Method for preparing titanium dioxide nanotube array photoelectrode

A nanotube array and titanium dioxide technology, applied in electrolytic coatings, surface reaction electrolytic coatings, coatings, etc., can solve the problems of low photocatalytic activity, toxic raw materials, complicated operation, etc., and achieve high photocatalytic activity and good stability , the effect of mild preparation conditions

Active Publication Date: 2013-10-23
QINGDAO AGRI UNIV
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Problems solved by technology

[0003] However, it also has certain defects: (1) The recombination rate of photogenerated carriers is high and the efficiency of photocatalytic reaction is low
(2) Pure TiO 2 Nanotube arrays are wide bandgap semiconductors, due to TiO 2 The band gap is wide and can only be excited by ultraviolet light with a wavelength of less than 400nm, and has no response in the visible light region, so the utilization of sunlight is low (about 5%), which limits their applications, and the intrinsic state titanium dioxide photogenerated electrons and space The hole recombination rate is relatively high, which also affects the improvement of photocatalytic efficiency.
(3) TiO 2 The barrier layer between the nanotube array and the substrate increases its resistance as an electrode material, which limits its development in the field of electrocatalysis and photoelectrocatalysis
[0004] In order to overcome the above defects, people have carried out a lot of research, but these technologies either use toxic raw materials in the preparation process, excessive preparation conditions, complex operation and poor reliability, or the prepared electrodes have poor stability, low photocatalytic activity, and do not conform to the environment. Development and market technology needs
Therefore, need a kind of raw material nontoxic in the preparation process, preparation condition is mild, simple and reliable, the prepared electrode stability is good, photocatalytic activity is high, green pollution-free, have the preparation method of photocatalytic activity of visible light photocatalytic titanium dioxide nanotube array , but there is no report in the prior art

Method used

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  • Method for preparing titanium dioxide nanotube array photoelectrode
  • Method for preparing titanium dioxide nanotube array photoelectrode
  • Method for preparing titanium dioxide nanotube array photoelectrode

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Such as figure 1 , 2 , The preparation method of the titanium dioxide nanotube array photoelectrode shown in 3, 4 is characterized in that, the steps are as follows:

[0022] 1) Cut pure titanium sheets (titanium > 99.9%) into 100×10×0.2mm strip-shaped foils, clean them with decontamination powder and hydrofluoric acid, and polish them with 1000-mesh sandpaper and 2000-mesh sandpaper, respectively. Acetone, ethanol and deionized water were ultrasonically cleaned for 5 minutes before use;

[0023] 2) Using the titanium sheet pretreated in step 1) as the substrate, the titanium dioxide nanotube array was prepared in situ by the constant current and constant voltage anodization method, and the electrolyte was 0.5% NaF and 1.0M Na 2 SO 4 Mixed solution, temperature 25°C, voltage 20V, current 0.004mA / cm 2 , oxidized for 2h, in situ generating titania nanotube arrays on the surface of the titanium sheet;

[0024] 3) calcining the nanotube array prepared in step 2) at 550...

Embodiment 2

[0029] 1) Cut pure titanium sheets (titanium>99.9%) into 100×10×0.2mm strip-shaped foils, clean them with decontamination powder and hydrofluoric acid, and polish them with 1000-mesh paper and 2000-mesh sandpaper. Acetone, ethanol and deionized water were ultrasonically cleaned for 5 minutes before use;

[0030] 2) Using the titanium sheet pretreated in step 1) as a base, prepare a titanium dioxide nanotube array, and the preparation method is the same as that in Example 1.

[0031] 3) Calcining the nanotube array prepared in step 2) at 450° C. for 2 hours, and cooling in the furnace for later use;

[0032] 4) take graphite powder as raw material, prepare graphene oxide, and preparation method is with embodiment 1;

[0033] 5) Using the titanium dioxide nanotube array as the working electrode and the platinum electrode as the cathode, the three-electrode system was used for pulse deposition and reduction in different concentrations of sodium tungstate and graphene oxide solut...

Embodiment 3

[0036]1) Cut pure titanium sheets (titanium>99.9%) into 100×10×0.2mm strip-shaped foils, clean them with decontamination powder and hydrofluoric acid, and polish them with 1000-mesh sandpaper and 2000-mesh sandpaper. Use acetone, ethanol and deionized water after ultrasonic cleaning;

[0037] 2) Using the titanium sheet pretreated in step 1) as a substrate, prepare a titanium dioxide nanotube array, and the preparation method is the same as in Example 1;

[0038] 3) Calcining the nanotube array prepared in step 2) at 750° C. for 2 hours, cooling in the furnace and then standby;

[0039] 4) take graphite powder as raw material, prepare graphene oxide, and preparation method is with embodiment 1;

[0040] 5) Using the titanium dioxide nanotube array as the working electrode and the platinum electrode as the cathode, a three-electrode system was used to perform pulse deposition and reduction in different concentrations of sodium tungstate and graphene oxide solutions. Electroly...

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Abstract

The invention discloses a method for preparing a titanium dioxide nanotube array photoelectrode. The method comprises the following steps of: 1, pretreating a titanium sheet; 2, by taking the pretreated titanium sheet as a substrate, preparing a titanium dioxide nanotube array by employing a constant current constant voltage anodic oxidation method; 3, calcining and cooling the titanium dioxide nanotube array, and obtaining a titanium dioxide nanotube array with different crystal structures; 4, by taking graphite powder as a raw material, preparing oxidized graphene with water solubility; 5, by taking the titanium dioxide nanotube array in the step 3 as a working electrode, taking a platinum electrode as a counter electrode, performing pulse deposition reduction in sodium tungstate and oxidized graphene solutions of different concentrations by utilizing a three-electrode system; 6, calcining the prepared photoelectrode under the vacuum condition of 100-300 DEG C to prepare graphene and tungsten trioxide modified titanium dioxide nanotube array photoelectrode. The raw materials in the preparation process are non-toxic, the preparation conditions are mild, the prepared electrode has high stability, the photocatalytic activity is high, and the electrode is environmentally-friendly and has high visible-light catalytic activity.

Description

technical field [0001] The invention relates to a method for preparing a titanium dioxide nanotube array photoelectrode, which belongs to the field of composite photoelectrode preparation. Background technique [0002] Titanium dioxide nanotube array photoelectrode has the advantages of large specific surface area, high stability, and good photocatalytic performance, so it exhibits high hydrogen sensitivity, photoelectric conversion efficiency and photocatalytic performance, making it widely used in gas sensing materials, solar cells, Photocatalysis and other aspects have immeasurable potential application value. The ordered nanotube array improves the transport and transfer ability of photogenerated electrons in immobilized titanium dioxide. Currently TiO 2 The preparation methods of nanotube array photoelectrodes include photoelectrochemical etching, sol-gel, hydrothermal method, template method and anodic oxidation method, among which the anodic oxidation method in fluo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D5/18C25D11/26C25D15/00
Inventor 辛言君刘永萍马东张娇
Owner QINGDAO AGRI UNIV
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