CN102795665B - Preparation method of titanium dioxide nanotube (rod) array - Google Patents
Preparation method of titanium dioxide nanotube (rod) array Download PDFInfo
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- CN102795665B CN102795665B CN201210310647.5A CN201210310647A CN102795665B CN 102795665 B CN102795665 B CN 102795665B CN 201210310647 A CN201210310647 A CN 201210310647A CN 102795665 B CN102795665 B CN 102795665B
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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 convert solar energy to electric energy, is considered to a kind of mode of the most effectively utilizing solar energy, is therefore subject to countries in the world all the time and pays much attention to.The solar cell of practical application is at present mainly silica-based solar cell, and it has higher efficiency and good stability, but its high manufacturing cost has limited its large-scale application.Therefore researcher is except carrying out, low cost, high efficiency silica-based solar cell commercialization technological improvement, more trying to explore novel solar battery on the one hand.In numerous solar cells, organic inorganic composite solar battery had both had the low cost of organic battery, had again without the higher stability of machine battery, was therefore subject to researcher and extensively paid attention to.
Organic inorganic composite solar battery is mainly comprised of the inorganic carrying semiconductor material of wide taboo (as zinc oxide, titanium oxide) and organic light absorbing material (as P3HT etc.).Current applied semiconductor material with wide forbidden band is mainly the nanostructure of zinc oxide, titanium oxide, comprises nanosphere, nano-porous films, the 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 feature: (1) can provide directly transmission channel fast for photo-generated carrier, thereby be conducive to reduce the compound of photo-generated carrier, promote it by external electrode, to be collected fast; (2) due to the strong light scattering of nano-array with capture effect, can reduce light anode to reflection of light, increase the absorption to sunlight.(3) vertical channel in nano-array is conducive to the infiltration of organic substance in array, thereby organic substance is fully contacted with inorganic matter.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 the novel solar batteries such as DSSC, quantum dot sensitized solar energy.Anode oxidation method is to prepare the most frequently used, the easiest method of Nano tube array of titanium dioxide.But Nano tube array of titanium dioxide prepared by this method is attached on titanium foil, be unfavorable for the application on organic inorganic composite solar battery.In order to be applied to organic inorganic composite solar battery, a kind of common method is on electro-conductive glass, to prepare the metal titanium membrane of one deck suitable thickness, and then adopts anode oxidation method that titanium film is oxidized to Nano tube array of titanium dioxide.But this method complex procedures, and need to utilize vacuum coating equipment, cost is too high, is therefore unsuitable for large-scale application.Therefore, develop simplely, do not need complex device low cost to prepare Nano tube array of titanium dioxide method and just seem particularly important.
Summary of the invention
The preparation method who the object of this invention is to provide the simple titania nanotube of a kind of technique (bar) array.
For achieving the above object, the preparation method that the present invention adopts is:
1) first the boric acid of the ammonium titanium fluoride of 8～10 mMs and 18～22 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and obtain mixed solution, again clean ITO electro-conductive glass substrate is immersed in mixed solution, then with deionized water, rinse well, dry up, on ITO electro-conductive glass substrate, make titanium dioxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds the two hydration zinc acetates of 1～16 mM, making monoethanolamine and the ratio of the amount of substance of zinc ion is 1: 1; Then the water-bath magnetic agitation that mixture is sealed and is placed in 58～62 ℃ evenly obtains zinc oxide colloidal sol, after zinc oxide colloidal sol is taken out at room temperature standing 12～18 hours, utilize spin coating technique with 3000 revs/min, above-mentioned zinc oxide colloidal sol after standing to be spin-coated on the ITO electro-conductive glass substrate of preparing titanium dioxide pretreatment layer, then place it in the baking oven of 195～205 ℃ and process 5～10 minutes, the Muffle furnace that ITO electro-conductive glass substrate is placed in to 450～500 ℃ is again processed 0.5～1 hour, obtains zinc oxide inculating crystal layer;
3) by the zinc nitrate hexahydrate of 4 mMs, the NaOH of 80 mMs is dissolved in respectively in deionized water, then zinc nitrate solution is poured in sodium hydroxide solution and mixed, in volumetric flask, be settled to again 100 milliliters, mix and obtain growth-promoting media, then the ITO electro-conductive glass substrate that is coated with zinc oxide inculating crystal layer of having prepared is immersed in growth-promoting media and grown 5～20 minutes in 80 ℃ of water-baths, then ITO electro-conductive glass substrate is taken out, with deionized water, rinse well, dry up, obtain zinc oxide nano-wire array;
4) boric acid of the ammonium titanium fluoride of 5～7.5 mMs and 15～20 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and make deposit fluid, then will be prepared with in the ITO electro-conductive glass substrate immersion deposition liquid of zinc oxide nano-wire array, then by its taking-up, with deionized water, rinse well, dry up, the Muffle furnace that gained ITO electro-conductive glass substrate is placed in to 400～450 degrees Celsius is processed 1 hour, obtains titania nanotube (bar) array of crystallization.
