CN1888135A - Process of preparing single-layer nanometer TiO2 rod film in pure rutile structure - Google Patents
Process of preparing single-layer nanometer TiO2 rod film in pure rutile structure Download PDFInfo
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- CN1888135A CN1888135A CN 200610052743 CN200610052743A CN1888135A CN 1888135 A CN1888135 A CN 1888135A CN 200610052743 CN200610052743 CN 200610052743 CN 200610052743 A CN200610052743 A CN 200610052743A CN 1888135 A CN1888135 A CN 1888135A
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Abstract
The preparation process of single-layer nanometer TiO2 rod film in pure rutile structure includes the following steps: mixing hydrofluoric acid, nitric acid and deionized water to compound acid pickling solution; adding nitric acid and hexamethylenetetramine to obtain reactant solution A; pickling metal titanium plate with the acid pickling solution, soaking the pickled metal titanium plate inside the reactant solution A for reaction at 60-80 deg.c of 24-60 hr to obtain reactant solution B after taking out the plate; pickling one other metal titanium plate, soaking the pickled metal titanium plate inside hydrogen peroxide solution for reaction at 60-80 deg.c of 5-15 min, taking out the plate and washing with deionized water to obtain titanium base plate; soaking the titanium base plate inside the reactant solution B for reaction at 60-80 deg.c over 12 hr, washing the reacted titanium base plate with deionized water and drying to obtain the nanometer TiO2 rod film.
Description
Technical field
The present invention relates to a kind of method for preparing single-layer nanometer TiO 2 rod film in pure rutile structure.
Background technology
The nanometer titania film has a wide range of applications in high-tech areas such as photochemical catalysis, gas sensor, solar cell, biomaterial and nano-devices.The preparation of the ordered nano-structure titanium dioxide individual layer ultrathin film of oriented growth is the basis that makes up some nano-devices, and still, it is also very difficult at present that the acquisition big area has the film of above-mentioned fine structure uniformly.
In addition, the cold condition down nano thin-film of preparation crystalline structure can be avoided impelling the heat treatment step of film crystallization in the conventional technology of preparing, thereby film grain growth, the specific surface area of having avoided thermal treatment to cause descend, and shortcoming such as film cracking.
Summary of the invention
The purpose of this invention is to provide the method for preparing single-layer nanometer TiO 2 rod film in pure rutile structure under a kind of cold condition.
The method for preparing single-layer nanometer TiO 2 rod film in pure rutile structure of the present invention may further comprise the steps:
1) preparating acid washing lotion
With mass concentration is that 50～55% hydrofluoric acid, mass concentration are that 65～68% nitric acid mixes with deionized water 1: 2 by volume～4: 5～7, pickle solution;
2) preparation reaction solution A
In mass concentration is 20～30% hydrogen peroxide solution, add the nitric acid of 0.1～0.4 mol and the Hexamine of 0.01～0.02 mol, reaction solution A;
3) preparation feedback liquid B
After the pickle solution pickling of pickling metal titanium plate with the step 1) gained, clean up in ultrasonic wave with deionized water again, be immersed in then among the reaction solution A, take out metallic titanium plate in reaction under 60～80 ℃ after 24～60 hours, the reaction surplus solution is reaction solution B;
4) preparation titanium-base
Other gets a metallic titanium plate, the surface pickle solution pickling of step 1) gained, clean up in ultrasonic wave with deionized water again, be immersed in mass concentration then and be in 15～30% the hydrogen peroxide solution, after reacting 5～15 minutes under 60～80 ℃, take out, rinse well, get titanium-base with deionized water;
5) reaction
Above-mentioned titanium-base is immersed among the reaction solution B, reacts more than 12 hours down at 60～80 ℃; Use washed with de-ionized water then, drying can obtain single-layer nanometer TiO 2 rod film in pure rutile structure on the surface.
