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Electrically conductive diamond electrode, and sulfuric acid electrolysis method and sulfuric acid electrolysis apparatus each utilizing same

A conductive diamond and sulfuric acid electrolysis technology, which is applied in the direction of electrodes, electrode coatings, electrolytic components, etc., can solve the problem of electrode durability, high oxidizing substances, unclear correlation of conductive diamond electrodes, and undisclosed correlation of conductive diamond electrodes and other issues, to achieve the effect of high current efficiency and high durability

Active Publication Date: 2013-10-30
DE NORA PERMELEC LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] However, in Patent Document 3, diamond-like carbon is used as the electrode, and the relationship between the crystallinity of the conductive diamond electrode and the Raman spectral characteristics / potential window, and the relationship between the crystallinity of the conductive diamond electrode and the potential window are not disclosed. Relationship between persulfuric acid such as peroxodisulfuric acid and oxidizing substances in washing liquid, current efficiency and productivity such as battery voltage
[0012] However, in the methods described in the above-mentioned Patent Documents 1 to 3, the relationship between the crystallinity of the conductive diamond electrode and the Raman spectral characteristics / potential window is not clear, and these methods cannot produce electrodes with high durability and Conductive diamond electrode with high oxidizing species generation efficiency at low cell voltage

Method used

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  • Electrically conductive diamond electrode, and sulfuric acid electrolysis method and sulfuric acid electrolysis apparatus each utilizing same
  • Electrically conductive diamond electrode, and sulfuric acid electrolysis method and sulfuric acid electrolysis apparatus each utilizing same
  • Electrically conductive diamond electrode, and sulfuric acid electrolysis method and sulfuric acid electrolysis apparatus each utilizing same

Examples

Experimental program
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Embodiment

[0131] Next, the present invention will be specifically described with reference to Examples and Comparative Examples. However, the present invention is not limited by these Examples.

[0132] It should be noted that the Raman spectrum characteristic measurement of the electrode produced in the present invention, the film thickness measurement of the conductive diamond electrode, the boron concentration measurement, the durability test of the electrode, the measurement of the potential window, the sulfuric acid ion used in the electrolysis The preparation of the electrolytic solution and the measurement of the concentration of the oxidizing substance in the produced oxidizing substance solution were carried out by the following method.

[0133]

[0134] In order to determine whether conductive diamond can be produced and the A / B intensity ratio, the surface Raman measurement of the electrode was performed.

[0135] ・Measuring device: Raman spectrophotometer manufactured by ...

Embodiment 2～10

[0205] As Examples 2-10, the oxidizing substance solution was obtained according to the method as in Example 1, the difference is: by changing the methane flow rate, the trimethyl borate flow rate and the film formation time, the conductive diamond film thickness, potential window , A / B, and boron concentration were changed as shown in Tables 1 and 2, and the electrode thus obtained was used as an anode.

[0206] The results of the obtained oxidizing substance solution are shown in Tables 6 and 7.

Embodiment 11～14

[0208] The oxidizing substance solution was obtained by the same method as in Example 1, except that the sulfuric acid ion concentration and the acid concentration in the electrolytic solution were changed as shown in Tables 2-3.

[0209] The results of the obtained oxidizing substance solutions are shown in Tables 7-8.

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Abstract

The present invention provides an electrically conductive diamond electrode comprising an electrically conductive substrate and an electrically conductive diamond layer coated on the surface of the electrically conductive substrate, featuring that: 1) the thickness of the electrically conductive diamond layer is 1ˆ¼25µm, 2) the potential window fulfills Equation (1) and 3) the ratio (A / B) of the diamond component A and the non-diamond component B by the Raman spectroscopic analysis fulfills Equation (2). 2.1 �¢ V ‰¦ potential window ‰¦ 3.5 �¢ V 1.5 < A / B ‰¦ 6.5 A: Intensity at the wave number 1300cm -1 by the Raman spectroscopic analysis B: Intensity at the wave number 1500cm -1 by the Raman spectroscopic analysis. The present invention intends to provide an electrically conductive diamond electrode with a high durability as electrode, which achieves a high current efficiency of oxidizing agent at a low cell voltage by controlling the thickness of the electrically conductive diamond layer and crystallinity of the electrically conductive diamond, a sulfuric acid electrolysis method and an electrolysis apparatus of sulfuric acid applying the electrically conductive diamond electrode.

Description

technical field [0001] The invention relates to a conductive diamond electrode, a sulfuric acid electrolysis method and a sulfuric acid electrolysis device for stably generating oxidizing substances by using the conductive diamond electrode to directly electrolyze sulfuric acid. Background technique [0002] As a pretreatment agent or etchant for metal plating, an oxidizing agent in chemical mechanical polishing in semiconductor equipment manufacturing, an oxidizing agent for organic matter in wet analysis, and a detergent for silicon wafers, it is used in various manufacturing processes and inspection processes, Persulfuric acid and persulfate are used. These persulfuric acids and persulfates are called "oxidizing substances", and it is known that the "oxidizing substances" are produced by electrolysis of sulfuric acid, and industrial-scale electrolytic production has already been realized. [0003] In the present invention, the "oxidizing substance" refers to persulfuric ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/06C01B31/06C25B1/28C25B9/19
CPCC25B1/285C25B11/0447C25B1/30C25B1/29C25B11/075C25B11/043C25B11/083C25B9/19
Inventor 加藤昌明土门宏纪小坂纯子
Owner DE NORA PERMELEC LTD