xenon light shining, react 2h.Obtained immobilization monocrystalline anatase octahedrite TiO is checked by measuring the clearance placing different time after stain thing
2the photocatalysis characteristic of film with nano lines.Table 1 is immobilization monocrystalline anatase octahedrite TiO
2film with nano lines is to pollutant removal table.
Table 1 immobilization monocrystalline anatase octahedrite TiO
2film with nano lines is to pollutant removal table
Although give some embodiments of the present invention, it will be understood by those of skill in the art that without departing from the spirit of the invention herein, can change embodiment herein.Above-described embodiment is exemplary, should using embodiment herein as the restriction of interest field of the present invention.
Claims (4)
1. an immobilization monocrystalline anatase octahedrite TiO
2the preparation method of film with nano lines, is characterized in that, comprises the following steps:
Pre-treatment: certain thickness titanium sheet is cut into strip, then with sand paper to its surface finish, and rinse dry for standby well;
Anodic oxidation treatment: adopt two electrode systems, using pretreated titanium sheet as anode, platinized platinum, as negative electrode, prepares anatase octahedrite TiO through anodic oxidation treatment
2film with nano lines;
Aftertreatment: calcine in atmosphere through anodised titanium sheet.
2. a kind of immobilization monocrystalline anatase octahedrite TiO as claimed in claim 1
2the preparation method of film with nano lines, is characterized in that, in described anodic oxidation treatment step, electrolytic solution is be the ethylene glycol solution of 1 ~ 1.5% moisture containing volume percent, and the mass percentage content of Neutral ammonium fluoride is 0.4 ~ 0.6%.
3. a kind of immobilization monocrystalline anatase octahedrite TiO as claimed in claim 1
2the preparation method of film with nano lines, is characterized in that, in described anodic oxidation treatment step, temperature of reaction controls at 24 ~ 26 DEG C, and the mode of boosting step by step applies voltage, and rate of pressure rise is 1V/s, and last voltage constant is at 55 ~ 65V, and the treatment time is 2 ~ 4h.
4. a kind of immobilization monocrystalline anatase octahedrite TiO as claimed in claim 1
2the preparation method of film with nano lines, is characterized in that, in described post-processing step, calcination temperature is 400 ~ 500 DEG C, and calcine 2 ~ 3 hours, temperature rise rate is 1 DEG C/min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105220202A (en) * | 2015-10-23 | 2016-01-06 | 北京科技大学 | The preparation method of the three-dimensional porous titanium dioxide zone of oxidation of a kind of titanium base |
| CN106978619A (en) * | 2017-04-10 | 2017-07-25 | 四川理工学院 | A kind of enhancing titania nanotube is to visible light-responded preparation method |
| CN110512264A (en) * | 2019-08-28 | 2019-11-29 | 青岛农业大学 | A kind of preparation method of optoelectronic pole |
| CN110512260A (en) * | 2019-08-28 | 2019-11-29 | 青岛农业大学 | A kind of preparation method of complex light electrode |
| CN110512263A (en) * | 2019-08-28 | 2019-11-29 | 青岛农业大学 | A kind of preparation method of optoelectronic pole |
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| CN101234343A (en) * | 2008-01-24 | 2008-08-06 | 上海交通大学 | Method for preparing high specific area TiO2 photo-catalytic material |
| CN103361689A (en) * | 2013-05-28 | 2013-10-23 | 青岛农业大学 | Method for preparing titanium dioxide nanotube array photoelectrode |
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2015
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| CN101234343A (en) * | 2008-01-24 | 2008-08-06 | 上海交通大学 | Method for preparing high specific area TiO2 photo-catalytic material |
| CN103361689A (en) * | 2013-05-28 | 2013-10-23 | 青岛农业大学 | Method for preparing titanium dioxide nanotube array photoelectrode |
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| QINGHUA CHEN等: "Controlled anodic growth of TiO2 nanobelts and assessment of photoelectrochemical and photocatalytic properties", 《ELECTROCHIMICA ACTA》 * |
| 陈清华: "改性TiO2纳米带制备及光催化降解水中左氧氟沙星研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105220202A (en) * | 2015-10-23 | 2016-01-06 | 北京科技大学 | The preparation method of the three-dimensional porous titanium dioxide zone of oxidation of a kind of titanium base |
| CN105220202B (en) * | 2015-10-23 | 2018-03-06 | 北京科技大学 | A kind of preparation method of the three-dimensional porous titanium dioxide oxide layer of titanium-based |
| CN106978619A (en) * | 2017-04-10 | 2017-07-25 | 四川理工学院 | A kind of enhancing titania nanotube is to visible light-responded preparation method |
| CN110512264A (en) * | 2019-08-28 | 2019-11-29 | 青岛农业大学 | A kind of preparation method of optoelectronic pole |
| CN110512260A (en) * | 2019-08-28 | 2019-11-29 | 青岛农业大学 | A kind of preparation method of complex light electrode |
| CN110512263A (en) * | 2019-08-28 | 2019-11-29 | 青岛农业大学 | A kind of preparation method of optoelectronic pole |
| CN110512264B (en) * | 2019-08-28 | 2020-12-29 | 青岛农业大学 | Preparation method of photoelectrode |
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