CN102795665A - Preparation method of titanium dioxide nanotube (rod) array - Google Patents
Preparation method of titanium dioxide nanotube (rod) array Download PDFInfo
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- CN102795665A CN102795665A CN2012103106475A CN201210310647A CN102795665A CN 102795665 A CN102795665 A CN 102795665A CN 2012103106475 A CN2012103106475 A CN 2012103106475A CN 201210310647 A CN201210310647 A CN 201210310647A CN 102795665 A CN102795665 A CN 102795665A
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Abstract
The invention discloses a preparation method of a titanium dioxide nanotube (rod) array. A wet chemical method is adopted in the whole preparation process. The preparation method comprises the following steps of: firstly, preparing a zinc oxide seed crystal layer on conductive glass by using a sol-gel method; then, growing a zinc oxide nanorod array template on the seed crystal layer by using a liquid phase deposition method; and then, converting the zinc oxide nanorod array template into a titanium dioxide nanotube (rod) array by using the liquid phase deposition method to obtain a one-dimensional titanium dioxide nanotube (rod) array. The preparation method has the advantages that (1) compared with other methods such as an anodic oxidation method, the method is simple in process, free of complex equipment and severe environment and capable of preparing the titanium dioxide nanotube (rod) array on the conductive glass directly; and (2) the method can be used for conveniently controlling the diameter and the length of a zinc oxide nanowire and the thickness of a titanium dioxide shell layer.
Description
Technical field
The present invention relates to a kind of preparation method of nano-array, be specifically related to the preparation method of a kind of titania nanotube (bar) array.
Background technology
Solar cell can directly become electric energy with solar energy converting, is considered to a kind of mode of the most effectively utilizing sun power, therefore receives countries in the world all the time and pays much attention to.The solar cell of practical application at present mainly is a silica-based solar cell, and it has higher efficient and stable preferably, but its high manufacturing cost has limited its large-scale application.Therefore the researchist is except carry out trying to explore novel solar battery more low cost, the high-level efficiency silica-based solar cell commercialization technological improvement on the one hand.In numerous solar cells, organic inorganic composite solar battery had both had the low cost that machine battery is arranged, and had no machine battery advantages of higher stability again, therefore received the researchist and extensively paid attention to.
Organic inorganic composite solar battery mainly is made up of the inorganic carrying semiconductor material of wide taboo (like zinc oxide, titanium oxide) and organic light absorbing material (like P3HT etc.).Present applied semiconductor material with wide forbidden band mainly is the nanostructure of zinc oxide, titanium oxide, comprises nanometer ball, nano-porous films, nanostructures such as one-dimensional nano line, nano rod, nanotube (bar) array.In these nanostructures; One-dimensional nano-array is particularly noticeable; Because they have following several characteristics: (1) can provide directly transmission path fast for photo-generated carrier, thereby helps reducing the compound of photo-generated carrier, promotes it to be collected by outer electrode fast; (2) since the strong scattering of light of nano-array with capture effect, can reduce the light anode to reflection of light, increase is to the absorption of sunshine.(3) vertical channel in the nano-array helps the infiltration of organism in array, thereby organism is fully contacted with inorganics.Therefore, how to prepare the one-dimensional nano-array that is applicable to organic inorganic composite solar battery and just seem particularly important.
Titania nanotube (bar) array is a kind of very important nanostructure, and it is widely used in the research of novel solar batteries such as dye sensitization solar battery, quantum dot sensitized sun power.Anonizing is the most frequently used, the easiest method of preparation Nano tube array of titanium dioxide.But the Nano tube array of titanium dioxide of this method preparation is unfavorable for the application on organic inorganic composite solar battery attached on the titanium foil.In order to be applied to organic inorganic composite solar battery, a kind of domestic method is the metal titanium membrane of preparation one deck suitable thickness on conductive glass, and then adopts anonizing that titanium film is oxidized to Nano tube array of titanium dioxide.But this method complex procedures, and need utilize vacuum coating film equipment, cost is too high, therefore is inappropriate for large-scale application.Therefore, develop simplely, do not need the low-cost preparation of complex apparatus Nano tube array of titanium dioxide method just to seem particularly important.
Summary of the invention
The preparation method who the purpose of this invention is to provide the simple titania nanotube of a kind of technology (bar) array.