The ITO electro-conductive glass substrate that described step 3) is coated with zinc oxide inculating crystal layer faces down zinc oxide inculating crystal layer to immerse in growth-promoting media with 60 degree angles.
Described step 3) is controlled the length of zinc oxide nanowire by controlling growth time.
Described step 4) is prepared with ITO electro-conductive glass substrate the facing down with in 60 degree angle immersion deposition liquid zinc oxide nano-wire array of zinc oxide nano-wire array.
The present invention all adopts wet chemistry method to prepare titania nanotube (bar) array, mainly comprise that liquid phase deposition prepares titanium dioxide pretreatment layer, sol-gal process is prepared zinc oxide inculating crystal layer, liquid phase deposition is prepared zinc oxide nano-wire array, and liquid phase deposition is prepared titania nanotube (bar) array.The features such as whole process has experimental facilities, environmental requirement is low, and technical process is simple, reproducible.The method that the present invention proposes is easy to control the pattern parameter of nanotube (bar) array, such as controlling Zinc oxide nano-rod template length by controlling the liquid deposition time, thereby controls the length of gained titania nanotube (bar).
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of Zinc oxide nano-rod array mould plate;
Fig. 2 is the scanning electron microscope (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 described in further details.
Embodiment 1:
1) first the boric acid of the ammonium titanium fluoride of 10 mMs and 20 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and obtain mixed solution, again clean ITO electro-conductive glass substrate is at room temperature immersed in mixed solution 30 minutes, then with deionized water, rinse well, dry up, on ITO electro-conductive glass substrate, make titanium dioxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds the two hydration zinc acetates of 10 mMs, making monoethanolamine and the ratio of the amount of substance of zinc ion is 1: 1; Then the water-bath magnetic agitation that mixture is sealed and is placed in 60 ℃ evenly obtains zinc oxide colloidal sol, after zinc oxide colloidal sol is taken out at room temperature standing 12 hours, utilize spin coating technique with 3000 revs/min, above-mentioned zinc oxide colloidal sol after standing to be spin-coated on the ITO electro-conductive glass substrate of preparing titanium dioxide pretreatment layer, then place it in the baking oven of 200 ℃ and process 5 minutes, the Muffle furnace that ITO electro-conductive glass substrate is placed in to 500 ℃ is again processed 1 hour, obtains zinc oxide inculating crystal layer;
3) by the zinc nitrate hexahydrate of 4 mMs, the NaOH of 80 mMs is dissolved in respectively in deionized water, then zinc nitrate solution is poured in sodium hydroxide solution and mixed, in volumetric flask, be settled to again 100 milliliters, mix and obtain growth-promoting media, then the ITO electro-conductive glass substrate that is coated with zinc oxide inculating crystal layer of having prepared is faced down zinc oxide inculating crystal layer to immerse in growth-promoting media and grow 10 minutes in 80 ℃ of water-baths with 60 degree angles, then ITO electro-conductive glass substrate is taken out, with deionized water, rinse well, dry up, obtain zinc oxide nano-wire array; As shown in Figure 1.
4) boric acid of the ammonium titanium fluoride of 5 mMs and 15 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and make deposit fluid, then ITO electro-conductive glass substrate the facing down with in 60 degree angle immersion deposition liquid zinc oxide nano-wire array of zinc oxide nano-wire array will be prepared with, after 10 minutes by its taking-up, with deionized water, rinse well, dry up, the Muffle furnace that gained ITO electro-conductive glass substrate is placed in to 450 degrees Celsius is processed 1 hour, obtain titania nanotube (bar) array of crystallization.As shown in Figure 2, X ray diffracting spectrum as shown in Figure 3 for its surface topography.
