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Self-standing TiO2 nanotube array membrane and preparation method thereof

A nanotube array, self-supporting technology, applied in photosensitive equipment, semiconductor/solid-state device manufacturing, electrolytic capacitors, etc., can solve the problems of small potential application, curling into groups, and unrealizable research fields

Inactive Publication Date: 2010-10-13
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are several reports about the preparation of self-supporting TNT films (Nano Lett. Since the TNT film has not been annealed, it has an amorphous structure, and its potential application is very small.
When high-temperature annealing is performed to crystallize the nanotubes, the wall thickness of the nanotubes is not uniform (the nozzle part is thin, and the tube bottom part is thick), which causes the stress difference between the two sides of the film, so that the self-supporting film will inevitably bend, crack, or even collapse. Phenomena such as curling into agglomerates (such as figure 1 shown)
This makes this self-supporting TNT thin film unrealizable in the research field of photoelectrochemistry

Method used

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  • Self-standing TiO2 nanotube array membrane and preparation method thereof
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  • Self-standing TiO2 nanotube array membrane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0058] At room temperature, place a titanium sheet (15×30mm) with PTFE tape on the back and edges in 20mL containing 0.25wt%NH 4 F, 1wt%H 2 In the ethylene glycol solution of O, the anodic oxidation was carried out under the bias voltage of 30V for 72h, and the thickness of the obtained TNT film was 9 μm. After the oxidation was completed, the titanium sheet with the TNT film was taken out, placed in an ethanol solution for ultrasonic cleaning twice, and then transferred to an open tube furnace for annealing at 350 °C for 1 h at a heating rate of 5 °C / min. The annealed sample is again placed in fresh ethylene glycol electrolyte for anodic oxidation, the voltage is 12V, and the oxidation time is 3h, which is the secondary anodic oxidation, and the formed amorphous TiO 2 The thickness of the oxide layer is 300nm. After the secondary anodic oxidation is finished, take the sample out, first wash it with ethanol (analytical grade), then place it in a petri dish, and gradually add...

Embodiment 2

[0060] At room temperature, place a titanium sheet (15 × 30 mm) covered with PTFE tape on the back and edges in 20 mL of 0.25 wt% NH 4 F, 1wt%H 2 In the ethylene glycol solution of O, the anodic oxidation was carried out under 50V bias for 24h, and the thickness of the obtained TNT film layer was 25μm. After the oxidation was completed, the titanium sheet with the TNT film was taken out, placed in an ethanol solution for ultrasonic cleaning twice, and then transferred to an open tube furnace for annealing at 350 °C for 1 h at a heating rate of 5 °C / min. The annealed sample was again placed in the same ethylene glycol electrolyte as the primary oxidation for secondary anodic oxidation, the voltage was 15V, and the oxidation time was 1h, the formed TiO 2 The thickness of the oxide layer is 200nm. After the secondary anodic oxidation is completed, the sample is taken out, rinsed with ethanol first, and then placed in a petri dish, and deionized water is gradually added. With th...

Embodiment 3

[0063] A TNT film with a thickness of 42 μm (oxidized at 50 V in ethylene glycol system for 48 h, the preparation conditions are the same as in Example 1) was placed in a tube furnace for annealing at 500° C. for 1 h, and the heating rate was 5° C. / min. After cooling, place the sample again in fresh ethylene glycol electrolyte for secondary anodic oxidation, the voltage is 15V, the oxidation time is 30min, the formed TiO 2 The thickness of the oxide layer is 100 nm. After the secondary anodic oxidation, the sample was taken out, rinsed with ethanol first, then placed in a petri dish, and gradually added to deionized water for soaking. The edge of the film was not obviously separated from the substrate. At this point, remove the aqueous solution and add 10ml of 1M HNO to the Petri dish 3 solution. After soaking for about 1 hour, the solution turns light yellow, and the edge of the TNT film is separated from the substrate, becoming a self-supporting film. The film was soaked ...

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Abstract

The invention relates to a self-standing TiO2 nanotube array membrane and a preparation method thereof. The preparation method comprises: a), performing the primary anodic oxidation of a titanium foil, and forming a TiO2 nanotube array membrane on the titanium foil; b), annealing and crystallizing the titanium foil obtained by the processing of the step a); c) performing the secondary anodic oxidation of the processed titanium foil, and forming an amorphous oxide layer with a certain thickness between the titanium foil and the TiO2 nanotube array membrane; and d) stripping the TiO2 nanotube array membrane from the amorphous oxide layer. Meanwhile, the invention also provides a preparation method of the self-standing TiO2 nanotube array membrane and a dye-sensitized solar cell prepared by using the membrane. The self-standing TiO2 nanotube array membrane of the invention is flat in a large area and can be used for constructing an element such as the dye-sensitized solar cell based on the TiO2 nanotube array membrane conveniently.

Description

technical field [0001] The present invention relates to nanotube array films, in particular, to a self-supporting TiO 2 Nanotube array film (hereinafter referred to as TNT film or TNT array) and its preparation method, and dye-sensitized solar cell (hereinafter referred to as DSC) prepared from the film. Background technique [0002] Metal titanium is anodized in a suitable electrolyte, and can self-assemble to form an ordered one-dimensional structure TNT film (J.Mater.Res.2001, 16, 3331; Angew.Chem.Int.Ed.2005, 44, 7463; J. Phys. Chem. B 2006, 110, 16179). TNT-based hydrogen sensing (Adv.Mater.2003, 15, 624; Nanotechnology 2006, 17, 398), dye-sensitized solar cells (ACS Nano 2008, 2, 1113; Nano Lett.2006, 6, 215), light Water splitting (Nano Lett. 2005, 5, 191; J Phy. Chem. C 2007, 111, 8677) and other research work have been carried out accordingly, and have shown excellent performance. However, since the TNT array is attached to the metal titanium substrate, annealing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26H01G9/20H01G9/042H01L51/42H01L51/44H01L51/46
CPCY02E10/542Y02E10/549
Inventor 陈清伟徐东升
Owner PEKING UNIV
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