CN101514471A - Method for preparing TiO2 nanotube array film - Google Patents
Method for preparing TiO2 nanotube array film Download PDFInfo
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- CN101514471A CN101514471A CNA2009100714570A CN200910071457A CN101514471A CN 101514471 A CN101514471 A CN 101514471A CN A2009100714570 A CNA2009100714570 A CN A2009100714570A CN 200910071457 A CN200910071457 A CN 200910071457A CN 101514471 A CN101514471 A CN 101514471A
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Abstract
The invention provides a method for a preparing TiO2 nanotube array film, relating to a method for preparing a nanotube film. The method solves the problems of the prior art that the prepared nanotube array film features thin film, irregular micro appearance, heterogeneous length of nanotubes, reunion of tube orifice and cracking of the film. The preparation method comprises: 1. a titanium plate is cut into two titanium sheets of the same size, and polishing, ultrasound processing and washing are carried out on the two titanium sheets; 2. electrolyte is prepared; 3. primary anodic oxidation is carried out on the titanium sheets; 4. demoulding is carried out; 5. secondary anodic oxidation is carried out on the titanium sheets; 6. the titanium sheets are dried after ultrasonic processing; and 7. calcination treatment is carried out, thus obtaining the TiO2 nanotube array film. In the invention, twice anodic oxidations are carried out on the titanium sheets, thus producing the TiO2 nanotube array film featuring regular micro appearance, homogeneous, smoothness, thick film layer, reunion-free tube orifice and no cracking. The preparation method of the invention features simple technique and equipment and controllable thickness of the nanotube film.
Description
Technical field
The present invention relates to a kind of preparation method of nano-tube film.
Background technology
Titanium dioxide (TiO
2) as a kind of important inorganic semiconductor functional materials, transform and superior characteristics such as photocatalysis performance because of having wet quick, air-sensitive, dielectric effect, photoelectricity, in fields 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.At present, preparation TiO
2The method of nanotube mainly contains three kinds: template, hydrothermal method and anonizing.Wherein anonizing is because of TiO simple to operate and preparation
2Directly link to each other with Schottky barrier between nanotube and the metal titanium conductive substrates, in conjunction with firmly, so the most commonly used; (inorganic electrolyte liquid is to TiO but because of there are many shortcomings in employed electrolytic solution in preparation process
2Have very strong dissolving power and the organic solvent in the organic electrolyte that the electrochemical reaction of oxidising process is had certain restraining effect), the nano-pipe array thin film that causes obtaining exists that rete thin (the nano-pipe array thin film thickness of inorganic electrolyte liquid preparation is 1～7 μ m), microscopic appearance are irregular, nanotube length heterogeneity, the mouth of pipe are reunited and film rimose problem.
Summary of the invention
The present invention seeks to have in order to solve nano-pipe array thin film that existing method prepares that rete is thin, microscopic appearance is irregular, nanotube length heterogeneity, the mouth of pipe reunite and film rimose problem, and provides a kind of TiO
2The preparation method of nano-pipe array thin film.
A kind of TiO
2The preparation method of nano-pipe array thin film realizes according to the following steps: one, the titanium plate is cut into two measure-alike titanium sheets, then two titanium sheets are polished, then put into acetone supersound process 10～60min, use distilled water flushing then 3～5 times; Two, the Neutral ammonium fluoride that takes by weighing 0.5～1.5g is dissolved in the distilled water of 4～10mL, and ethylene glycol or the glycerol with 100～200mL mixes then, makes electrolytic solution; Three, in the electrolytic solution that will make through the parallel immersion step 2 of two titanium sheets that step 1 is handled at ambient temperature, a slice is an anode, and another sheet is a negative electrode, applies the voltage of 20～70V, then electrolysis treatment 20～60min; Four, take out as anodic titanium sheet, put into dilute acid soln supersound process 5～30min, use distilled water flushing then 3～5 times; Five, as anode, apply the voltage of 20～60V, then electrolysis treatment 0.5～72h in the freshly prepd electrolytic solution of step 4 being handled of titanium sheet immersion step 2; Six, take out as anodic titanium sheet, put into ethanol supersound process 5～20min, dry naturally; Seven, the titanium sheet after will drying is put into retort furnace, is that calcination processing 2～5h cools to room temperature with the furnace, promptly obtains TiO under 300～700 ℃ the condition in temperature
2Nano-pipe array thin film; Wherein dilute acid soln is dilution heat of sulfuric acid, dilute nitric acid solution or dilute hydrochloric acid solution in the step 4.
