CN106978619A - A kind of enhancing titania nanotube is to visible light-responded preparation method - Google Patents
A kind of enhancing titania nanotube is to visible light-responded preparation method Download PDFInfo
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- CN106978619A CN106978619A CN201710227885.2A CN201710227885A CN106978619A CN 106978619 A CN106978619 A CN 106978619A CN 201710227885 A CN201710227885 A CN 201710227885A CN 106978619 A CN106978619 A CN 106978619A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of enhancing titania nanotube to visible light-responded preparation method, the preparation method is comprised the steps of：Pure titanium sheet polishing, cleaning are taken, chemical polishing is carried out in hydrogen fluoride solution；Two grades of stepped-up voltage anodic oxidations are carried out in ammonium fluoride, glycerine, water solution system；It is heat-treated in air atmosphere.The preparation method has easy to operate, and the modification to Nano tube array of titanium dioxide is realized by generating homogeneity defect, without introducing second of dopant.Thus response of the Nano tube array of titanium dioxide obtained by preparation method to visible ray is strengthened.
Description
Technical field
It is specially a kind of enhancing the present invention relates to technical field of material chemistry, especially optical electro-chemistry and photocatalysis technology field
Titania nanotube is to visible light-responded preparation method.
Background technology
1972, Japanese Fujishima and Honda reported TiO on Nature magazines2Electrode is in ultraviolet light
Lower energy decomposition water produces hydrogen and oxygen, makes TiO2Enter the sight of researcher as a kind of catalysis material of photoinduction.With TiO2
Turn into the effective sewage disposal of one kind green for getting most of the attention and quickly growing in recent years for the photocatalysis oxidation technique of catalyst
Technology.
At present, TiO2The research of catalyst is concentrated mainly on powder TiO2Application in suspended phase, one of problem
It is the TiO of suspended phase2Photochemical catalyst is separated by filtration difficulty, it is difficult to secondary to use, and which has limited TiO2Application.Using TiO2It is thin
Film then can effectively solve this problem, therefore by titanium-based film material photocatalyst, the new focus as Recent study.
Nano tube array of titanium dioxide can be grown in titanium substrate by electrochemistry anodic oxidation（TNA）Film.
The titania nanotube has well-regulated array structure, high-specific surface area, good mechanically and chemically stability.Due to TNA
In titanium dioxide using the preferable Detitanium-ore-type of photocatalytic activity as primary structure, the structure have 3.2 eV bandwidth, photoproduction
Electron-hole pair is easy and fast to be combined, therefore TNA very low to the absorption efficiency of sunshine, and which has limited its practical application.
In order to improve the visible light-responded of titanium dioxide, conventional method is by Cu2O、BiOI、CdSe、Ag2The low bandwidth such as S
Semiconductor substance and titanium dioxide be compounded to form hetero-junctions.This method preferably be applied to powder titanium dioxide, but
Prepared by anodizing does not apply to then in TNA, cannot be because these materials or its presoma are poorly soluble in the electrolytic solution
Doping is realized while TNA grows.TNA is carried out with metal, metal oxide, nonmetallic materials surface modification be enhancing its can
See another approach of light absorbs activity.The materials such as graphite, gold, silver are used to relative TNA and modified, but in correlation report
In road, the modification approach used is relatively complicated, and used some materials also costly, not possess good promotion price
Value.
Existing defects can also promote photo-generate electron-hole to efficiently separating in semiconductor, but the research of this respect
Then it is rarely reported.
The content of the invention
The present invention is exactly for above technical problem there is provided a kind of enhancing titania nanotube to visible light-responded system
Preparation Method.In this method, Nano tube array of titanium dioxide TNA is prepared with electrochemistry anodic oxidation, in TNA growth course
In, regulate and control electrical parameter, TNA inhomogeneous growth is occurred, is produced homogeneity defect, the photoelectricity of visible ray is rung so as to strengthen TNA
Should activity, absorption rate of the raising to visible ray.
