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Preparation method of boron-doped diamond film electrode taking porous titanium as matrix

A boron-doped diamond and thin-film electrode technology, applied in the field of electrode materials, can solve problems such as the influence of electron transfer performance, poor conductivity of passivation film, and electrode film peeling off, and achieve the advantages of increasing binding force, wide potential window and improving stability. Effect

Inactive Publication Date: 2014-03-19
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, if the content of TiC is high, its loose and porous structure will easily cause the immersion of the electrolyte and cause the electrode film to fall off.
Chinese patent CN102864482A uses the method of anodic oxidation to form a passivation layer on the surface of the substrate that can effectively prevent the formation of titanium carbide, thereby improving the adhesion characteristics of the diamond film and the porous titanium substrate, but the passivation film formed on the surface of the titanium base has poor conductivity. Its electron transport properties may be affected

Method used

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  • Preparation method of boron-doped diamond film electrode taking porous titanium as matrix
  • Preparation method of boron-doped diamond film electrode taking porous titanium as matrix
  • Preparation method of boron-doped diamond film electrode taking porous titanium as matrix

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Experimental program
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Effect test

Embodiment 1

[0020] (1) The porous titanium matrix with a pore size of 15mm×15mm×1mm and a porosity of 60 μm and a porosity of 32% (measured by mercury porosimetry) is soaked in an aqueous NaOH solution with a mass fraction of 10% to fully deoil it, and degrease it with water. After ultrasonic cleaning of the final porous titanium substrate, put it into a beaker filled with 10% hydrochloric acid solution and heat it to a slight boiling state. Stir continuously until the solution gradually becomes light purple. Use deionized water to ultrasonically clean the porous titanium substrate for 5 minutes and rinse it clean. Then put it in deionized water for protection;

[0021] (2) The porous titanium processed in step (1) is used as the substrate, the tantalum wire is used as the hot wire, methane and hydrogen are used as the gas source, and trimethyl borate is used as the boron source. In the methane and hydrogen atmosphere, hot wire chemical vapor deposition is used. Method for growing boron-d...

Embodiment 2

[0027] (1) The porous titanium matrix with a pore size of 15mm×15mm×1mm and a porosity of 60 μm and a porosity of 32% (measured by mercury porosimetry) is soaked in an aqueous NaOH solution with a mass fraction of 10% to fully deoil it, and degrease it with water. After ultrasonic cleaning of the final porous titanium substrate, put it into a beaker filled with 10% hydrochloric acid solution and heat it to a slight boiling state. Stir continuously until the solution gradually becomes light purple. Use deionized water to ultrasonically clean the porous titanium substrate for 5 minutes and rinse it clean. Then put it in deionized water for protection;

[0028] (2) The porous titanium processed in step (1) is used as the substrate, the tantalum wire is used as the hot wire, methane and hydrogen are used as the gas source, and trimethyl borate is used as the boron source. In the methane and hydrogen atmosphere, hot wire chemical vapor deposition is used. Method for growing boron-dop...

Embodiment 3

[0034] (1) The porous titanium substrate with a size of 15mm×15mm×1mm, a pore size of 100μm, and a porosity of 27% (measured by mercury porosimetry) is soaked in an aqueous NaOH solution with a mass fraction of 10% to fully deoil it, and degrease it with water. After ultrasonic cleaning of the final porous titanium substrate, put it into a beaker filled with 10% hydrochloric acid solution and heat it to a slight boiling state. Stir continuously until the solution gradually becomes light purple. Use deionized water to ultrasonically clean the porous titanium substrate for 5 minutes and rinse it clean. Then put it in deionized water for protection;

[0035] (2) The porous titanium processed in step (1) is used as the substrate, the tantalum wire is used as the hot wire, methane and hydrogen are used as the gas source, and trimethyl borate is used as the boron source. In the methane and hydrogen atmosphere, hot wire chemical vapor deposition is used. Method for growing boron-dope...

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Abstract

The invention discloses a preparation method of a boron-doped diamond (BDD) film electrode taking porous titanium as a matrix. The preparation method is characterized in that the titanium matrix is a porous titanium material with the porosity of 20-50%, hot filament chemical vapor deposition equipment is adopted, and a porous titanium base BDD electrode is prepared through chemical vapor deposition by using a second-order boron concentration control mode. By adopting the method, the generation capacity of TiC is controlled by adjusting boron source concentrations of different stages during chemical vapor deposition, namely the formation of TiC is inhibited by using high boron doping at the initial stage to improve the bonding force between a base and a film, and the boron source concentration is reduced in the later period of reaction to perform low boron doping. The porous titanium base BDD electrode prepared by the method disclosed by the invention is uniform and compact in diamond grain, and the porous titanium matrix is completely covered by a diamond film, so that the electrode has good stability and a relatively wide potential window.

Description

technical field [0001] The invention belongs to the technical field of electrode materials, and in particular relates to a method for preparing a boron-doped diamond thin film electrode (BDD) by chemical vapor deposition on a porous titanium substrate by means of second-order boron concentration control. Background technique [0002] Among many known anode materials, boron-doped diamond film electrode (BDD) has the characteristics of wide potential window, low background current, good electrochemical stability, strong corrosion resistance, and surface is not easy to be polluted. The electrode material with the highest oxygen potential (E° ·OH / H2O =2.80V vs. SHE), it has broad application prospects in electrooxidation, electrosynthesis, electroanalysis, supercapacitors, electrochemical sensors, etc. Due to the good electrical conductivity, high mechanical strength and cheap price of metal titanium (Ti), DSA (dimensionally Stable Anodes) type titanium-based BDD electrodes (Ti...

Claims

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Application Information

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IPC IPC(8): C23C16/30C23C16/02C23C16/52
Inventor 林海波辛丽孙见蕊何亚鹏解秉尧黄卫民
Owner JILIN UNIV
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