CN102534725A - Method for preparing Ag2S-doped TiO2 nanotube electrode - Google Patents
Method for preparing Ag2S-doped TiO2 nanotube electrode Download PDFInfo
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- CN102534725A CN102534725A CN2012100088117A CN201210008811A CN102534725A CN 102534725 A CN102534725 A CN 102534725A CN 2012100088117 A CN2012100088117 A CN 2012100088117A CN 201210008811 A CN201210008811 A CN 201210008811A CN 102534725 A CN102534725 A CN 102534725A
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Abstract
The invention provides a method for preparing a Ag2S-doped TiO2 nanotube electrode, relating to methods for the preparation of electrodes. The method for preparing the Ag2S-doped TiO2 nanotube electrode comprises the following steps of: (1) preparing a TiO2 nanotube on a Ti substrate by adopting an anodic oxidation method; and (2) doping Ag2S on the surface of the TiO2 nanotube by using a continuous ion layer adsorption and reaction method through taking a AgNO3 methanol solution and a Na2S methanol solution as electrolytes, so as to obtain the Ag2S-doped TiO2 nanotube electrode, wherein the concentration of AgNO3 is 0.001 mol/L, and the concentration of Na2S is 0.001 mol/L. The Ag2S-doped TiO2 nanotube electrode prepared by using the method has the advantages that: the Ag2S grains are small in size and even in distribution, so that an excellent degradation effect is achieved when the Ag2S-doped TiO2 nanotube electrode is applied to a photoelectric catalytic oxidation organic substance; and the photoelectrocatalytic performance of the prepared Ag2S-doped TiO2 nanotube electrode can be remarkably improved.
Description
Technical field
The present invention relates to a kind of method for preparing electrode, particularly relate to a kind of preparation Ag
2S doped Ti O
2The method of nanotube electrode.
Background technology
Titanium oxide (TiO
2) be a kind of important inorganic semiconductor functional materials; Having wet quick, air-sensitive, dielectric effect, photoelectricity transforms and superior characteristics such as photocatalysis performance; In high-tech areas such as transmitter, dielectric materials, automatically cleaning material, solar cell, photocatalytic degradation pollutents important application prospects is arranged, become both at home and abroad competitively one of focus of research.With general nano-TiO
2Powder is compared, TiO
2The special construction of nanotube makes it have bigger specific surface area and stronger adsorptive power, is expected to show the electricity conversion of better photocatalysis performance and Geng Gao.
Yet, Detitanium-ore-type TiO
2Energy gap be 3.2 eV, can only absorbing wavelength less than the sunshine of 387.5 nm, and arrive the sunshine medium ultraviolet light (λ of earth surface<400 nm) radiant section has only accounted for about 4% of whole sunshine power spectrum, and visible light content is about 45%, therefore develops the important topic that visible-light-responsive photocatalyst becomes present photocatalysis field.In addition, TiO
2Also there is the on the low side and unhappy problem of degradation rate of quantum yield in photochemical catalysis, and its photon efficiency generally is no more than 10%, and the recombination probability that how to reduce light induced electron and hole also is a problem demanding prompt solution.Existing research shows, adopt metal ion mixing, nonmetal doping, noble metal loading, semi-conductor is compound and method such as surface light sensitization to TiO
2Carry out suitable doping or surface-treated, not only can suppress the compound of light induced electron and hole effectively, and can expand TiO
2Thereby the absorption of visible light scope is improved its photocatalysis performance.
Semi-conductor modification TiO through low energy gap
2Be to pay close attention to many problems at present, but use more narrow gap semiconductor improving TiO at present
2Also human and environment have been caused huge potential hazard in the time of photocatalytic activity, these materials such as CdS and PbS etc. possibly cause secondary pollution.As a kind of important chalcogenide, silver sulfide (Ag
2S), its energy gap is that 0.92 eV is than TiO
2Want much narrow, the toxicity that it had simultaneously is also low than CdS or PbS.Though now about with Ag or Ag
2O is to TiO
2The research of doping vario-property is existing a lot, but about using Ag
2The S particle is to high-sequential, self-assembly TiO
2The adulterated research report of nanotube also seldom.
Summary of the invention
The object of the present invention is to provide a kind of preparation Ag
2S doped Ti O
2The method of nanotube electrode.Make Ag in this way
2The adulterated TiO of S
2Nanotube electrode, Ag
2The S particle is little, is evenly distributed, and is used for catalyzing oxidation of organic compounds and has good degradation effect.