The concrete technical scheme of the present invention is as follows：
A kind of enhancing titania nanotube is to visible light-responded preparation method, and this method refers to：Electrochemical anodic oxidation exists
During growing Nano tube array of titanium dioxide TNA in titanium substrate, using the method regulation and control TNA growth speed of two grades of stepped-up voltages
Rate, it is spontaneous that homogeneity defect is produced in TNA.
This method is specifically comprised the following steps：
The first step, titanium sheet substrate pretreatment.120#, 240#, 400#, 600#, 800#, 000#, 1200# waterproof abrasive paper are used successively
Polish step by step titanium sheet, it is each in deionized water, ethanol successively to be cleaned by ultrasonic 2 minutes, then change in 0.02M aqueous hydrogen fluoride solutions
Optical polishing 30s.
Second step, stepped-up voltage anodic oxidation.Using pretreated titanium sheet as anode, by 10 times of titanium sheet area of area
Stainless steel substrates are negative electrode, are put into oxidation solution and carry out anodic oxidation, and the distance of negative electrode and anode is 5 cm.
Oxidation solution is the solution system that ammonium fluoride is dissolved in G ＆ W, and the mass percent of ammonium fluoride is 0.2% ~ 2%, glycerine
Volume ratio with water is 0.1:1~1:0.1.
Change anodic oxidation voltage in oxidizing process in different levels, make the anodic oxidation of titanium sheet in two grades of stepped-up voltages
It is lower to carry out.Concrete operations are：First with 10 ~ 50V voltage oxide 1 ~ 5 hour, then do not closing power supply, the middle condition not powered off
Under, oxidation voltage is adjusted to 10 ~ 50V, reoxidized 1 ~ 5 hour.On the one hand such voltage mechanism cause TNA to be kept in titanium sheet
Continuous growth, on the other hand makes TNA grow at a different rate, the spontaneous generation homogeneity defect in TNA.
3rd step, high-temperature heat treatment.Titanium sheet after anodic oxidation is put into deionized water after washing, is entered in air atmosphere
Row heat treatment, makes titanium dioxide be changed into required crystalline structure.
Heat treatment temperature is 450 ~ 550 DEG C, and heat treatment time is 1 ~ 5 hour, and room temperature is naturally cooling to after heat treatment and is produced
Required product.
A kind of enhancing titania nanotube that the present invention is provided is to visible light-responded method, by its gained TNA shape
Looks scanning electron microscopic observation, crystalline structure is characterized with X-ray diffraction.TNA visible ray photoelectricity is determined with electrochemistry potentiostatic method
Response.Electro-chemical test is using saturated calomel electrode as reference electrode, and platinized platinum is auxiliary electrode, and attachment TNA titanium sheet is work electricity
Pole, in the 0.1 M Na contained with quartz beaker2SO4Carried out in solution, the visible ray sent with 500 W xenon lamp simulated solars, often
Interval 30s does a switch motion, and the TNA faces of titanium sheet are just to xenon source during test, and the two distance keeps 20 cm.Tested
Apply 0.5 V bias-voltage in journey to Ti electrode by electrochemical workstation, by detecting that the size of photoelectric current judges TNA visible rays
The quality of response.
The positive effect of the present invention is embodied in：
（One）Product obtained by this method obtained by the visible light-responded more single anodic oxidation voltages of Nano tube array of titanium dioxide TNA
There is significant enhancing.
（2）Enhancing visible light-responded TNA is realized by the addition of second of material, but by changing TNA's
Growth rate, homogeneity defect is produced in TNA and to strengthen its visible light-responded.
（3）Using the mechanism of two grades of ladder oxidation voltages in TNA growth courses, control is easy in operating process.
Brief description of the drawings
Fig. 1 is embodiment 1, embodiment 2 and comparative example 1, comparative example 2, comparative example 3 in change of the oxidation current with the time
The curve map of change
Fig. 2 is embodiment 1, embodiment 2 and comparative example 1, comparative example 2, the X ray diffracting spectrum of the products obtained therefrom of comparative example 3
Fig. 3 is the products obtained therefrom TNA20V of comparative example 1 scanning electron microscope (SEM) photograph
Fig. 4 is the products obtained therefrom TNA30V of comparative example 2 scanning electron microscope (SEM) photograph
Fig. 5 is the products obtained therefrom TNA40V of comparative example 3 scanning electron microscope (SEM) photograph
Fig. 6 is the products obtained therefrom TNA30-20V of embodiment 1 scanning electron microscope (SEM) photograph
Fig. 7 is the products obtained therefrom TNA30-40V of embodiment 2 scanning electron microscope (SEM) photograph
Fig. 8 is that embodiment 1, embodiment 2 and comparative example 1, comparative example 2, the products obtained therefrom of comparative example 3 are visible during photoswitch
Photoresponse figure
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiment pair
The present invention is described in further detail, but this should not be interpreted as to the scope of above-mentioned theme of the invention is only limitted to following implementations
Example.