Embodiment 2:
1) first the boric acid of the ammonium titanium fluoride of 9 mMs and 20 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and obtain mixed solution, again clean ITO electro-conductive glass substrate is at room temperature immersed in mixed solution 30 minutes, then with deionized water, rinse well, dry up, on ITO electro-conductive glass substrate, make titanium dioxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds the two hydration zinc acetates of 1 mM, making monoethanolamine and the ratio of the amount of substance of zinc ion is 1: 1; Then the water-bath magnetic agitation that mixture is sealed and is placed in 58 ℃ evenly obtains zinc oxide colloidal sol, after zinc oxide colloidal sol is taken out at room temperature standing 15 hours, utilize spin coating technique with 3000 revs/min, above-mentioned zinc oxide colloidal sol after standing to be spin-coated on the ITO electro-conductive glass substrate of preparing titanium dioxide pretreatment layer, then place it in the baking oven of 195 ℃ and process 10 minutes, the Muffle furnace that ITO electro-conductive glass substrate is placed in to 480 ℃ is again processed 1 hour, obtains zinc oxide inculating crystal layer;
3) by the zinc nitrate hexahydrate of 4 mMs, the NaOH of 80 mMs is dissolved in respectively in deionized water, then zinc nitrate solution is poured in sodium hydroxide solution and mixed, in volumetric flask, be settled to again 100 milliliters, mix and obtain growth-promoting media, then the ITO electro-conductive glass substrate that is coated with zinc oxide inculating crystal layer of having prepared is faced down zinc oxide inculating crystal layer to immerse in growth-promoting media and grow 15 minutes in 80 ℃ of water-baths with 60 degree angles, then ITO electro-conductive glass substrate is taken out, with deionized water, rinse well, dry up, obtain zinc oxide nano-wire array;
4) boric acid of the ammonium titanium fluoride of 7.5 mMs and 20 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and make deposit fluid, then ITO electro-conductive glass substrate the facing down with in 60 degree angle immersion deposition liquid zinc oxide nano-wire array of zinc oxide nano-wire array will be prepared with, after 10 minutes by its taking-up, with deionized water, rinse well, dry up, the Muffle furnace that gained ITO electro-conductive glass substrate is placed in to 430 degrees Celsius is processed 1 hour, obtain titania nanotube (bar) array of crystallization.
Embodiment 3:
1) first the boric acid of the ammonium titanium fluoride of 8 mMs and 18 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and obtain mixed solution, again clean ITO electro-conductive glass substrate is at room temperature immersed in mixed solution 30 minutes, then with deionized water, rinse well, dry up, on ITO electro-conductive glass substrate, make titanium dioxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds the two hydration zinc acetates of 5 mMs, making monoethanolamine and the ratio of the amount of substance of zinc ion is 1: 1; Then the water-bath magnetic agitation that mixture is sealed and is placed in 60 ℃ evenly obtains zinc oxide colloidal sol, after zinc oxide colloidal sol is taken out at room temperature standing 18 hours, utilize spin coating technique with 3000 revs/min, above-mentioned zinc oxide colloidal sol after standing to be spin-coated on the ITO electro-conductive glass substrate of preparing titanium dioxide pretreatment layer, then place it in the baking oven of 200 ℃ and process 8 minutes, the Muffle furnace that ITO electro-conductive glass substrate is placed in to 500 ℃ is again processed 0.5 hour, obtains zinc oxide inculating crystal layer;
3) by the zinc nitrate hexahydrate of 4 mMs, the NaOH of 80 mMs is dissolved in respectively in deionized water, then zinc nitrate solution is poured in sodium hydroxide solution and mixed, in volumetric flask, be settled to again 100 milliliters, mix and obtain growth-promoting media, then the ITO electro-conductive glass substrate that is coated with zinc oxide inculating crystal layer of having prepared is faced down zinc oxide inculating crystal layer to immerse in growth-promoting media and grow 5 minutes in 80 ℃ of water-baths with 60 degree angles, then ITO electro-conductive glass substrate is taken out, with deionized water, rinse well, dry up, obtain zinc oxide nano-wire array;
4) boric acid of the ammonium titanium fluoride of 6 mMs and 18 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and make deposit fluid, then ITO electro-conductive glass substrate the facing down with in 60 degree angle immersion deposition liquid zinc oxide nano-wire array of zinc oxide nano-wire array will be prepared with, after 5 minutes by its taking-up, with deionized water, rinse well, dry up, the Muffle furnace that gained ITO electro-conductive glass substrate is placed in to 400 degrees Celsius is processed 1 hour, obtain titania nanotube (bar) array of crystallization.
Embodiment 4:
1) first the boric acid of the ammonium titanium fluoride of 10 mMs and 22 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and obtain mixed solution, again clean ITO electro-conductive glass substrate is at room temperature immersed in mixed solution 30 minutes, then with deionized water, rinse well, dry up, on ITO electro-conductive glass substrate, make titanium dioxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds the two hydration zinc acetates of 16 mMs, making monoethanolamine and the ratio of the amount of substance of zinc ion is 1: 1; Then the water-bath magnetic agitation that mixture is sealed and is placed in 62 ℃ evenly obtains zinc oxide colloidal sol, after zinc oxide colloidal sol is taken out at room temperature standing 12 hours, utilize spin coating technique with 3000 revs/min, above-mentioned zinc oxide colloidal sol after standing to be spin-coated on the ITO electro-conductive glass substrate of preparing titanium dioxide pretreatment layer, then place it in the baking oven of 205 ℃ and process 5 minutes, the Muffle furnace that ITO electro-conductive glass substrate is placed in to 450 ℃ is again processed 1 hour, obtains zinc oxide inculating crystal layer;
3) by the zinc nitrate hexahydrate of 4 mMs, the NaOH of 80 mMs is dissolved in respectively in deionized water, then zinc nitrate solution is poured in sodium hydroxide solution and mixed, in volumetric flask, be settled to again 100 milliliters, mix and obtain growth-promoting media, then the ITO electro-conductive glass substrate that is coated with zinc oxide inculating crystal layer of having prepared is faced down zinc oxide inculating crystal layer to immerse in growth-promoting media and grow 20 minutes in 80 ℃ of water-baths with 60 degree angles, then ITO electro-conductive glass substrate is taken out, with deionized water, rinse well, dry up, obtain zinc oxide nano-wire array;
4) boric acid of the ammonium titanium fluoride of 7.5 mMs and 20 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and make deposit fluid, then ITO electro-conductive glass substrate the facing down with in 60 degree angle immersion deposition liquid zinc oxide nano-wire array of zinc oxide nano-wire array will be prepared with, after 10 minutes by its taking-up, with deionized water, rinse well, dry up, the Muffle furnace that gained ITO electro-conductive glass substrate is placed in to 450 degrees Celsius is processed 1 hour, obtain titania nanotube (bar) array of crystallization.
Claims (4)
1. the preparation method of titania nanotube/bar array, is characterized in that:
1) first the boric acid of the ammonium titanium fluoride of 8～10 mMs and 18～22 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and obtain mixed solution, again clean ITO electro-conductive glass substrate is immersed in mixed solution, then with deionized water, rinse well, dry up, on ITO electro-conductive glass substrate, make titanium dioxide pretreatment layer;
2) monoethanolamine is dissolved in 20 milliliters of EGMEs, and then adds the two hydration zinc acetates of 1～16 mM, making monoethanolamine and the ratio of the amount of substance of zinc ion is 1:1; Then the water-bath magnetic agitation that mixture is sealed and is placed in 58～62 ℃ evenly obtains zinc oxide colloidal sol, after zinc oxide colloidal sol is taken out at room temperature standing 12～18 hours, utilize spin coating technique with 3000 revs/min, above-mentioned zinc oxide colloidal sol after standing to be spin-coated on the ITO electro-conductive glass substrate of preparing titanium dioxide pretreatment layer, then place it in the baking oven of 195～205 ℃ and process 5～10 minutes, the Muffle furnace that ITO electro-conductive glass substrate is placed in to 450～500 ℃ is again processed 0.5～1 hour, obtains zinc oxide inculating crystal layer;
3) by the zinc nitrate hexahydrate of 4 mMs, the NaOH of 80 mMs is dissolved in respectively in deionized water, then zinc nitrate solution is poured in sodium hydroxide solution and mixed, in volumetric flask, be settled to again 100 milliliters, mix and obtain growth-promoting media, then the ITO electro-conductive glass substrate that is coated with zinc oxide inculating crystal layer of having prepared is immersed in growth-promoting media and grown 5～20 minutes in 80 ℃ of water-baths, then ITO electro-conductive glass substrate is taken out, with deionized water, rinse well, dry up, obtain zinc oxide nano-wire array;
4) boric acid of the ammonium titanium fluoride of 5～7.5 mMs and 15～20 mMs is dissolved in respectively in deionized water, then BAS is poured in ammonium titanium fluoride solution, after mixing, be settled to 100 milliliters and make deposit fluid, then will be prepared with in the ITO electro-conductive glass substrate immersion deposition liquid of zinc oxide nano-wire array, then by its taking-up, with deionized water, rinse well, dry up, the Muffle furnace that gained ITO electro-conductive glass substrate is placed in to 400～450 degrees Celsius is processed 1 hour, obtains the titania nanotube/bar array of crystallization.
2. the preparation method of titania nanotube/bar array according to claim 1, is characterized in that: the ITO electro-conductive glass substrate that described step 3) is coated with zinc oxide inculating crystal layer faces down zinc oxide inculating crystal layer to immerse in growth-promoting media with 60 degree angles.
3. the preparation method of titania nanotube/bar array according to claim 1, is characterized in that: described step 3) is controlled the length of zinc oxide nanowire by controlling growth time.
4. the preparation method of titania nanotube/bar array according to claim 1, is characterized in that: described step 4) is prepared with ITO electro-conductive glass substrate the facing down with in 60 degree angle immersion deposition liquid zinc oxide nano-wire array of zinc oxide nano-wire array.
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