For achieving the above object, the preparation method that the present invention adopts is:
1) at first be dissolved in the ammonium titanium fluoride of 8～10 mmoles and the boric acid of 18～22 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to 100 milliliters after mixing and get mixing solutions, cleaner ITO conductive glass substrate is immersed in the mixing solutions, rinse well with deionized water then; Dry up, on ITO conductive glass substrate, make the titanium oxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds two hydration zinc acetates of 1～16 mmole, making the monoethanolamine and the ratio of the amount of substance of zine ion is 1: 1; Then with mixture sealing and place 58～62 ℃ water-bath magnetic agitation evenly to obtain zinc oxide colloidal sol; With at room temperature leaving standstill 12～18 hours after the taking-up of zinc oxide colloidal sol; Utilize spin coating technology the zinc oxide colloidal sol after above-mentioned the leaving standstill to be spin-coated on the ITO conductive glass substrate for preparing the titanium oxide pretreatment layer with 3000 rev/mins; Place it in then in 195～205 ℃ the baking oven and handled 5～10 minutes; Place 450～500 ℃ retort furnace to handle 0.5～1 hour ITO conductive glass substrate again, obtain the zinc oxide inculating crystal layer;
3) with the zinc nitrate hexahydrate of 4 mmoles; The sodium hydroxide of 80 mmoles is dissolved in the deionized water respectively; Then zinc nitrate solution is poured in the sodium hydroxide solution and mixed, in volumetric flask, be settled to 100 milliliters again, mix and obtain growth media; The ITO conductive glass substrate that is coated with the zinc oxide inculating crystal layer that will prepare then immerses in the growth media grew 5～20 minutes in 80 ℃ of water-baths; Then ITO conductive glass substrate is taken out, rinse well, dry up, obtain zinc oxide nano-wire array with deionized water;
4) be dissolved in the ammonium titanium fluoride of 5～7.5 mmoles and the boric acid of 15～20 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to 100 milliliters after mixing and process deposit fluid; To prepare then has the ITO of zinc oxide nano-wire array conductive glass substrate to immerse in the deposit fluid, then with its taking-up, rinses well, dries up with deionized water; Place 400～450 degrees centigrade retort furnace to handle 1 hour gained ITO conductive glass substrate, promptly obtain titania nanotube (bar) array of crystallization.
The ITO conductive glass substrate that said step 3) is coated with the zinc oxide inculating crystal layer faces down the zinc oxide inculating crystal layer with in the 60 degree angles immersion growth media.
Said step 3) is through the length of control growing time controlled oxidation zinc nano wire.
Said step 4) preparation has the ITO conductive glass substrate of zinc oxide nano-wire array that facing down of zinc oxide nano-wire array immersed in the deposit fluid with 60 degree angles.
The present invention all adopts wet chemistry method to prepare titania nanotube (bar) array; Comprise that mainly liquid phase deposition prepares the titanium oxide pretreatment layer; Prepared by Sol Gel Method zinc oxide inculating crystal layer; Liquid phase deposition prepares zinc oxide nano-wire array, and liquid phase deposition prepares titania nanotube (bar) array.Whole process has experimental installation, environmental requirement is low, and technological process is simple, characteristics such as good reproducibility.The method that the present invention proposes is easy to control the pattern parameter of nanotube (bar) array, such as can be through control liquid deposition time controlled oxidation zinc nano rod template length, thus the length of control gained titania nanotube (bar).
Description of drawings
Fig. 1 is the sem photograph of Zinc oxide nano-rod array mould plate;
Fig. 2 is the sem photograph of titanium oxide nanotubes (bar) array;
Fig. 3 is the X-ray diffractogram of Zinc oxide nano-rod array mould plate and titania nanotube (bar) array.
Embodiment
Below in conjunction with accompanying drawing the present invention is explained further details.
Embodiment 1:
1) at first be dissolved in the ammonium titanium fluoride of 10 mmoles and the boric acid of 20 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to after mixing 100 milliliters mixing solutions, cleaner ITO conductive glass substrate was at room temperature immersed in the mixing solutions 30 minutes, rinse well with deionized water then; Dry up, on ITO conductive glass substrate, make the titanium oxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds two hydration zinc acetates of 10 mmoles, making the monoethanolamine and the ratio of the amount of substance of zine ion is 1: 1; Then with mixture sealing and place 60 ℃ water-bath magnetic agitation evenly to obtain zinc oxide colloidal sol; With at room temperature leaving standstill 12 hours after the taking-up of zinc oxide colloidal sol; Utilize spin coating technology the zinc oxide colloidal sol after above-mentioned the leaving standstill to be spin-coated on the ITO conductive glass substrate for preparing the titanium oxide pretreatment layer with 3000 rev/mins; Place it in then in 200 ℃ the baking oven and handled 5 minutes; Place 500 ℃ retort furnace to handle 1 hour ITO conductive glass substrate again, obtain the zinc oxide inculating crystal layer;
3) with the zinc nitrate hexahydrate of 4 mmoles; The sodium hydroxide of 80 mmoles is dissolved in the deionized water respectively; Then zinc nitrate solution is poured in the sodium hydroxide solution and mixed, in volumetric flask, be settled to 100 milliliters again, mix and obtain growth media; The ITO conductive glass substrate that is coated with the zinc oxide inculating crystal layer that will prepare then faces down the zinc oxide inculating crystal layer in 80 ℃ of water-baths, to grow 10 minutes in the 60 degree angles immersion growth media; Then ITO conductive glass substrate is taken out, rinse well, dry up, obtain zinc oxide nano-wire array with deionized water; Shown in accompanying drawing 1.