Embodiment 1：
The first step, one size of interception is 20mm × 15mm × 1mm, and purity is 99.99% titanium sheet.Successively with 120#, 240#,
400#, 600#, 800#, 000#, 1200# waterproof abrasive paper polishing titanium sheet, it is each in deionized water, ethanol successively to be cleaned by ultrasonic 2 points
Clock, then the chemical polishing 30s in 0.02M aqueous hydrogen fluoride solutions.
Second step, two grades of stepped-up voltage anodic oxidations.Using pretreated titanium sheet as anode, an area is titanium sheet area 10
Stainless steel substrates again are negative electrode, are put into oxidation solution and carry out anodic oxidation, and the distance of negative electrode and anode is 5 cm.
Oxidation solution is that ammonium fluoride is dissolved in the solution system of G ＆ W, and the mass percent of ammonium fluoride is 0.5 %, glycerine with
The volume ratio of water is 1:1.
Oxidation voltage is 30-20V stepped-up voltage, and total oxidization time is 180 minutes.First in 30V voltages in oxidizing process
After lower oxidation 90 minutes, centre, which is not powered off, to be directly adjusted to 20V oxygen by voltage and changes again 90 minutes.
3rd step, high-temperature heat treatment.Titanium sheet after anodic oxidation is put into deionized water after washing, is entered in air atmosphere
Row heat treatment.
Heat treatment temperature is 500 DEG C, and heat treatment time is 2 hours, and room temperature is naturally cooling to after heat treatment and produces required production
Product, labeled as " TNA30-20V ".
Embodiment 2：
The first step, one size of interception is 20mm × 15mm × 1mm, and purity is 99.99% titanium sheet.Successively with 120#, 240#,
400#, 600#, 800#, 000#, 1200# waterproof abrasive paper polishing titanium sheet, it is each in deionized water, ethanol successively to be cleaned by ultrasonic 2 points
Clock, then the chemical polishing 30s in 0.02M aqueous hydrogen fluoride solutions.
Second step, two grades of stepped-up voltage anodic oxidations.Using pretreated titanium sheet as anode, an area is titanium sheet area 10
Stainless steel substrates again are negative electrode, are put into oxidation solution and carry out anodic oxidation, and the distance of negative electrode and anode is 5 cm.
Oxidation solution is that ammonium fluoride is dissolved in the solution system of G ＆ W, and the mass percent of ammonium fluoride is 0.5 %, glycerine with
The volume ratio of water is 1:1.
Oxidation voltage is 30-40V stepped-up voltage, and total oxidization time is 180 minutes.First in 30V voltages in oxidizing process
After lower oxidation 90 minutes, centre, which is not powered off, to be directly adjusted to 40V by voltage and reoxidizes 90 minutes.
3rd step, high-temperature heat treatment.Titanium sheet after anodic oxidation is put into deionized water after washing, is entered in air atmosphere
Row heat treatment.
Heat treatment temperature is 500 DEG C, and heat treatment time is 2 hours, and room temperature is naturally cooling to after heat treatment and produces required production
Product, labeled as " TNA30-40V ".
Comparative example 1
The first step, one size of interception is 20mm × 15mm × 1mm, and purity is 99.99% titanium sheet.Successively with 120#, 240#,
400#, 600#, 800#, 000#, 1200# waterproof abrasive paper polishing titanium sheet, it is each in deionized water, ethanol successively to be cleaned by ultrasonic 2 points
Clock, then the chemical polishing 30s in 0.02M aqueous hydrogen fluoride solutions.
