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Fabrication method of long-life titanium base electrode

A long-life, titanium-based technology, used in electrodes, electrolysis processes, electrolysis components, etc., can solve problems such as the difficulty of preparing large-area uniform nanotubes, reducing the oxygen evolution potential of electrodes, affecting the use efficiency of electrodes and electrocatalytic activity, etc. It is convenient for industrialized large-scale production, high electrocatalytic activity, and the effect of realizing large-scale production

Active Publication Date: 2013-04-03
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are many improvement methods to improve the service life of titanium-based tin dioxide electrodes, which are mainly divided into the following three categories: one is to dope other metal or non-metal elements in the antimony-doped tin dioxide layer, but there are some limitations, such as The incorporation of elements such as ruthenium and iridium will significantly reduce the oxygen evolution potential of the electrode, affecting the use efficiency and electrocatalytic activity of the electrode; the second is to insert an intermediate layer between the tin dioxide layer and the titanium substrate, which also has the above problems; Surface modification of the titanium matrix itself, such as the introduction of anodized titanium dioxide nanotubes, but due to the limitations of the anodic oxidation method itself, the preparation of large-area uniform nanotubes is difficult, so this technology can only be used to prepare electrodes with small surface areas , there is still a distance from the actual industrial application
Therefore, so far, various electrode preparation technologies to improve the service life of titanium-based tin dioxide electrodes still have their own defects.

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preparation example Construction

[0041] The preparation method of the long-life titanium-based electrode provided by the present invention uses impregnation, reduction, electrodeposition, and thermal oxidation to prepare a long-life and high oxygen evolution potential titanium-based tin dioxide electrode, which specifically includes the following steps:

[0042] 1) Preparation of titanium oxide layer on the surface of titanium substrate by dipping-thermal oxidation method

[0043] Polish the surface of the titanium substrate to smooth, remove oil with alkali, and clean it after oxalic acid etching. After drying, immerse the titanium substrate in the alcohol solution containing titanate, take it out after standing for a period of time, and heat and calcinate at 490-500°C for 0.5 -2h, a silver-gray titanium oxide intermediate layer is prepared.

[0044] 2) Reduction treatment is performed on the surface of the titanium oxide layer in a reducing atmosphere.

[0045] The titanium substrate prepared with the tita...

Embodiment 1

[0050] A method for preparing a long-life titanium-based electrode, comprising the following steps:

[0051] 1) Using the titanium sheet as the substrate, cut the titanium sheet into a size of 1.0cm×4.0cm with scissors, and polish the surface of the titanium sheet with 200-mesh coarse sandpaper and 40-mesh fine sandpaper successively to reveal the metallic luster;

[0052] Then heat and boil in the sodium hydroxide solution of 10% mass fraction concentration for 10min to remove oil;

[0053] Then heat the titanium sheet in a 10% mass fraction oxalic acid solution to slightly boil for 2 hours for acid etching, rinse with deionized water and place it in a 1% volume fraction oxalic acid solution for use;

[0054] Rinse the treated titanium sheet and dry it, then immerse the titanium sheet in the impregnation solution, the composition of the impregnation solution is 70% by volume of butyl titanate, 29% by volume of ethanol, and 1% by volume of nitric acid. After standing in the i...

Embodiment 2

[0062] A method for preparing a long-life titanium-based electrode, comprising the following steps:

[0063] 1) A titanium rod with a length of 55 cm and a diameter of 1 cm is used as the substrate, and the pretreatment steps of the substrate are the same as those in Example 1. Rinse the treated titanium rod and dry it;

[0064] Then immerse the titanium rod in the impregnation solution, the composition of the impregnation solution is 90% by volume of titanate, 9% by volume of ethanol, and 1% by volume of nitric acid. Heat and calcinate the impregnated titanium rod at 510°C for 0.5h in a muffle furnace to obtain a silver-gray titanium oxide layer.

[0065] 2) Pass dry high-purity hydrogen and high-purity ammonia into the reaction furnace at a ratio of 9:1 by volume, and reduce the titanium oxide layer prepared on the surface of the titanium substrate at 400-500 ° C under the condition of isolating oxygen Treat for 10-15 minutes.

[0066] 3) Using the titanium rod as the cat...

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Abstract

The invention discloses a fabrication method of a long-life titanium base electrode, which comprises the steps of fabricating a titanium oxide layer on a titanium substrate by a dipping-thermal decomposition method, reducing the titanium oxide layer in a reducing atmosphere, synchronously depositing a tin metal simple substance and an antimony metal simple substance in proportion on the surface of the titanium oxide layer by an electrodeposition method, and conducting thermal oxidation to allow an antimony doped tin oxide layer to be tightly combined with the titanium oxide layer connected with the titanium substrate to form a solid solution structure. The prepared titanium base tin dioxide electrode has the advantages of long service life, high oxygen evolution potential, high electrocatalytic activity, high generation efficiency of ozone from electrolyzed water, and the like. In addition, the cost of the fabrication process is low, the requirement of equipment is low, the operation is easy to control, and industrial mass production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of preparation of electrochemical catalytic electrodes, and relates to a preparation method of a long-life titanium-based electrode. Background technique [0002] Metal oxide anode, also known as DSA (Dimensionally Stable Anode), or DSE (Dimensionally Stable Electrode), was invented by H.B.Beer and was first industrialized by Italian De Nora Company in 1968 (Titanium Electrode Engineering, Beijing: Metallurgy Industrial Press, 2003). DSA is composed of a metal matrix and a surface active coating. The metal matrix acts as a skeleton and conducts electricity, and the surface active coating participates in the electrochemical reaction of the anode to play a catalytic and conductive role. At present, DSA has been widely used in the fields of chlor-alkali industry, electrolysis industry, electroplating industry, wastewater treatment, organic electrosynthesis and electrometallurgy. [0003] In the electrochemica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/10C25B11/06
Inventor 延卫邵丹徐浩
Owner XI AN JIAOTONG UNIV
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