The present invention by two step anonizings at titanium matrix surface one deck nano-pipe array thin film of having grown, the film that obtains have rete thick (90～110 μ m), neat microscopic appearance, nanometer mouth of pipe homogeneous, smooth, do not have and reunite and film does not have the rimose advantage, and can be by adjusting the structure of anodizing time control nano-tube array, in addition can also be in nanotube the assembling metal ion.Technology of the present invention is simple and equipment is simple.
Description of drawings
Fig. 1 is embodiment 35 resultant product TiO
2The stereoscan photograph of nano-pipe array thin film, Fig. 2 are the stereoscan photographs of the nano-pipe array thin film of inorganic electrolyte liquid preparation, and Fig. 3 is the stereoscan photograph of the nano-pipe array thin film of organic electrolyte preparation.
Embodiment
Embodiment one: present embodiment TiO
2The preparation method of nano-pipe array thin film realizes according to the following steps: one, the titanium plate is cut into two measure-alike titanium sheets, then two titanium sheets are polished, then put into acetone supersound process 10～60min, use distilled water flushing then 3～5 times; Two, the Neutral ammonium fluoride that takes by weighing 0.5～1.5g is dissolved in the distilled water of 4～10mL, and ethylene glycol or the glycerol with 100～200mL mixes then, makes electrolytic solution; Three, in the electrolytic solution that will make through the parallel immersion step 2 of two titanium sheets that step 1 is handled at ambient temperature, a slice is an anode, and another sheet is a negative electrode, applies the voltage of 20～70V, then electrolysis treatment 20～60min; Four, take out as anodic titanium sheet, put into dilute acid soln supersound process 5～30min, use distilled water flushing then 3～5 times; Five, as anode, apply the voltage of 20～60V, then electrolysis treatment 0.5～72h in the freshly prepd electrolytic solution of step 4 being handled of titanium sheet immersion step 2; Six, take out as anodic titanium sheet, put into ethanol supersound process 5～20min, dry naturally; Seven, the titanium sheet after will drying is put into retort furnace, is that calcination processing 2～5h cools to room temperature with the furnace, promptly obtains TiO under 300～700 ℃ the condition in temperature
2Nano-pipe array thin film; Wherein dilute acid soln is dilution heat of sulfuric acid, dilute nitric acid solution or dilute hydrochloric acid solution in the step 4.
Employed chemical reagent all is an analytical pure in the present embodiment.
The TiO of present embodiment preparation
2The thickness of nano-pipe array thin film thickens along with electrolytic time lengthening.
The purpose of polishing in the present embodiment step 1 is in order thoroughly to dispose the dirt on the titanium sheet.
Employed negative electrode still is the titanium sheet in the step 3 in the present embodiment step 5.
Using the purpose of distilled water in the present embodiment is in order to dispose the organic solvent on the anode titanium sheet.
Embodiment two: what present embodiment and embodiment one were different is that two titanium sheets are of a size of 25mm * 10mm in the step 1.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is to adopt 50～300Cw water-proof abrasive paper, 500～1000Cw water-proof abrasive paper and 1500～2500Cw water-proof abrasive paper to polish respectively to two titanium sheets in the step 1.Other step and parameter are identical with embodiment one or two.
Embodiment four: what present embodiment was different with embodiment one or two is to adopt 120Cw water-proof abrasive paper, 800Cw water-proof abrasive paper and 2000Cw water-proof abrasive paper to polish respectively to two titanium sheets in the step 1.Other step and parameter are identical with embodiment one or two.
Embodiment five: what present embodiment and embodiment three were different is that ultrasonic frequency is that 30～60kHz, power are 150～200W in the step 1.Other step and parameter are identical with embodiment three.
Embodiment six: what present embodiment and embodiment three were different is that ultrasonic frequency is that 40kHz, power are 200W in the step 1.Other step and parameter are identical with embodiment three.
Embodiment seven: present embodiment and embodiment one to six are different be in the step 1 supersound process time be 20～50min.Other step and parameter are identical with embodiment one to six.
Embodiment eight: present embodiment and embodiment one to six are different be in the step 1 supersound process time be 30min.Other step and parameter are identical with embodiment one to six.
Embodiment nine: what present embodiment was different with embodiment seven or eight is that the distilled water flushing number of times is 4 times in the step 1.Other step and parameter are identical with embodiment seven or eight.
Embodiment ten: what present embodiment and embodiment one, two or five were different is that the Neutral ammonium fluoride that takes by weighing 0.6～1.2g in the step 2 is dissolved in the distilled water of 5～9mL, and ethylene glycol or the glycerol with 120～180mL mixes then.Other step and parameter are identical with embodiment one, two or five.
Embodiment 11: what present embodiment and embodiment one, two or five were different is that the Neutral ammonium fluoride that takes by weighing 1.0g in the step 2 is dissolved in the distilled water of 5mL, and ethylene glycol or the glycerol with 150mL mixes then.Other step and parameter are identical with embodiment one, two or five.
Embodiment 12: what present embodiment and embodiment one to ten were different is that the voltage that applies in the step 3 is 30～60V.Other step and parameter are identical with embodiment one to ten.
Embodiment 13: what present embodiment and embodiment one to ten were different is that the voltage that applies in the step 3 is 40V.Other step and parameter are identical with embodiment one to ten.
Embodiment 14: present embodiment is different with embodiment 12 or 13 be in the step 3 electrolysis treatment time be 30～50min.Other step and parameter are identical with embodiment 12 or 13.
Embodiment 15: present embodiment is different with embodiment 12 or 13 be in the step 3 electrolysis treatment time be 40min.Other step and parameter are identical with embodiment 12 or 13.
Embodiment 16: present embodiment and embodiment one, two, five or 12 are different is that the volumetric molar concentration of dilute acid soln in the step 4 is 0.5～3mol/L.Other step and parameter are identical with embodiment one, two, five or 12.
Using the purpose of diluted acid in the present embodiment is in order to slough the rete of titanium plate surface.
Embodiment 17: present embodiment and embodiment one, two, five or 12 are different is that the volumetric molar concentration of dilute acid soln in the step 4 is 2mol/L.Other step and parameter are identical with embodiment one, two, five or 12.
Embodiment 18: present embodiment and embodiment one to 16 are different be in the step 4 supersound process time be 10～20min.Other step and parameter are identical with embodiment one to 16.
Embodiment 19: present embodiment and embodiment one to 16 are different be in the step 4 supersound process time be 15min.Other step and parameter are identical with embodiment one to 16.
Embodiment 20: what present embodiment was different with embodiment 18 or 19 is that the distilled water flushing number of times is 4 times in the step 4.Other step and parameter are identical with embodiment 18 or 19.
Embodiment 21: what present embodiment was different with embodiment 16 or 17 is that the voltage that applies in the step 5 is 30～50V.Other step and parameter are identical with embodiment 16 or 17.
Embodiment 22: what present embodiment was different with embodiment 16 or 17 is that the voltage that applies in the step 5 is 40V.Other step and parameter are identical with embodiment 16 or 17.