Second step, single ultor oxidation.Using pretreated titanium sheet as anode, an area is 10 times of titanium sheet area
Stainless steel substrates are negative electrode, are put into oxidation solution and carry out anodic oxidation, and the distance of negative electrode and anode is 5 cm.
Oxidation solution is that ammonium fluoride is dissolved in the solution system of G ＆ W, and the mass percent of ammonium fluoride is 0.5 %, glycerine with
The volume ratio of water is 1:1.
Oxidation voltage is 20V single voltage, and oxidization time is 180 minutes.
3rd step, high-temperature heat treatment.Titanium sheet after anodic oxidation is put into deionized water after washing, is entered in air atmosphere
Row heat treatment.
Heat treatment temperature is 500 DEG C, and heat treatment time is 2 hours, and room temperature is naturally cooling to after heat treatment and produces required production
Product, labeled as " TNA20V ".
Comparative example 2
The first step, one size of interception is 20mm × 15mm × 1mm, and purity is 99.99% titanium sheet.Successively with 120#, 240#,
400#, 600#, 800#, 000#, 1200# waterproof abrasive paper polishing titanium sheet, it is each in deionized water, ethanol successively to be cleaned by ultrasonic 2 points
Clock, then the chemical polishing 30s in 0.02M aqueous hydrogen fluoride solutions.
Second step, single ultor oxidation.Using pretreated titanium sheet as anode, an area is 10 times of titanium sheet area
Stainless steel substrates are negative electrode, are put into oxidation solution and carry out anodic oxidation, and the distance of negative electrode and anode is 5 cm.
Oxidation solution is that ammonium fluoride is dissolved in the solution system of G ＆ W, and the mass percent of ammonium fluoride is 0.5 %, glycerine with
The volume ratio of water is 1:1.
Oxidation voltage is 30V single voltage, and oxidization time is 180 minutes.
3rd step, high-temperature heat treatment.Titanium sheet after anodic oxidation is put into deionized water after washing, is entered in air atmosphere
Row heat treatment.
Heat treatment temperature is 500 DEG C, and heat treatment time is 2 hours, and room temperature is naturally cooling to after heat treatment and produces required production
Product, labeled as " TNA30V ".
Comparative example 3
The first step, one size of interception is 20mm × 15mm × 1mm, and purity is 99.99% titanium sheet.Successively with 120#, 240#,
400#, 600#, 800#, 000#, 1200# waterproof abrasive paper polishing titanium sheet, it is each in deionized water, ethanol successively to be cleaned by ultrasonic 2 points
Clock, then the chemical polishing 30s in 0.02M aqueous hydrogen fluoride solutions.
Second step, single ultor oxidation.Using pretreated titanium sheet as anode, an area is 10 times of titanium sheet area
Stainless steel substrates are negative electrode, are put into oxidation solution and carry out anodic oxidation, and the distance of negative electrode and anode is 5 cm.
Oxidation solution is that ammonium fluoride is dissolved in the solution system of G ＆ W, and the mass percent of ammonium fluoride is 0.5 %, glycerine with
The volume ratio of water is 1:1.
Oxidation voltage is 40V single voltage, and oxidization time is 180 minutes.
3rd step, high-temperature heat treatment.Titanium sheet after anodic oxidation is put into deionized water after washing, is entered in air atmosphere
Row heat treatment.
Heat treatment temperature is 500 DEG C, and heat treatment time is 2 hours, and room temperature is naturally cooling to after heat treatment and produces required production
Product, labeled as " TNA40V ".
Embodiment and comparative example analysis：
As seen from Figure 1, under the single oxidation voltage mechanism of comparative example 1,2,3, after the oxidation reaction of 90 minutes, electricity
Stream remains in that basicly stable.In two grades of ladders oxidation of embodiment 1, voltage is adjusted to 20V after being aoxidized 90 minutes through 30V,
Significantly rising to occurs in oxidation current, and shows that TNA growth rate is increased.In two grades of ladders oxidation of embodiment 2, warp
Voltage is adjusted to 40V by 30V after aoxidizing 90 minutes, and oxidation current is substantially reduced, and shows that TNA growth rate reduces.