4) be dissolved in the ammonium titanium fluoride of 5 mmoles and the boric acid of 15 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to 100 milliliters after mixing and process deposit fluid; To prepare then has the ITO of zinc oxide nano-wire array conductive glass substrate that facing down of zinc oxide nano-wire array immersed in the deposit fluid with 60 degree angles, with its taking-up, rinses well, dries up with deionized water after 10 minutes; Place 450 degrees centigrade retort furnace to handle 1 hour gained ITO conductive glass substrate, promptly obtain titania nanotube (bar) array of crystallization.Its surface topography is shown in accompanying drawing 2, and X ray diffracting spectrum is shown in accompanying drawing 3.
Embodiment 2:
1) at first be dissolved in the ammonium titanium fluoride of 9 mmoles and the boric acid of 20 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to after mixing 100 milliliters mixing solutions, cleaner ITO conductive glass substrate was at room temperature immersed in the mixing solutions 30 minutes, rinse well with deionized water then; Dry up, on ITO conductive glass substrate, make the titanium oxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds two hydration zinc acetates of 1 mmole, making the monoethanolamine and the ratio of the amount of substance of zine ion is 1: 1; Then with mixture sealing and place 58 ℃ water-bath magnetic agitation evenly to obtain zinc oxide colloidal sol; With at room temperature leaving standstill 15 hours after the taking-up of zinc oxide colloidal sol; Utilize spin coating technology the zinc oxide colloidal sol after above-mentioned the leaving standstill to be spin-coated on the ITO conductive glass substrate for preparing the titanium oxide pretreatment layer with 3000 rev/mins; Place it in then in 195 ℃ the baking oven and handled 10 minutes; Place 480 ℃ retort furnace to handle 1 hour ITO conductive glass substrate again, obtain the zinc oxide inculating crystal layer;
3) with the zinc nitrate hexahydrate of 4 mmoles; The sodium hydroxide of 80 mmoles is dissolved in the deionized water respectively; Then zinc nitrate solution is poured in the sodium hydroxide solution and mixed, in volumetric flask, be settled to 100 milliliters again, mix and obtain growth media; The ITO conductive glass substrate that is coated with the zinc oxide inculating crystal layer that will prepare then faces down the zinc oxide inculating crystal layer in 80 ℃ of water-baths, to grow 15 minutes in the 60 degree angles immersion growth media; Then ITO conductive glass substrate is taken out, rinse well, dry up, obtain zinc oxide nano-wire array with deionized water;
4) be dissolved in the ammonium titanium fluoride of 7.5 mmoles and the boric acid of 20 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to 100 milliliters after mixing and process deposit fluid; To prepare then has the ITO of zinc oxide nano-wire array conductive glass substrate that facing down of zinc oxide nano-wire array immersed in the deposit fluid with 60 degree angles, with its taking-up, rinses well, dries up with deionized water after 10 minutes; Place 430 degrees centigrade retort furnace to handle 1 hour gained ITO conductive glass substrate, promptly obtain titania nanotube (bar) array of crystallization.