The objective of the invention is to realize through following technical scheme:
Preparation Ag
2S doped Ti O
2The method of nanotube electrode, said method comprises following preparation process:
(1) pre-treatment of Ti substrate: pure titanium sheet is cut into the small pieces of 50 mm * 60 mm, successively through the emery paper polishing of 600#, 1000# to can't see obvious cut, more successively at zero(ppm) water, ultrasonic immersing was cleaned 10 minutes in the acetone, at last with HF, dense HNO
3, H2O processes chemical brightening solution by the volume ratio of 1:4:5, cleaned titanium sheet is put into polishing fluid soak 1 minute up to can't see obvious bubble generation; Use washed with de-ionized water afterwards, drying for standby in vacuum drying oven;
(2) TiO
2The preparation of nanotube electrode: adopting range is the current regulator power supply of 0-30V, and anode is the titanium sheet, and platinum guaze is made negative electrode, and electrolytic solution is 0.5 wt%NH
4F and 0.5 mol/L Na
2SO
4The aqueous solution, the pH value of solution is with NaOH and H
2SO4 is adjusted to 3; The anodic oxidation voltage scope is 20-25 V, and the polarization time is 60-120 min, and room temperature is carried out under magnetic agitation; The titanium sheet sample that makes cleans through zero(ppm) water, behind air drying, places retort furnace, in air atmosphere, calcines 3 h down for 500 ℃;
(3) Ag
2S doped Ti O
2The preparation of nanotube electrode: with the TiO that makes
2Nanotube is immersed in 0.001 mol/L AgNO successively
3Methanol solution, methanol solution, 0.001 mol/L Na
2The methanol solution of S, methanol solution constitutes a circulation; Repeat the Ag that above step makes different dopings
2S doped Ti O
2Nanotube electrode; With electrode 150 ℃ of drying 1 h in vacuum drying oven, make Ag
2S doped Ti O
2Nanotube electrode.
Described preparation Ag
2S doped Ti O
2The method of nanotube electrode, it is with TiO
2Nanotube electrode is immersed in 0.001 mol/L AgNO
3Methanol solution, methanol solution, 0.001 mol/L Na
2The methanol solution of S, methanol solution constitutes a circulation, obtains Ag one time
2The adulterated TiO of S
2Nanotube electrode; Repeat above-mentioned steps, utilize different number of cycles, can obtain the Ag of different dopings
2The adulterated TiO of S
2Nanotube electrode.
Described preparation Ag
2S doped Ti O
2The method of nanotube electrode, its described repetition above-mentioned steps, the Ag that 10 ~ 16 circulations of warp obtain
2The adulterated TiO of S
2Nanotube electrode.
Advantage of the present invention and effect are:
The present invention is 3 0.5 wt%NH with pH
4F and 0.5 mol/L Na
2SO
4The aqueous solution is ionogen, under the voltage of 20 ~ 25 V, adopts anonizing on the Ti substrate, to prepare TiO
2Nanotube is through 500
oTiO after the C thermal treatment
2Nanotube.With the TiO that makes
2Nanotube is immersed in 0.001 mol/L AgNO successively
3Methanol solution, methanol solution, 0.001 mol/L Na
2The methanol solution of S, methanol solution obtains Ag
2The adulterated TiO of S
2Nanotube electrode.The step of repetition 2 makes the Ag of different dopings
2S doped Ti O
2Nanotube electrode.Make Ag in this way
2The adulterated TiO of S
2Nanotube electrode, Ag
2The S particle is little, is evenly distributed, and is used for catalyzing oxidation of organic compounds and has good degradation effect.
Description of drawings
Fig. 1 is 10 the number Ag that mix
2TiO behind the S
2The SEM figure of nanotube electrode;
Fig. 2 is 16 the number Ag that mix
2TiO behind the S
2The SEM figure of nanotube electrode;
Fig. 3 is 25 the number Ag that mix
2TiO behind the S
2The SEM figure of nanotube electrode;
Fig. 4 is the Ag of different doping number of times
2S doped Ti O
2The tropeolin-D photoelectrocatalysis percent of decolourization of nanotube electrode.
Annotate: Fig. 1-Fig. 4 of the present invention is the analysis synoptic diagram or the photo of product state, figure Chinese words or the unintelligible understanding that does not influence technical scheme of the present invention of image.