The single-layer nanometer TiO 2 rod film in pure rutile structure visual inspection of the present invention's preparation is faint yellow or pink or peak green uniformly, concrete color depends on the thickness of film, is uniform crystalline structure titanium deoxid film produces interference effect to visible light result.Reaction conditions during control preparation feedback liquid B, and the reaction conditions of preparation single thin film, the gained film thickness can be controlled between 120～180 nanometers.All films all are made up of the individual layer nanorod structure titanium dioxide oriented growth that makes progress, and titanium dioxide is well-crystallized's pure rutile structure.About 10～30 nanometers of the diameter of single nanometer rod, about 120～180 nanometers of length.
Simple, the easy row of the method that the present invention adopts, good reproducibility, the single-layer nanometer TiO 2 rod film in pure rutile structure of preparation is even, well-crystallized, purity height.
Description of drawings
Fig. 1 is the high power field emission scanning electron microscope photo of the titanium-base of embodiment 1 preparation;
Fig. 2 is the high power field emission scanning electron microscope photo of titanium-base of the surface coverage titanium dioxide nano-rod single thin film of embodiment 1 preparation;
Fig. 3 is the x-ray diffraction pattern of titanium-base of the surface coverage titanium dioxide nano-rod single thin film of embodiment 1 preparation, among the figure, and Ruti1e: rutile, Ti: titanium;
Fig. 4 is the high power field emission scanning electron microscope photo of titanium-base of the surface coverage titanium dioxide nano-rod single thin film of embodiment 2 preparation;
Fig. 5 is the x-ray diffraction pattern of titanium-base of the surface coverage titanium dioxide nano-rod single thin film of embodiment 2 preparation, among the figure, and Rutile: rutile, Ti: titanium;
Fig. 6 is the high power field emission scanning electron microscope photo of titanium-base of the surface coverage titanium dioxide nano-rod single thin film of embodiment 3 preparation;
Fig. 7 is the high power field emission scanning electron microscope photo of titanium-base of the surface coverage titanium dioxide nano-rod single thin film of embodiment 4 preparation;
Embodiment
Further set forth the inventive method below in conjunction with embodiment.But the present invention not only is confined to following embodiment.
1) preparating acid washing lotion
With mass concentration is that 55% hydrofluoric acid, mass concentration are 65% nitric acid and 1: 3: 6 by volume mixed of deionized water, pickle solution.
2) preparation reaction solution A
The 50ml mass concentration is that to add 1.0 milliliters of mass concentrations in 30% the hydrogen peroxide solution successively be 63% nitric acid and 100 milligrams of Hexamines (mass percent purity＞99.5%), reaction solution A.
3) preparation feedback liquid B
Be of a size of 5 * 5 * 0.01 (cm
3) pickling metal titanium plate pickle solution pickling under 60 ℃ of temperature of step 1) gained, then in ultrasonic wave, clean up with deionized water.
The metallic titanium plate that cleans up is immersed among the 50ml reaction solution A, reacted 52 hours down, must react surplus solution, i.e. reaction solution B at 80 ℃.
4) preparation titanium-base
Other gets one and is of a size of 5 * 5 * 0.01 (cm
3) metallic titanium plate, the surface then cleans up in ultrasonic wave with deionized water with pickle solution pickling under 60 ℃ of temperature of step 1) gained.
It is in 30% the hydrogen peroxide solution that the metallic titanium plate that cleans up is immersed in the 50ml mass concentration, 80 ℃ of reactions 10 minutes down, titanium-base.
5) reaction
Above-mentioned titanium-base is immersed among the reaction solution B, reacted 20 hours reacted titanium-base deionized water rinsing, drying at 80 ℃ down.
Reaction result
The titanium-base surface topography as shown in Figure 1, the growth of shown nanometer micropore structure nanometer rod single thin film when inducing its afterreaction has vital role.Titanium-base surface, reaction back is uniform pink, generates nanometer rod single thin film as shown in Figure 2, about 150 nanometers of the thickness of film.Fig. 3 shows that the titanium dioxide crystal structure is the pure rutile structure, the well-crystallized.
1) preparating acid washing lotion
With embodiment 1.
2) preparation reaction solution A
With embodiment 1.