Embodiment 3:
1) at first be dissolved in the ammonium titanium fluoride of 8 mmoles and the boric acid of 18 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to after mixing 100 milliliters mixing solutions, cleaner ITO conductive glass substrate was at room temperature immersed in the mixing solutions 30 minutes, rinse well with deionized water then; Dry up, on ITO conductive glass substrate, make the titanium oxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds two hydration zinc acetates of 5 mmoles, making the monoethanolamine and the ratio of the amount of substance of zine ion is 1: 1; Then with mixture sealing and place 60 ℃ water-bath magnetic agitation evenly to obtain zinc oxide colloidal sol; With at room temperature leaving standstill 18 hours after the taking-up of zinc oxide colloidal sol; Utilize spin coating technology the zinc oxide colloidal sol after above-mentioned the leaving standstill to be spin-coated on the ITO conductive glass substrate for preparing the titanium oxide pretreatment layer with 3000 rev/mins; Place it in then in 200 ℃ the baking oven and handled 8 minutes; Place 500 ℃ retort furnace to handle 0.5 hour ITO conductive glass substrate again, obtain the zinc oxide inculating crystal layer;
3) with the zinc nitrate hexahydrate of 4 mmoles; The sodium hydroxide of 80 mmoles is dissolved in the deionized water respectively; Then zinc nitrate solution is poured in the sodium hydroxide solution and mixed, in volumetric flask, be settled to 100 milliliters again, mix and obtain growth media; The ITO conductive glass substrate that is coated with the zinc oxide inculating crystal layer that will prepare then faces down the zinc oxide inculating crystal layer in 80 ℃ of water-baths, to grow 5 minutes in the 60 degree angles immersion growth media; Then ITO conductive glass substrate is taken out, rinse well, dry up, obtain zinc oxide nano-wire array with deionized water;
4) be dissolved in the ammonium titanium fluoride of 6 mmoles and the boric acid of 18 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to 100 milliliters after mixing and process deposit fluid; To prepare then has the ITO of zinc oxide nano-wire array conductive glass substrate that facing down of zinc oxide nano-wire array immersed in the deposit fluid with 60 degree angles, with its taking-up, rinses well, dries up with deionized water after 5 minutes; Place 400 degrees centigrade retort furnace to handle 1 hour gained ITO conductive glass substrate, promptly obtain titania nanotube (bar) array of crystallization.
Embodiment 4:
1) at first be dissolved in the ammonium titanium fluoride of 10 mmoles and the boric acid of 22 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to after mixing 100 milliliters mixing solutions, cleaner ITO conductive glass substrate was at room temperature immersed in the mixing solutions 30 minutes, rinse well with deionized water then; Dry up, on ITO conductive glass substrate, make the titanium oxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds two hydration zinc acetates of 16 mmoles, making the monoethanolamine and the ratio of the amount of substance of zine ion is 1: 1; Then with mixture sealing and place 62 ℃ water-bath magnetic agitation evenly to obtain zinc oxide colloidal sol; With at room temperature leaving standstill 12 hours after the taking-up of zinc oxide colloidal sol; Utilize spin coating technology the zinc oxide colloidal sol after above-mentioned the leaving standstill to be spin-coated on the ITO conductive glass substrate for preparing the titanium oxide pretreatment layer with 3000 rev/mins; Place it in then in 205 ℃ the baking oven and handled 5 minutes; Place 450 ℃ retort furnace to handle 1 hour ITO conductive glass substrate again, obtain the zinc oxide inculating crystal layer;
3) with the zinc nitrate hexahydrate of 4 mmoles; The sodium hydroxide of 80 mmoles is dissolved in the deionized water respectively; Then zinc nitrate solution is poured in the sodium hydroxide solution and mixed, in volumetric flask, be settled to 100 milliliters again, mix and obtain growth media; The ITO conductive glass substrate that is coated with the zinc oxide inculating crystal layer that will prepare then faces down the zinc oxide inculating crystal layer in 80 ℃ of water-baths, to grow 20 minutes in the 60 degree angles immersion growth media; Then ITO conductive glass substrate is taken out, rinse well, dry up, obtain zinc oxide nano-wire array with deionized water;
4) be dissolved in the ammonium titanium fluoride of 7.5 mmoles and the boric acid of 20 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to 100 milliliters after mixing and process deposit fluid; To prepare then has the ITO of zinc oxide nano-wire array conductive glass substrate that facing down of zinc oxide nano-wire array immersed in the deposit fluid with 60 degree angles, with its taking-up, rinses well, dries up with deionized water after 10 minutes; Place 450 degrees centigrade retort furnace to handle 1 hour gained ITO conductive glass substrate, promptly obtain titania nanotube (bar) array of crystallization.