Embodiment 23: present embodiment and embodiment one to 21 are different be in the step 5 electrolysis treatment time be 2～68h.Other step and parameter are identical with embodiment one to 21.
Embodiment 24: present embodiment and embodiment one to 21 are different be in the step 5 electrolysis treatment time be 8～50h.Other step and parameter are identical with embodiment one to 21.
Embodiment 25: present embodiment and embodiment one to 21 are different be in the step 5 electrolysis treatment time be 30h.Other step and parameter are identical with embodiment one to 21.
Embodiment 26: present embodiment and embodiment one to 21 are different be in the step 5 electrolysis treatment time be 40h.Other step and parameter are identical with embodiment one to 21
Embodiment 27: what present embodiment and embodiment one, two, five, 12 or 21 were different is that ultrasonic frequency is that 30～60kHz, power are 80～100W in the step 6.Other step and parameter are identical with embodiment one, two, five, 12 or 21.
Embodiment 28: what present embodiment and embodiment one, two, five, 12 or 21 were different is that ultrasonic frequency is that 40kHz, power are 70W in the step 6.Other step and parameter are identical with embodiment one, two, five, 12 or 21.
Embodiment 29: present embodiment and embodiment one to 27 are different be in the step 6 supersound process time be 8～16min.Other step and parameter are identical with embodiment one to 27.
Embodiment 30: present embodiment and embodiment one to 27 are different be in the step 6 supersound process time be 12min.Other step and parameter are identical with embodiment one to 27.
The embodiment hentriaconta-: that present embodiment is different with embodiment 27 or 28 is calcination processing 3～4h in the step 7.。Other step and parameter are identical with embodiment 27 or 28.
Embodiment 32: that present embodiment is different with embodiment 27 or 28 is calcination processing 3.5h in the step 7.。Other step and parameter are identical with embodiment 27 or 28.
Embodiment 33: present embodiment and embodiment one to hentriaconta-different be that temperature is 400～600 ℃ in the step 7.Other step and parameter and embodiment one to 30 are in identical.
Embodiment 34: present embodiment and embodiment one to hentriaconta-different be that temperature is 500 ℃ in the step 7.Other step and parameter are identical to hentriaconta-with embodiment one.
Embodiment 35: present embodiment TiO
2The preparation method of nano-pipe array thin film realizes according to the following steps: one, the titanium plate is cut into two titanium sheets that are of a size of 25mm * 10mm, then two titanium sheets are polished, then put into acetone supersound process 30min, use distilled water flushing then 4 times; Two, the Neutral ammonium fluoride that takes by weighing 1.0g is dissolved in the distilled water of 8mL, and the ethylene glycol with 150mL mixes then, makes electrolytic solution; Three, in the electrolytic solution that will make through the parallel immersion step 2 of two titanium sheets that step 1 is handled at ambient temperature, a slice is an anode, and another sheet is a negative electrode, applies the voltage of 50V, then electrolysis treatment 30min; Four, take out as anodic titanium sheet, putting into concentration is the dilute nitric acid solution supersound process 10min of 1.5mol/L, uses distilled water flushing then 4 times; Five, as anode, apply the voltage of 60V, then electrolysis treatment 26h in the freshly prepd electrolytic solution of step 4 being handled of titanium sheet immersion step 2; Six, take out as anodic titanium sheet, put into ethanol supersound process 10min, dry naturally; Seven, the titanium sheet after will drying is put into retort furnace, is that calcination processing 3h cools to room temperature with the furnace, promptly obtains TiO under 500 ℃ the condition in temperature
2Nano-pipe array thin film.
Adopt the TiO of present embodiment preparation
2Nano-pipe array thin film, TiO
2The scanning electron microscope analysis figure of nano-pipe array thin film as shown in Figure 1.TiO
2The nano-pipe array thin film surface presents state smooth, the diameter homogeneous, diameter is about 110nm, and length is about 90 μ m.
