CN104986797B - A kind of anatase TiO2the preparation method of nano-tube film - Google Patents
A kind of anatase TiO2the preparation method of nano-tube film Download PDFInfo
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- 239000002071 nanotube Substances 0.000 title claims abstract description 51
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000010936 titanium Substances 0.000 claims abstract description 46
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002253 acid Substances 0.000 claims abstract description 39
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 39
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 229910001868 water Inorganic materials 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 38
- 239000002070 nanowire Substances 0.000 abstract description 28
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 239000003513 alkali Substances 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 230000005684 electric field Effects 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract 1
- 238000005067 remediation Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 51
- 239000000243 solution Substances 0.000 description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 9
- 238000010306 acid treatment Methods 0.000 description 8
- 239000010409 thin film Substances 0.000 description 8
- 238000001000 micrograph Methods 0.000 description 7
- 230000010355 oscillation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The open a kind of anatase TiO of the present invention2The preparation method of nano-tube film, its key step is as follows: metallic titanium plate is immersed in 1.0～2.0 mol/L sodium hydroxide solutions, it is incubated in hydrothermal reaction kettle under 200～220 ° of C after 12～24 hours and is cooled to room temperature, then immerse and hydrochloric acid solution carries out acid exchange obtain metatitanic acid nano wire film；Metatitanic acid nano wire film is immersed in 80 ° of C sulfuric acid solutions of pH=1.5～2.5 and react 24 ~ 72 hours, obtain anatase TiO2Nano-tube film.The inventive method is without reaction template or extra electric field, simple, low cost, the anatase TiO of preparation2Nano-tube film is uniform, well-crystallized is firmly combined with matrix, and photocatalytic activity is significantly higher than alkali full-boiled process and combines the anatase TiO that subsequent heat treatment obtains2Nano wire film, can be applicable to the fields such as photocatalysis environment remediation.
Description
Technical field
The present invention relates to a kind of TiO2The preparation method of thin film, particularly relates to a kind of anatase TiO2The preparation method of nano-tube film.
Background technology
TiO2Nanotube is owing to having the tubular structure of uniqueness and bigger specific surface area, and the application relating to surface reaction and carrier mobility at such as photocatalysis, photoelectrocatalysis, thin-film solar cells, gas sensor etc. possesses excellent performance.But with regard to hollow nanotube structure TiO2For, existing technology of preparing or relate to templated synthesis or need extra electric field anodic oxidation, and the nanotube that the arrangement that produces of High Temperature High Pressure is unordered, industrialization is relatively costly.Such as, patent of invention CN201310497349.6 discloses a kind of by TiO2Nanosphere powder and polyhydroxy Organic substance add in sodium hydroxide solution, and through hydro-thermal reaction, acid exchange and subsequent calcination process and obtain anatase TiO2The technology of nanotube；Patent of invention CN200910071457.0 discloses a kind of electrochemistry anodic oxidation and prepares TiO2The technology of nano-tube film；Patent of invention CN201310223306.9 discloses one and utilizes Ti silk, prepares TiO by electrochemistry anodic oxidation2Nano-tube film, then at TiO2Particle solution dips rear high-temperature calcination, obtains TiO2Nano-particle/TiO2The method of nanotube.
Summary of the invention
The invention provides a kind of without reaction template with extra electric field, the anatase TiO of simple low cost2The preparation method of nano-tube film.
The present invention is dissolved deposition self assembly in sulfuric acid solution by metatitanic acid nano wire and is prepared anatase TiO2Nano-tube film, and can be by regulating the wall thickness of sulfuric acid treatment time-controllable nanotube.Its key step is as follows:
1) metallic titanium plate is cleaned up, be then immersed in the sodium hydroxide solution that concentration is 10～2.0mol/L reacting 12 ~ 24 hours under 200～220 ° of C；
2) taking-up of reacted titanium sheet is cooled to room temperature, after deionized water rinsing, after sonic oscillation 5～10min, carries out acid exchange with the hydrochloric acid of pH=1.0.Preferably, acid exchange processes 2 hours.
3) it is subsequently placed in 80 ° of C hot water, with sulfur acid for adjusting pH value to 1.5 ~ 2.5, takes out after reacting 24～72 hours, with deionized water rinsing, be dried, i.e. can get anatase TiO2Nano-tube film.
In the present invention, being crucial with sulfur acid for adjusting pH value in step 3), i.e. final sulfuric acid solution concentration is the most crucial: excessive concentration, and metatitanic acid nano wire film is based on course of dissolution, it is impossible to form thin film at titanium plate surface；Concentration is too low, then course of dissolution is notable, has been not enough to dissolve regrouping process to form nano-pipe array thin film at titanium plate surface, and metatitanic acid nano wire film pattern generally remains constant.Best results when sulfuric acid solution concentration is pH=2 in the present invention.
After the metatitanic acid nano wire film that alkali full-boiled process is obtained by the present invention is directly immersed in sulfuric acid solution process, hydrogen metatitanic acid nano wire dissolves and is directly reassembled as the anatase TiO of well-crystallized2Nano-pipe array thin film, and its photocatalytic activity is significantly higher than alkali full-boiled process and combines the anatase TiO that subsequent heat treatment obtains2Nano wire film.The method of the present invention is without reaction template, it is not necessary to extra electric field, simple, reproducible, and preparation cost is promoted by low being easy to.