3) preparation feedback liquid B
Pickling metal titanium plate is cleaned with embodiment 1; The metallic titanium plate that cleans up is immersed among the 50ml reaction solution A, reacted 56 hours down, must react surplus solution, i.e. reaction solution B at 80 ℃.
4) preparation titanium-base
With embodiment 1.
5) reaction
Above-mentioned titanium-base is immersed among the reaction solution B, reacted 16 hours reacted titanium-base deionized water rinsing, drying at 80 ℃ down.
Reaction result
Titanium-base surface, reaction back is uniform peak green, generates nanometer rod single thin film as shown in Figure 4, about 125 nanometers of the thickness of film, about 30 nanometers of the diameter of single nanometer rod, about 120 nanometers of length.Fig. 5 shows that the titanium dioxide crystal structure is the pure rutile structure, the well-crystallized.
Embodiment 3
1) preparating acid washing lotion
With mass percent concentration is that 50% hydrofluoric acid, mass percent concentration are 68% nitric acid and 1: 4: 7 by volume mixed of deionized water, pickle solution.
2) preparation reaction solution A
The 50ml mass concentration is that to add 0.5 milliliter of mass concentration in 30% the hydrogen peroxide solution successively be 63% nitric acid and 70 milligrams of Hexamines (mass percent purity＞99.5%), reaction solution A.
3) preparation feedback liquid B
Be of a size of 5 * 5 * 0.01 (cm
3) pickling metal titanium plate pickle solution pickling under 60 ℃ of temperature of step 1) gained, then in ultrasonic wave, clean up with deionized water.
The metallic titanium plate that cleans up is immersed among the 50ml reaction solution A, reacted 48 hours down, must react surplus solution, i.e. reaction solution B at 60 ℃.
4) preparation titanium-base
Other gets one and is of a size of 5 * 5 * 0.01 (cm
3) metallic titanium plate, the surface then cleans up in ultrasonic wave with deionized water with pickle solution pickling under 60 ℃ of temperature of step 1) gained;
It is in 20% the hydrogen peroxide solution that the metallic titanium plate that cleans up is immersed in the 50ml mass concentration, 70 ℃ of reactions 8 minutes down, titanium-base.
5) reaction
Above-mentioned titanium-base is immersed among the reaction solution B, reacted 24 hours reacted titanium-base deionized water rinsing, drying at 70 ℃ down.
Reaction result
Titanium-base surface, reaction back is faint yellow uniformly, generates nanometer rod single thin film as shown in Figure 6, about 160 nanometers of the thickness of film, and the titanium dioxide crystal structure is the pure rutile structure, the well-crystallized.
Embodiment 4
1) preparating acid washing lotion
With embodiment 1.
2) preparation reaction solution A
The 50ml mass concentration is that to add 2.0 milliliters of mass concentrations in 30% the hydrogen peroxide solution successively be 63% nitric acid and 140 milligrams of Hexamines (mass percent purity＞99.5%), reaction solution A.
3) preparation feedback liquid B
Pickling metal titanium plate is cleaned with embodiment 1; The metallic titanium plate that cleans up is immersed among the 50ml reaction solution A, reacted 24 hours down, must react surplus solution, i.e. reaction solution B at 70 ℃.
4) preparation titanium-base
Other gets one and is of a size of 5 * 5 * 0.01 (cm
3) metallic titanium plate, surface cleaning is with embodiment 1;
It is in 30% the hydrogen peroxide solution that the metallic titanium plate that cleans up is immersed in the 50ml mass concentration, 60 ℃ of reactions 15 minutes down, titanium-base.
5) reaction
Above-mentioned titanium-base is immersed among the reaction solution B, reacted 48 hours reacted titanium-base deionized water rinsing, drying at 60 ℃ down.
Reaction result
Titanium-base surface, reaction back is faint yellow uniformly, generates nanometer rod single thin film as shown in Figure 7, about 180 nanometers of the thickness of film, and the titanium dioxide crystal structure is the pure rutile structure, the well-crystallized.