Embodiment
Embodiment 1
Pure titanium sheet is cut into the small pieces of 50 mm * 60 mm, successively through the emery paper polishing of 600#, 1000# to can't see obvious cut, more successively at zero(ppm) water, ultrasonic immersing was cleaned 10 minutes in the acetone, at last with HF, dense HNO
3, H
2O processes chemical brightening solution by the volume ratio of 1:4:5, cleaned titanium sheet is put into polishing fluid soak 1 minute up to can't see obvious bubble generation.Use washed with de-ionized water afterwards, drying for standby in vacuum drying oven.
Adopting range is the current regulator power supply of 0-30V, and anode is the titanium sheet, and platinum guaze is made negative electrode, and electrolytic solution is 0.5 wt%NH
4F and 0.5 mol/L Na
2SO
4The aqueous solution, the pH value of solution is with NaOH and H
2SO
4Be adjusted to 3.The anodic oxidation voltage scope is 20-25 V, and the polarization time is 60-120 min, and room temperature is carried out under magnetic agitation.The titanium sheet sample that makes cleans through zero(ppm) water, behind air drying, places retort furnace, in air atmosphere, calcines 3 h down for 500 ℃.
With the TiO that makes
2Nanotube is immersed in 0.001 mol/L AgNO successively
3Methanol solution, methanol solution, 0.001 mol/L Na
2The methanol solution of S, methanol solution constitutes a circulation.Repeat the Ag that above step makes different dopings
2S doped Ti O
2Nanotube electrode.With electrode 150 ℃ of drying 1 h in vacuum drying oven, make Ag
2S doped Ti O
2Nanotube electrode.The surface topography that makes electrode is seen accompanying drawing 1 ~ 3.
Adopt three-electrode system test Ag
2S doped Ti O
2The photoelectrocatalysis performance of nanotube electrode is with the NaNO of 0.1 mol/L
3Solution is ionogen, and the xenon lamp source of parallel light is the simulated solar light source, and RST3000 type electrochemical workstation is a power supply, in the self-control quartz reactor, with the Ag of preparation
2S doped Ti O
2Nanotube electrode is a working electrode, and platinum guaze is a counter electrode, and the Ag/AgCl electrode is the three-electrode system degraded tropeolin-D (MO) of reference electrode, and concentration is 20 mg/L, and applying bias is 800 mV, and degradation time is 3 h.The Ag of different doping number of times
2S doped Ti O
2The efficient of the photoelectrocatalysis of nanotube electrode (PEC) degraded tropeolin-D is seen accompanying drawing 4.
Test result shows that employing photoelectrocatalysioxidization oxidization tropeolin-D effect is obvious; The doping number of times increases; The methyl orange degradation rate increases, but all the percent of decolourization than 10 correspondences of mixing is low for the percent of decolourization of the tropeolin-D 16 times, 25 times time of mixing, so doping is with the degradation effect the best 10 times time of mixing.Than unadulterated TiO
2Nanotube electrode, Ag
2The TiO that the S doping is 10 times
2Degradation rate can reach 83 % after nanotube electrode was degraded 60 minutes, had improved nearly 20 %.
Claims (3)
1. prepare Ag
2S doped Ti O
2The method of nanotube electrode is characterized in that, said method comprises following preparation process:
(1) pre-treatment of Ti substrate: pure titanium sheet is cut into the small pieces of 50 mm * 60 mm, successively through the emery paper polishing of 600#, 1000# to can't see obvious cut, more successively at zero(ppm) water, ultrasonic immersing was cleaned 10 minutes in the acetone, at last with HF, dense HNO
3, H2O processes chemical brightening solution by the volume ratio of 1:4:5, cleaned titanium sheet is put into polishing fluid soak 1 minute up to can't see obvious bubble generation; Use washed with de-ionized water afterwards, drying for standby in vacuum drying oven;
(2) TiO
2The preparation of nanotube electrode: adopting range is the current regulator power supply of 0-30V, and anode is the titanium sheet, and platinum guaze is made negative electrode, and electrolytic solution is 0.5 wt%NH
4F and 0.5 mol/L Na
2SO
4The aqueous solution, the pH value of solution is with NaOH and H
2SO4 is adjusted to 3; The anodic oxidation voltage scope is 20-25 V, and the polarization time is 60-120 min, and room temperature is carried out under magnetic agitation; The titanium sheet sample that makes cleans through zero(ppm) water, behind air drying, places retort furnace, in air atmosphere, calcines 3 h down for 500 ℃;
(3) Ag
2S doped Ti O
2The preparation of nanotube electrode: with the TiO that makes
2Nanotube is immersed in 0.001 mol/L AgNO successively
3Methanol solution, methanol solution, 0.001 mol/L Na
2The methanol solution of S, methanol solution constitutes a circulation; Repeat the Ag that above step makes different dopings
2S doped Ti O
2Nanotube electrode; With electrode 150 ℃ of drying 1 h in vacuum drying oven, make Ag
2S doped Ti O
2Nanotube electrode.