Accompanying drawing explanation
Fig. 1 is the covering field emission scanning electron microscope picture at the metatitanic acid nano wire film of titanium plate surface of embodiment 1 preparation；
Fig. 2 is the covering X-ray diffractogram at the metatitanic acid nano wire film of titanium plate surface of embodiment 1 preparation, in X-ray diffractogram, H2Ti5O11·H2O, H2Ti4O9·H2O: hydrogen metatitanic acid, Ti: titanium；
Fig. 3 is the covering TiO at titanium plate surface of embodiment 1 preparation2The low power field emission scanning electron microscope picture of nano-tube film；
Fig. 4 is the covering TiO at titanium plate surface of embodiment 1 preparation2The high power field emission scanning electron microscope picture of nano-tube film；
Fig. 5 is the covering TiO at titanium plate surface of embodiment 2 preparation2The low power field emission scanning electron microscope picture of nano-tube film；
Fig. 6 is the covering TiO at titanium plate surface of embodiment 2 preparation2The high power field emission scanning electron microscope picture of nano-tube film；
Fig. 7 is the covering TiO at titanium plate surface of embodiment 2 preparation2The X-ray diffractogram of nano-tube film, in X-ray diffractogram, H2Ti4O9·H2O: hydrogen metatitanic acid, A: anatase, Ti: titanium；
Fig. 8 is the covering TiO at titanium plate surface of embodiment 3 preparation2The low power field emission scanning electron microscope picture of nano-tube film；
Fig. 9 is the covering TiO at titanium plate surface of embodiment 3 preparation2The high power field emission scanning electron microscope picture of nano-tube film；
Figure 10 is the covering TiO at titanium plate surface of embodiment 4 preparation2The low power field emission scanning electron microscope picture of nano-tube film；
Figure 11 is the covering TiO at titanium plate surface of embodiment 4 preparation2The high power field emission scanning electron microscope picture of nano-tube film；
Figure 12 is the TiO that alkali full-boiled process combines the preparation in 1 hour of follow-up 450 ° of C heat treatments2The X-ray diffractogram of nano wire film, in X-ray diffractogram, A: anatase, Ti: titanium；
Figure 13 is the concentration curve of film light catalytic degradation rhodamine B aqueous solution.
Detailed description of the invention
The present invention is expanded on further below in conjunction with drawings and Examples and prepares TiO2The method of nano-tube film.But the present invention is not limited solely to following embodiment.
Embodiment
1
Prepared by step 1 metatitanic acid nano wire film
Metallic titanium plate (a size of 2.5 × 2.5 cm that will clean up2) be immersed in the sodium hydroxide solution that 35 milliliters of concentration is 1.25 M, to react 20 hours under 220 ° of C, reaction cleans titanium sheet thin film with deionized water after terminating, and through the acid exchange of the hydrochloric acid of sonic oscillation 5 ~ 10 min and pH=1, obtains hydrogen metatitanic acid nano wire film.
Step 2 sulfuric acid treatment
Titanium sheet step 1 obtained is immersed in the sulfuric acid solution that 12.5 ml of ph are 2.0, reacts 72 hours under 80 ° of C, and reaction is cleaned with deionized water after terminating, and is dried, obtains nano-tube film.
Metatitanic acid nano wire film typical case's pattern that Fig. 1 step display 1 obtains.Fig. 2 illustrates that the metatitanic acid nano wire phase composition that step 1 obtains is mainly two kinds of different hydrogen metatitanic acids.Fig. 3 low power electron scanning micrograph shows, generates uniform TiO at titanium plate surface2Nano-tube film.Figure 4, it is seen that nanotube ordered arrangement, the nano-particles self assemble of diameter about 16 nm forming, the average diameter of nanotube is about 100nm, wall thickness about 33 nm.
Embodiment 2
Prepared by step 1 metatitanic acid nano wire film
With embodiment 1.
Step 2 sulfuric acid treatment
Titanium sheet step 1 obtained is immersed in the sulfuric acid solution that 12.5 ml of ph are 2.0, reacts 48 hours under 80 ° of C, and reaction is cleaned with deionized water after terminating, and is dried, obtains nano-tube film.
The nanotube of Fig. 5 low power electron scanning micrograph display titanium plate surface is evenly distributed and intensive.Fig. 6 high power electron scanning micrograph shows, compares with embodiment 1, and the average diameter of the nanotube of gained is about 125 nm, wall thickness about 41 nm.Fig. 7 shows that nanotube crystalline phase consists of Anatase and a part of unconverted hydrogen metatitanic acid completely.
Embodiment 3
Prepared by step 1 metatitanic acid nano wire film
With embodiment 1.
Step 2 sulfuric acid treatment
Titanium sheet step 1 obtained is immersed in the sulfuric acid solution that 12.5 ml of ph are 2.0, reacts 36 hours under 80 ° of C, and reaction is cleaned with deionized water after terminating, and is dried, obtains nano-tube film.