Claims (4)
1. the preparation method of titania nanotube (bar) array is characterized in that:
1) at first be dissolved in the ammonium titanium fluoride of 8～10 mmoles and the boric acid of 18～22 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to 100 milliliters after mixing and get mixing solutions, cleaner ITO conductive glass substrate is immersed in the mixing solutions, rinse well with deionized water then; Dry up, on ITO conductive glass substrate, make the titanium oxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds two hydration zinc acetates of 1～16 mmole, making the monoethanolamine and the ratio of the amount of substance of zine ion is 1: 1; Then with mixture sealing and place 58～62 ℃ water-bath magnetic agitation evenly to obtain zinc oxide colloidal sol; With at room temperature leaving standstill 12～18 hours after the taking-up of zinc oxide colloidal sol; Utilize spin coating technology the zinc oxide colloidal sol after above-mentioned the leaving standstill to be spin-coated on the ITO conductive glass substrate for preparing the titanium oxide pretreatment layer with 3000 rev/mins; Place it in then in 195～205 ℃ the baking oven and handled 5～10 minutes; Place 450～500 ℃ retort furnace to handle 0.5～1 hour ITO conductive glass substrate again, obtain the zinc oxide inculating crystal layer;
3) with the zinc nitrate hexahydrate of 4 mmoles; The sodium hydroxide of 80 mmoles is dissolved in the deionized water respectively; Then zinc nitrate solution is poured in the sodium hydroxide solution and mixed, in volumetric flask, be settled to 100 milliliters again, mix and obtain growth media; The ITO conductive glass substrate that is coated with the zinc oxide inculating crystal layer that will prepare then immerses in the growth media grew 5～20 minutes in 80 ℃ of water-baths; Then ITO conductive glass substrate is taken out, rinse well, dry up, obtain zinc oxide nano-wire array with deionized water;
4) be dissolved in the ammonium titanium fluoride of 5～7.5 mmoles and the boric acid of 15～20 mmoles in the deionized water respectively; Then BAS is poured in the ammonium titanium fluoride solution; Be settled to 100 milliliters after mixing and process deposit fluid; To prepare then has the ITO of zinc oxide nano-wire array conductive glass substrate to immerse in the deposit fluid, then with its taking-up, rinses well, dries up with deionized water; Place 400～450 degrees centigrade retort furnace to handle 1 hour gained ITO conductive glass substrate, promptly obtain titania nanotube (bar) array of crystallization.
2. the preparation method of titania nanotube according to claim 1 (bar) array is characterized in that: the ITO conductive glass substrate that said step 3) is coated with the zinc oxide inculating crystal layer faces down the zinc oxide inculating crystal layer with in the 60 degree angles immersion growth media.
3. the preparation method of titania nanotube according to claim 1 (bar) array is characterized in that: said step 3) is through the length of control growing time controlled oxidation zinc nano wire.
4. the preparation method of titania nanotube according to claim 1 (bar) array is characterized in that: said step 4) preparation has the ITO conductive glass substrate of zinc oxide nano-wire array that facing down of zinc oxide nano-wire array immersed in the deposit fluid with 60 degree angles.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103464162A (en) * | 2013-09-03 | 2013-12-25 | 万华化学集团股份有限公司 | Preparation method and application of Co and Al2O3 compound nanotube array membrane catalyst |
| CN105642314A (en) * | 2016-01-18 | 2016-06-08 | 武汉理工大学 | Cadmium sulfide and zinc oxide core-shell multilayer nanorod array photocatalytic material and preparation method thereof |
| CN111599887A (en) * | 2020-05-23 | 2020-08-28 | 苏州镓敏光电科技有限公司 | Ultraviolet detector and preparation method thereof |
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| CN101649483A (en) * | 2008-08-12 | 2010-02-17 | 中国科学院理化技术研究所 | Method for preparing titanium dioxide nanorod array film |
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| CN101649483A (en) * | 2008-08-12 | 2010-02-17 | 中国科学院理化技术研究所 | Method for preparing titanium dioxide nanorod array film |
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| 《Nanotechnology》 20061231 Jijun Qiu, et al. Sol-gel assisted ZnO nanorod array template to synthesize TiO2 nanotube arrays 第4696页左栏第2段至第右栏第3段及图1 1-4 , * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103464162A (en) * | 2013-09-03 | 2013-12-25 | 万华化学集团股份有限公司 | Preparation method and application of Co and Al2O3 compound nanotube array membrane catalyst |
| CN105642314A (en) * | 2016-01-18 | 2016-06-08 | 武汉理工大学 | Cadmium sulfide and zinc oxide core-shell multilayer nanorod array photocatalytic material and preparation method thereof |
| CN105642314B (en) * | 2016-01-18 | 2019-01-25 | 武汉理工大学 | A kind of cadmium sulfide-zinc oxide nucleocapsid multi-layer nano stick array photo catalysis material and preparation method thereof |
| CN111599887A (en) * | 2020-05-23 | 2020-08-28 | 苏州镓敏光电科技有限公司 | Ultraviolet detector and preparation method thereof |
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