Adopt the preparation of inorganic electrolyte liquid nano-pipe array thin film stereoscan photograph as shown in Figure 2, as can be seen from Figure 2, that film surface presents is coarse, diameter is inhomogeneous.Adopt the organic electrolyte preparation nano-pipe array thin film stereoscan photograph as shown in Figure 3, as can be seen from Figure 3, that film surface presents is coarse, diameter is inhomogeneous.
Claims (10)
1, a kind of TiO
2The preparation method of nano-pipe array thin film is characterized in that TiO
2The preparation method of nano-pipe array thin film realizes according to the following steps: one, the titanium plate is cut into two measure-alike titanium sheets, then two titanium sheets are polished, then put into acetone supersound process 10～60min, use distilled water flushing then 3～5 times; Two, the Neutral ammonium fluoride that takes by weighing 0.5～1.5g is dissolved in the distilled water of 4～10mL, and ethylene glycol or the glycerol with 100～200mL mixes then, makes electrolytic solution; Three, in the electrolytic solution that will make through the parallel immersion step 2 of two titanium sheets that step 1 is handled at ambient temperature, a slice is an anode, and another sheet is a negative electrode, applies the voltage of 20～70V, then electrolysis treatment 20～60min; Four, take out as anodic titanium sheet, put into dilute acid soln supersound process 5～30min, use distilled water flushing then 3～5 times; Five, as anode, apply the voltage of 20～60V, then electrolysis treatment 0.5～72h in the freshly prepd electrolytic solution of step 4 being handled of titanium sheet immersion step 2; Six, take out as anodic titanium sheet, put into ethanol supersound process 5～20min, dry naturally; Seven, the titanium sheet after will drying is put into retort furnace, is that calcination processing 2～5h cools to room temperature with the furnace, promptly obtains TiO under 300～700 ℃ the condition in temperature
2Nano-pipe array thin film; Wherein dilute acid soln is dilution heat of sulfuric acid, dilute nitric acid solution or dilute hydrochloric acid solution in the step 4.
2, a kind of TiO according to claim 1
2The preparation method of nano-pipe array thin film is characterized in that two titanium sheets are of a size of 25mm * 10mm in the step 1.
3, a kind of TiO according to claim 1 and 2
2The preparation method of nano-pipe array thin film is characterized in that adopting 50～300Cw water-proof abrasive paper, 500～1000Cw water-proof abrasive paper and 1500～2500Cw water-proof abrasive paper to polish respectively to two titanium sheets in the step 1.
4, a kind of TiO according to claim 3
2The preparation method of nano-pipe array thin film is characterized in that ultrasonic frequency is that 30～60kHz, power are 150～200W in the step 1.
5, according to claim 1,2 or 4 described a kind of TiO
2The preparation method of nano-pipe array thin film is characterized in that the Neutral ammonium fluoride that takes by weighing 0.6～1.2g in the step 2 is dissolved in the distilled water of 5～9mL, and ethylene glycol or the glycerol with 120～180mL mixes then.
6, a kind of TiO according to claim 5
2The preparation method of nano-pipe array thin film is characterized in that the voltage that applies in the step 3 is 30～60V.
7, according to claim 1,2,4 or 6 described a kind of TiO
2The preparation method of nano-pipe array thin film, the volumetric molar concentration that it is characterized in that dilute acid soln in the step 4 is 0.5～3mol/L.
8, a kind of TiO according to claim 7
2The preparation method of nano-pipe array thin film is characterized in that the voltage that applies in the step 5 is 30～50V.
9, according to claim 1,2,4,6 or 8 described a kind of TiO
2The preparation method of nano-pipe array thin film is characterized in that ultrasonic frequency is that 30～60kHz, power are 80～100W in the step 6.
10, a kind of TiO according to claim 9
2The preparation method of nano-pipe array thin film is characterized in that calcination processing 3～4h in the step 7.
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