2. preparation Ag according to claim 1
2S doped Ti O
2The method of nanotube electrode is characterized in that, and is described with TiO
2Nanotube electrode is immersed in 0.001 mol/L AgNO
3Methanol solution, methanol solution, 0.001 mol/L Na
2The methanol solution of S, methanol solution constitutes a circulation, obtains Ag one time
2The adulterated TiO of S
2Nanotube electrode; Repeat above-mentioned steps, utilize different number of cycles, can obtain the Ag of different dopings
2The adulterated TiO of S
2Nanotube electrode.
3. preparation Ag according to claim 1
2S doped Ti O
2The method of nanotube electrode is characterized in that, described repetition above-mentioned steps, the Ag that 10 ~ 16 circulations of warp obtain
2The adulterated TiO of S
2Nanotube electrode.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194888A (en) * | 2013-04-17 | 2013-07-10 | 东华大学 | Preparation method of efficient and visible-light catalytic function textile |
| CN103205760A (en) * | 2013-04-27 | 2013-07-17 | 厦门大学 | Preparation method of Ag2S/TiO2 composite film photo-anode for photoproduction cathode protection |
| CN104525221A (en) * | 2014-12-22 | 2015-04-22 | 清华大学 | Method for preparing visible-light response titanium dioxide/silver sulfide composite film |
| CN108588130A (en) * | 2018-03-27 | 2018-09-28 | 安徽大学 | A kind of method that bioanalysis prepares titanium dioxide tube based composites |
| CN109746001A (en) * | 2018-12-13 | 2019-05-14 | 广东工业大学 | A kind of tin oxide photonic crystal load tungsten oxide and vulcanization silver composite membrane and its preparation method and application |
| CN110344096A (en) * | 2019-07-26 | 2019-10-18 | 中国科学院海洋研究所 | A kind of AgSbS2It is sensitized TiO2Composite film material and its preparation and application |
| CN114177921A (en) * | 2021-11-30 | 2022-03-15 | 盐城工学院 | Preparation method of lead sulfide and silver co-doped titanium dioxide nanotube with photocatalytic performance |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194888A (en) * | 2013-04-17 | 2013-07-10 | 东华大学 | Preparation method of efficient and visible-light catalytic function textile |
| CN103205760A (en) * | 2013-04-27 | 2013-07-17 | 厦门大学 | Preparation method of Ag2S/TiO2 composite film photo-anode for photoproduction cathode protection |
| CN103205760B (en) * | 2013-04-27 | 2016-01-20 | 厦门大学 | For the Ag of photoproduction galvanic protection 2s/TiO 2the preparation method of composite film photo-anode |
| CN104525221A (en) * | 2014-12-22 | 2015-04-22 | 清华大学 | Method for preparing visible-light response titanium dioxide/silver sulfide composite film |
| CN108588130A (en) * | 2018-03-27 | 2018-09-28 | 安徽大学 | A kind of method that bioanalysis prepares titanium dioxide tube based composites |
| CN108588130B (en) * | 2018-03-27 | 2021-04-13 | 安徽大学 | Method for preparing titanium dioxide tube-based composite material by biological method |
| CN109746001A (en) * | 2018-12-13 | 2019-05-14 | 广东工业大学 | A kind of tin oxide photonic crystal load tungsten oxide and vulcanization silver composite membrane and its preparation method and application |
| CN110344096A (en) * | 2019-07-26 | 2019-10-18 | 中国科学院海洋研究所 | A kind of AgSbS2It is sensitized TiO2Composite film material and its preparation and application |
| CN110344096B (en) * | 2019-07-26 | 2021-09-10 | 中国科学院海洋研究所 | AgSbS2Sensitized TiO2Composite membrane material and preparation and application thereof |
| CN114177921A (en) * | 2021-11-30 | 2022-03-15 | 盐城工学院 | Preparation method of lead sulfide and silver co-doped titanium dioxide nanotube with photocatalytic performance |
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Application publication date: 20120704 |