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Method for preparing noble metal nanocrystalline chemically based on titanium dioxide nanotube array

A noble metal nanocrystal and nanotube technology, applied in the field of material chemistry, can solve the problems of difficult uniform dispersion and attachment of noble metal nanoparticles, decline in catalytic performance, and influence on catalytic activity, and achieve a good template effect, improve catalytic activity, and improve the degree of dispersion. Effect

Inactive Publication Date: 2009-10-21
TONGJI UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, the traditional chemical and electrodeposition loading methods are difficult to achieve a high degree of dispersion of noble metals in the tube, and agglomeration still occurs during the loading process, which affects the improvement of catalytic activity.
On the one hand, because the nanotubes grown in situ are on a flat plate carrier, it is difficult to fully mix with the solution during the metal deposition process, so it is difficult for noble metal nanoparticles to uniformly disperse and attach to the nanotubes.
On the other hand, noble metals are directly deposited on the nanotubes to form agglomerates, which often block the openings of the nanotubes, resulting in a decrease in catalytic performance.

Method used

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  • Method for preparing noble metal nanocrystalline chemically based on titanium dioxide nanotube array
  • Method for preparing noble metal nanocrystalline chemically based on titanium dioxide nanotube array
  • Method for preparing noble metal nanocrystalline chemically based on titanium dioxide nanotube array

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Experimental program
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Effect test

Embodiment 1

[0031] Use 0.80mm pure titanium sheet (99%) in turn with 100 # , 300 # and 500 # Grinding with sandpaper, further polishing with metallographic sandpaper to make the surface of the substrate smooth, then ultrasonically cleaned in distilled water and acetone for 20 min each, and cleaned with double distilled water. The anodizing electrolyte composition is 0.5wt% NaF, 2%wtNaSO 4 , 10wt% polyethylene glycol (400). The anodization voltage was 20V, and the anodization time was 5h. The heat treatment temperature was 450°C, and the heating and cooling rates were both 1°C / min.

[0032] The plating solution is 0.1mol / L H 2 PtCl 6 . The supporting electrolyte was 0.1 mol / L sulfuric acid. Electrodeposition experiments used a three-electrode system on a CHI660C electrochemical workstation with TiO 2 NTs / Ti was the working electrode, platinum sheet was the auxiliary electrode, and saturated calomel electrode (SCE) was the reference electrode. The entire electrochemical reaction cel...

Embodiment 2

[0035] Use 0.50mm pure titanium sheet (99%) in turn with 100 # , 300 # and 500 # Grinding with sandpaper, further polishing with metallographic sandpaper to make the surface of the substrate smooth, then ultrasonically cleaned in distilled water and acetone for 20 min each, and cleaned with double distilled water. The anodizing electrolyte composition was 0.05wt% NaF, 2%wtNaSO 4 , 10wt% polyethylene glycol (400). The anodization voltage was 15V, and the anodization time was 3h. The heat treatment temperature was 550°C, and the heating and cooling rates were both 1°C / min.

[0036] The plating solution is 0.1mol / L PdCl 2 . The supporting electrolyte was 0.05 mol / L sulfuric acid. Electrodeposition experiments used a three-electrode system on a CHI660C electrochemical workstation with TiO 2 NTs / Ti was the working electrode, platinum sheet was the auxiliary electrode, and saturated calomel electrode (SCE) was the reference electrode. The entire electrochemical reaction cel...

Embodiment 3

[0039] Use 0.20mm pure titanium sheet (99%) in turn with 100 # , 300 # and 500 # Grinding with sandpaper, further polishing with metallographic sandpaper to make the surface of the substrate smooth, then ultrasonically cleaned in distilled water and acetone for 20 min each, and cleaned with double distilled water. The anodizing electrolyte composition was 0.8% wt NaF, 1.6% wt NaSO 4 , 20wt% polyethylene glycol (400). The anodization voltage was 10V, and the anodization time was 2h. The heat treatment temperature was 500°C, and the heating and cooling rates were both 1°C / min.

[0040] The plating solution is 0.1mol / L H 2 PtCl 6 and 0.1mol / L PdCl 2 mixed solution. The supporting electrolyte was 0.05 mol / L sulfuric acid. Electrodeposition experiments used a three-electrode system on a CHI660C electrochemical workstation with TiO 2 NTs / Ti was the working electrode, platinum sheet was the auxiliary electrode, and saturated calomel electrode (SCE) was the reference electro...

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Abstract

The invention relates to a method for preparing noble metal nanocrystalline chemically based on titanium dioxide nanotube array. The method comprises the following steps: adopting a method for using ultrasound to assist pulse electrodeposition, taking titanium dioxide nano tubes growing on the titanium base as carriers, and preparing a composite catalyst system which has stable structure and high catalytic activity and is dispersed in the nano tube by means of Pd with high dispersive property. The spherulitic crystal structure with high-dispersive property can provide more surface catalysis activity sites and specific surface area of catalytic reaction. The technique has simple and convenient operation, can obtain Pt-Pd falling type composite spherulitic crystal stable catalysis system which is dispersed highly in the nano tube and can improve catalytic activity and stability of the catalytic electrode when being applied to the energy fields of fuel cells and the like.

Description

technical field [0001] The invention belongs to the field of material chemistry, and relates to a method for preparing a precious metal bimetal composite catalytic electrode by using a titanium-based titanium dioxide nanotube as a carrier by a chemical method. Background technique [0002] In the study of electrocatalysts, obtaining highly dispersed, high specific surface area, and structurally stable catalysts is of great significance for improving the catalytic activity, anti-poisoning performance and lifespan of catalysts. This is also closely related to the selection and preparation of the catalytic carrier. A suitable catalytic dispersion carrier not only has good physical and chemical stability in the catalytic reaction, but also can realize the rapid transfer of electrons between the electrocatalyst and the carrier. The traditional electrocatalyst preparation method is to support noble metals such as Pt and Pd with high catalytic activity on carbon-based catalytic su...

Claims

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Application Information

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IPC IPC(8): C25B11/08C25B11/10C25D11/26
Inventor 赵国华雷燕竹童希立
Owner TONGJI UNIV
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