Claims (1)
1. method for preparing single-layer nanometer TiO 2 rod film in pure rutile structure is characterized in that may further comprise the steps:
1) preparating acid washing lotion
With mass concentration is that 50～55% hydrofluoric acid, mass concentration are that 65～68% nitric acid mixes with deionized water 1: 2 by volume～4: 5～7, pickle solution;
2) preparation reaction solution A
In mass concentration is 20～30% hydrogen peroxide solution, add the nitric acid of 0.1～0.4 mol and the Hexamine of 0.01～0.02 mol, reaction solution A;
3) preparation feedback liquid B
After the pickle solution pickling of pickling metal titanium plate with the step 1) gained, clean up in ultrasonic wave with deionized water again, be immersed in then among the reaction solution A, take out metallic titanium plate in reaction under 60～80 ℃ after 24～60 hours, the reaction surplus solution is reaction solution B;
4) preparation titanium-base
Other gets a metallic titanium plate, the surface pickle solution pickling of step 1) gained, clean up in ultrasonic wave with deionized water again, be immersed in mass concentration then and be in 15～30% the hydrogen peroxide solution, after reacting 5～15 minutes under 60～80 ℃, take out, rinse well, get titanium-base with deionized water;
5) reaction
Above-mentioned titanium-base is immersed among the reaction solution B, reacts more than 12 hours down at 60～80 ℃; Use washed with de-ionized water then, drying gets final product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101396651B (en) * | 2008-10-17 | 2010-04-21 | 浙江大学 | Nano phototranslating composite film in order structure and preparation method thereof |
| CN101250738B (en) * | 2007-12-04 | 2011-09-14 | 东南大学 | Photoelectrocatalysis oxidization preparation method for titanium alloy surface anticoagulant titanium white film |
| CN102225332A (en) * | 2011-05-06 | 2011-10-26 | 刘少光 | Nanometer linear structured TiO2 carrier with stainless steel substrate, denitration catalyst taking TiO2 carrier as carrier and preparation methods thereof |
| CN103274457A (en) * | 2013-06-17 | 2013-09-04 | 南京碧盾新材料科技有限公司 | General preparation method for TiO2 nanowire film on multiple substrates |
| CN103936066A (en) * | 2014-05-05 | 2014-07-23 | 浙江大学 | Method for preparing rutile titanium dioxide nanometer flower array thin film |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1205000A (en) * | 1996-09-13 | 1999-01-13 | 宏亚株式会社 | Process for preparing thin film of titanium oxide and photodecomposition catalyst |
| CN100391851C (en) * | 2006-02-14 | 2008-06-04 | 浙江大学 | Method for preparing three-dimensional nanometer structure titanium dioxide |
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2006
- 2006-08-01 CN CNB2006100527439A patent/CN100436644C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250738B (en) * | 2007-12-04 | 2011-09-14 | 东南大学 | Photoelectrocatalysis oxidization preparation method for titanium alloy surface anticoagulant titanium white film |
| CN101396651B (en) * | 2008-10-17 | 2010-04-21 | 浙江大学 | Nano phototranslating composite film in order structure and preparation method thereof |
| CN102225332A (en) * | 2011-05-06 | 2011-10-26 | 刘少光 | Nanometer linear structured TiO2 carrier with stainless steel substrate, denitration catalyst taking TiO2 carrier as carrier and preparation methods thereof |
| CN102225332B (en) * | 2011-05-06 | 2013-03-27 | 刘少光 | Nanometer linear structured TiO2 carrier with stainless steel substrate, denitration catalyst taking TiO2 carrier as carrier and preparation methods thereof |
| CN103274457A (en) * | 2013-06-17 | 2013-09-04 | 南京碧盾新材料科技有限公司 | General preparation method for TiO2 nanowire film on multiple substrates |
| CN103274457B (en) * | 2013-06-17 | 2015-01-07 | 南京碧盾新材料科技有限公司 | General preparation method for TiO2 nanowire film on multiple substrates |
| CN103936066A (en) * | 2014-05-05 | 2014-07-23 | 浙江大学 | Method for preparing rutile titanium dioxide nanometer flower array thin film |
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