The period exchanged in embodiment 1,2 voltages, because of the mutation of TNA growth rates, homogeneity defect will be produced in TNA.
As seen from Figure 2, the dioxy in embodiment 1, embodiment 2 and comparative example 1, comparative example 2, the gained TNA of comparative example 3
Changing titanium has identical anatase structured, shows there is homogeney in the titanium dioxide obtained by two stages of embodiment 1,2.
It can be seen that by Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7 and be respectively provided with and received by embodiment 1,2 and the gained TNA of comparative example 1,2,3
Mitron array structure.
As seen from Figure 8, the visible light-responded of TNA is better than by comparative example obtained by embodiment 1,2 two grades of stepped-up voltages
1st, TNA's obtained by 2,3 single voltages is visible light-responded, shows that one kind that the present invention is provided strengthens titania nanotube to visible
The method of photoresponse, can effectively strengthen response of the titania nanotube to visible ray.
Example described above is only the preferred embodiment of this patent, but the protection domain of this patent is not limited thereto.
It should be pointed out that for those skilled in the art, on the premise of this patent principle is not departed from, according to this specially
The technical scheme and its inventional idea of profit, can also make some improvements and modifications, and these improvements and modifications also should be regarded as this specially
The protection domain of profit.
Claims (4)
1. a kind of enhancing titania nanotube is to visible light-responded preparation method, it is characterised in that comprise the following steps：
The first step, titanium sheet substrate pretreatment, titanium sheet of being polished step by step with waterproof abrasive paper, ultrasound is clear in deionized water, ethanol successively
Wash, then the chemical polishing in 0.2 M aqueous hydrogen fluoride solutions；
Second step, stepped-up voltage anodic oxidation is stainless by 10 times of titanium sheet area of area using pretreated titanium sheet as anode
Steel disc is negative electrode, and anodic oxidation is carried out in ammonium fluoride, glycerine, the aqueous solution；
3rd step, high-temperature heat treatment, the titanium sheet after anodic oxidation is put into deionized water after washing, and heat is carried out in air atmosphere
Processing, makes titanium dioxide be changed into required crystalline structure.
2. a kind of enhancing titania nanotube is to visible light-responded preparation method according to claim 1, its feature exists
It is in the composition of anodic oxidation electrolyte：The mass percent of ammonium fluoride is 0.2% ~ 2%, and the volume ratio of glycerine and water is 0.1:1~
1:0.1。
3. a kind of enhancing titania nanotube is to visible light-responded preparation method according to claim 1, its feature exists
Carried out in anodic oxidation under two grades of stepped-up voltages：First in 10 ~ 50V oxidation at voltages 1 ~ 5 hour, then in the condition not powered off
Under, oxidation voltage is adjusted to 10 ~ 50V, reoxidized 1 ~ 5 hour.
4. a kind of enhancing titania nanotube is to visible light-responded preparation method according to claim 1, its feature exists
In：Sample after anodic oxidation is through high-temperature heat treatment, and the temperature of heat treatment is 450 ~ 550 DEG C, and heat treatment time is 1 ~ 5 hour,
Room temperature is naturally cooling to after heat treatment.
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Cited By (4)
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| CN108677208A (en) * | 2018-05-29 | 2018-10-19 | 四川理工学院 | A kind of preparation method of the TiO 2 nanotubes modified enhancing photoelectric respone of manganese |
| CN109750339A (en) * | 2019-03-25 | 2019-05-14 | 四川农业大学 | With absorption visible light and near-infrared mixing appearance structure optoelectronic pole and preparation method |
| CN110699733A (en) * | 2019-11-20 | 2020-01-17 | 中国计量大学 | Preparation method, product and application of titanium alloy porous oxide film |
| RU2732130C1 (en) * | 2019-06-18 | 2020-09-11 | Федеральное государственное автономное образовательное учреждение высшего образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" | Method of producing photocatalyst based on nanotubular titanium dioxide |
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| CN110699733A (en) * | 2019-11-20 | 2020-01-17 | 中国计量大学 | Preparation method, product and application of titanium alloy porous oxide film |
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Application publication date: 20170725 |