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A kind of preparation method of ordered electrode

A technology of electrodes and working electrodes, which is applied in the field of preparation of ordered electrodes, can solve the problems of limited high specific surface area of ​​titanium dioxide nanotubes, and achieve the effects of improving catalytic activity and stability, low cost and stable structure

Active Publication Date: 2016-03-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the direct pulse electrodeposition method, the noble metal particles are too large to be 100nm, and the noble metal electrocatalyst can only be dispersed on the surface of titanium dioxide nanotubes and cannot enter the nanotubes, which limits the advantages of high specific surface area of ​​titanium dioxide nanotubes.

Method used

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  • A kind of preparation method of ordered electrode
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  • A kind of preparation method of ordered electrode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The titanium sheet (99.7%) was polished successively with 500 and 1000 mesh sandpaper to make the substrate surface smooth, and then ultrasonically cleaned in distilled water, absolute ethanol and acetone for 30 min respectively. The selected composition is 0.5wt% NH 4 F, 10wt% water and 89.5wt% ethylene glycol electrolyte for anodic oxidation. The oxidation voltage was 50V. The oxidation time is 3h.

[0041] The nickel plating solution is composed of: pH 4.4 aqueous solution 1.1MNiSO 4 +0.5MNiCl 2 +1.65MH 3 BO 3 . The pulse current density is 100mAcm -2 , temperature 25°C. Electrodeposition adopts three-electrode system, electrodeposition adopts two-electrode system, pulse conduction time t on 1.4ms, disconnection time t off is 5.2ms. The electrodeposition time is 25s.

[0042] figure 1 and figure 2 The Ni-titania nanotube electrode obtained by anodizing the titanium dioxide nanotube array and pulse electrodeposition according to the conditions in Exampl...

Embodiment 2

[0044] The titanium sheet (99.7%) was polished successively with 500 and 1000 mesh sandpaper to make the substrate surface smooth, and then ultrasonically cleaned in distilled water, absolute ethanol and acetone for 30 min respectively. The selected composition is 1.0wt% NH 4 F, the electrolytic solution of 15wt% water and 84wt% ethylene glycol carries out anodic oxidation. The oxidation voltage was 50V. The oxidation time is 4h.

[0045] The electroplating solution for nickel is composed of: pH 4 aqueous solution 1.1MNiSO 4 +1.5MH 3 BO 3 . The pulse current density is 100mAcm -2 , temperature 25°C. Electrodeposition adopts two-electrode system, pulse conduction time t on 1.2ms, disconnection time t off is 5.2ms. The electrodeposition time is 10s. After nickel was electrodeposited, it was dipped into 10mM potassium chloroplatinate solution for 20min.

[0046] image 3 It is a PtNi-titania nanotube ordered electrode prepared according to the conditions in Example 2...

Embodiment 3

[0049] The titanium sheet (99.7%) was polished successively with 500 and 1000 mesh sandpaper to make the substrate surface smooth, and then ultrasonically cleaned in distilled water, absolute ethanol and acetone for 30 min respectively. The selected composition is 1.0wt% NH 4 F, the electrolytic solution of 15wt% water and 84wt% ethylene glycol carries out anodic oxidation. The oxidation voltage was 50V. The oxidation time is 4h.

[0050] The electroplating solution for nickel is composed of: pH 5 aqueous solution 1.1MNiSO 4 +0.5MNiCl 2 +1.2MH 3 BO 3 . The pulse current density is 100mAcm -2 , temperature 25°C. Electrodeposition adopts two-electrode system, pulse conduction time t on 1.2ms, disconnection time t off is 5.2ms. The electrodeposition time is 10s. After nickel was electrodeposited, it was immersed in 10mM chloropalladium acid solution for 20min.

[0051] Figure 5 It is a PdNi-titania nanotube ordered electrode prepared according to the conditions in ...

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Abstract

The invention relates to a method for preparation of an ordered electrode with noble metal nanoparticles loaded on a titanium dioxide nano-array. Specifically, the titanium dioxide nanotube array grows on a titanium sheet, the array is adopted as the base to prepare an Ni precursor by a pulse electrodeposition technique, and then precious metals such as platinum, palladium, gold and the like are loaded on the precursor through replacement. For the prepared electrode, a noble metal catalyst not only can be uniformly distributed on the surface of the titanium dioxide nano-array, but also can be evenly dispersed in the nanotubes. The electrode precursor Ni is well covered by the noble metal catalyst, and can provide more surface catalytic active sites and larger catalytic reaction specific surface area. The method has the advantages of simple operation and low cost, and application of the method in fuel cells, photocatalysis and other fields can improve the catalytic activity and stability of the catalytic electrode.

Description

technical field [0001] The invention relates to a method for preparing orderly electrodes by using electrodeposition precursors and replacing precious metals, which may be used in fuel cells and photocatalysis, with titanium-based titanium dioxide nanotube arrays as carriers. Background technique [0002] A suitable catalyst support not only has good physical and chemical stability, but also can realize the rapid transfer of electrons between the electrocatalyst and the support. Traditional catalyst supports generally use carbon bases such as carbon black, activated carbon, etc. However, when these carbon-based supports run in the reaction system for a long time, they have poor stability and are prone to aggregation, which may cause the loss of noble metal catalysts and affect the catalytic activity. Recently, the use of carbon nanotubes, carbon nanoscrolls, etc. as catalyst supports has also been reported. Compared with traditional supports, carbon nanotubes and nanovolum...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/88
CPCY02E60/50
Inventor 俞红梅张长昆李永坤邵志刚衣宝廉
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI