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Preparation method of boron-doped diamond electrode with mesh cage multilayer structure

A technology of diamond electrode, multi-layer structure, applied in the direction of chemical instruments and methods, lamination, coating, etc.

Active Publication Date: 2021-06-18
UNIV OF SCI & TECH BEIJING +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although BDD electrodes have excellent characteristics and wide applications, some problems have yet to be solved and explored, such as the preparation of BDDs with larger sizes or complex structures; they should have good surface film firmness and stability during electrolysis; how to How to better introduce immobilized active groups to improve surface reproducibility; how to reduce the surface roughness of electrodes and apply it to the technical application of microelectrodes; how to ensure a higher effective treatment area in actual treatment and improve electrode treatment efficiency are all issues. The current problems to be solved, especially by changing the diamond preparation process to achieve improved BDD electrode performance while maintaining high stability

Method used

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  • Preparation method of boron-doped diamond electrode with mesh cage multilayer structure

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Embodiment 1

[0030]First, TiNb metal mesh and boron-doped diamond micropowder with a particle size of 50 μm are alternately placed layer by layer. The diamond powder and TiNb metal mesh were processed by high temperature and high pressure forming at a pressure of 200 MPa and a temperature of 1200 °C for 3 h. Next, a boron-doped diamond protective layer is deposited on the upper side of the composite electrode by microwave plasma chemical vapor deposition technology to enhance the strength of the multi-channel sandwich structure diamond electrode. Make sure the deposition temperature is about 780°C. using CH 4 :H 2 =7% CH 4 Nucleation for 2 h followed by reduction of CH 4 ratio to 5% for diamond growth while introducing boron source of H 2 The proportion is 5% of the total pure hydrogen gas flow. And the lower surface of the composite electrode is again grown with a boron-doped diamond layer with the same roughness as the upper surface by the above-mentioned process. Afterwards, the...

Embodiment 2

[0032] Firstly, TiNb metal mesh and boron-doped diamond micropowder with a particle size of 100 μm are alternately placed layer by layer. The diamond powder and TiNb metal mesh were processed by high temperature and high pressure forming at a pressure of 300 MPa and a temperature of 1300 °C for 4 h. Next, a boron-doped diamond protective layer is deposited on the upper side of the composite electrode by microwave plasma chemical vapor deposition technology to enhance the strength of the multi-channel sandwich structure diamond electrode. Make sure the deposition temperature is about 820°C. using CH 4 :H 2 =9% CH 4 Nucleation for 1 h, followed by reduction of CH 4 ratio to 3% for diamond growth while introducing boron source of H 2 The proportion is 5% of the total pure hydrogen gas flow. And the lower surface of the composite electrode is again grown with a boron-doped diamond layer with the same roughness as the upper surface by the above-mentioned process. After that...

Embodiment 3

[0034] Firstly, TiNb metal mesh and boron-doped diamond micropowder with a particle size of 1 μm were alternately placed layer by layer. The diamond powder mixed with the pre-graphite powder and the TiNb metal mesh were processed by high temperature and high pressure molding at a pressure of 150 MPa and a temperature of 1000 °C for 5 h. Then, a boron-doped diamond protective layer is deposited on the upper side of the composite electrode by DC arc plasma chemical vapor deposition technology to enhance the strength of the multi-channel sandwich structure diamond electrode. Make sure the deposition temperature is about 800°C. using CH 4 :H 2 =7% CH 4 Nucleation for 2 h followed by reduction of CH 4 ratio to 5% for diamond growth while introducing boron source of H 2 The proportion accounts for 10% of the total pure hydrogen gas flow. And the lower surface of the composite electrode is again grown with a boron-doped diamond layer with the same roughness as the upper surfac...

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Abstract

The invention relates to a preparation method of a boron-doped diamond electrode with a mesh cage multilayer structure, and belongs to the field of semiconductor material preparation. The preparation method comprises the following steps: firstly, alternately placing TiNb metal mehses and boron-doped diamond micro powder with the particle size of 1-100 [mu] m layer by layer, and carrying out hot isostatic pressing forming treatment for 30 minutes to 5 hours under the conditions that the pressure is 100-300 MPa and the temperature is 1000-1400 DEG C; then, respectively depositing boron-doped diamond protective layers on the upper side and the lower side of a diamond / TiNb composite electrode through a microwave plasma or direct-current arc plasma chemical vapor deposition technology so as to enhance the strength of the boron-doped diamond electrode with the mesh cage multilayer structure; and then, carrying out heat treatment on the electrode for 2-10 hours at the temperature of 800-1000 DEG C, and finally forming the stable high-performance boron-doped diamond electrode with the mesh cage multilayer structure with a higher effective reaction surface area. The preparation method is suitable for preparing the diamond electrode.

Description

technical field [0001] The invention relates to a method for preparing a mesh cage multi-layer structure boron-doped diamond electrode, which belongs to the field of semiconductor material preparation. Background technique [0002] In recent years, highly boron-doped diamond (BDD) electrodes have attracted the attention of researchers due to their electrochemical properties and wide application possibilities. The research results show that the BDD electrode has good electrical conductivity and is an excellent electrode material. The covalent structure of the surface, wide band gap and doping, etc., make it different from ordinary metal electrodes and become a carbon functional electrode whose performance is superior to traditional electrodes, pyrolytic graphite and other forms of electrodes. It has the incomparable advantages of many electrode materials, so it has been widely concerned by scientists from all over the world. [0003] The BDD electrode has a wide potential w...

Claims

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Application Information

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IPC IPC(8): C23C16/27C23C16/511C23C16/503C23C16/56G01N27/30C02F1/461B32B15/02B32B9/00B32B9/04B32B33/00B32B37/00B32B37/06B32B37/10
CPCB32B5/16B32B15/02B32B15/16B32B33/00B32B37/00B32B37/06B32B37/10B32B2037/246B32B2457/00C02F1/46109C02F2001/46133C23C16/272C23C16/274C23C16/278C23C16/56G01N27/308
Inventor 郑宇亭李成明张钦睿刘思彤魏俊俊刘金龙陈良贤
Owner UNIV OF SCI & TECH BEIJING
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