Fig. 8 low power electron scanning micrograph display titanium plate surface covers the more uniform and intensive nano-tube film of ratio, the unconverted hydrogen metatitanic acid nano wire of some lodging.Fig. 9 high power electron scanning micrograph shows, the average diameter of nanotube is about 133 nm, wall thickness about 58 nm.
Embodiment 4
Prepared by step 1 metatitanic acid nano wire film
With embodiment 1.
Step 2 sulfuric acid treatment
Titanium sheet step 1 obtained is immersed in the sulfuric acid solution that 12.5 ml of ph are 2.0, reacts 24 hours under 80 ° of C, and reaction is cleaned with deionized water after terminating, and is dried, obtains nano-tube film.
Figure 10 low power electron scanning micrograph shows that nano-tube film is uniform and intensive, but compared with Example 3, there is the nano wire of more lodging on surface.From Figure 11 high power electron scanning micrograph it can be seen that the average diameter of nanotube is about 141 nm, wall thickness about 66 nm.
Embodiment 5
Prepared by step 1 metatitanic acid nano wire film
Metallic titanium plate (a size of 2.5 × 2.5 cm that will clean up2) be immersed in the sodium hydroxide solution that 35 milliliters of concentration is 1.0 M, to react 24 hours under 200 ° of C, reaction cleans titanium sheet thin film with deionized water after terminating, and through the acid exchange of the hydrochloric acid of sonic oscillation 5 ~ 10 min and pH=1, obtains hydrogen metatitanic acid nano wire film.
Step 2 sulfuric acid treatment
Titanium sheet step 1 obtained is immersed in the sulfuric acid solution that 12.5 ml of ph are 2.5, reacts 24 hours under 80 ° of C, and reaction is cleaned with deionized water after terminating, and is dried, obtains nano-tube film.
Titanium plate surface covers the most intensive nano-tube film.
Embodiment 6
Prepared by step 1 metatitanic acid nano wire film
Metallic titanium plate (a size of 2.5 × 2.5 cm that will clean up2) be immersed in the sodium hydroxide solution that 35 milliliters of concentration is 2.0 M, to react 12 hours under 200 ° of C, reaction cleans titanium sheet thin film with deionized water after terminating, and through the acid exchange of the hydrochloric acid of sonic oscillation 5 ~ 10 min and pH=1, obtains hydrogen metatitanic acid nano wire film.
Step 2 sulfuric acid treatment
Titanium sheet step 1 obtained is immersed in the sulfuric acid solution that 12.5 ml of ph are 1.5, reacts 48 hours under 80 ° of C, and reaction is cleaned with deionized water after terminating, and is dried, obtains nano-tube film.
Titanium plate surface covers the most intensive nano-tube film.
Photocatalysis performance is tested
By embodiment 1,2,4 sizes obtained are 1.25 × 1.25cm2Nano-tube film carry out photocatalysis performance test.Target degradation product is 12.5 milliliters, the rhodamine B aqueous solution of initial concentration 0.005 mM.After dark absorption 1 hour, under the ultra violet lamp of 18 W, carry out the photocatalysis experiment of 2 hours.
Comparative sample: the metatitanic acid nano wire film that embodiment 1 step 1 obtains, heat treatment 1 hour under 450 ° of C.The XRD result of Figure 12 shows, the phase composition of this nano wire film is anatase TiO2。
It can be observed from fig. 13 that the TiO obtained through sulfuric acid treatment 24～72 h2The photocatalysis performance of nano-tube film is significantly better than that alkali full-boiled process combines anatase TiO prepared by subsequent heat treatment2Nano wire film.
Claims (3)
1. an anatase TiO2The preparation method of nano-tube film, it is characterised in that comprise the steps:
1) clean metallic titanium plate is immersed in the sodium hydroxide solution that concentration is 1.0～2.0mol/L, uses hydro-thermal method to be incubated 12～24 hours under 200 ~ 220 ° of C；
2) after the metallic titanium plate taking-up deionized water rinsing that step 1) is processed, immerse in the hydrochloric acid of pH=1.0, carry out acid exchange；
3) by step 2) metallic titanium plate that processes is placed in 80 ° of C hot water, is 1.5～2.5 with sulfur acid for adjusting pH value, takes out after reacting 24 ~ 72 hours, and with deionized water rinsing, it is dried, obtains anatase TiO2Nano-tube film.
Anatase TiO the most according to claim 12The preparation method of nano-tube film, it is characterised in that described step 2) in acid exchange handling duration be 2 hours.
Anatase TiO the most according to claim 12The preparation method of nano-tube film, it is characterised in that be 2 with sulfur acid for adjusting pH value in described step 3).
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| CN112442688B (en) * | 2020-11-25 | 2021-11-26 | 成都大学 | Anatase phase TiO prepared by titanium substrate2Method for nanotube film |
| CN113600161B (en) * | 2021-08-09 | 2024-02-23 | 大连海事大学 | Preparation method of titanium dioxide nanotube network catalytic plate and application of titanium dioxide nanotube network catalytic plate in sludge antibiotic resistance gene treatment |
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