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A kind of preparation method of cage multilayer structure boron doped diamond electrode

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

Active Publication Date: 2021-08-20
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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  • A kind of preparation method of cage multilayer structure boron doped diamond electrode

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Experimental program
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Effect test

Embodiment 1

[0031] Firstly, TiNb metal mesh and boron-doped diamond powder with particle size of 50 μm were placed alternately layer by layer. Diamond powder and TiNb metal mesh were processed by high temperature and high pressure molding under the conditions of pressure of 200 MPa and temperature of 1200 °C for 3 h. Then, a boron-doped diamond protective layer is deposited on the composite electrode by microwave plasma chemical vapor deposition technology to enhance the strength of the diamond electrode with multi-channel sandwich structure. Make sure that the deposition temperature is around 780°C. Using CH 4 / H 2 nucleation in an atmosphere with a flow ratio of 7% for 2 h, followed by the reduction of CH 4 Ratio to CH 4 / H 2 The flow ratio is 5% for diamond growth, and the carrier H of the boron source is introduced at the same time 2 Gas flow as a percentage of total H 2 The proportion of gas flow is 5%. And the lower surface of the composite electrode is again realized by the...

Embodiment 2

[0033] Firstly, TiNb metal mesh and boron-doped diamond powder with particle size of 100 μm were alternately placed layer by layer. The diamond powder and the TiNb metal mesh were processed by high temperature and high pressure molding at a pressure of 300 MPa and a temperature of 1300 °C for 4 h. Then, a boron-doped diamond protective layer is deposited on the composite electrode by microwave plasma chemical vapor deposition technology to enhance the strength of the diamond electrode with multi-channel sandwich structure. Make sure that the deposition temperature is around 820°C. in CH 4 / H 2 nucleation in an atmosphere with a flow ratio of 9% for 1 h, followed by the reduction of CH 4 Ratio to CH 4 / H 2 The flow ratio is 3% for diamond growth, and the carrier H of the boron source is introduced at the same time 2 Gas flow as a percentage of total H 2 The proportion of gas flow is 5%. And the lower surface of the composite electrode is again realized by the above proc...

Embodiment 3

[0035] First, the TiNb metal mesh and boron-doped diamond powder 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 protection layer is deposited on the composite electrode by DC arc plasma chemical vapor deposition technology to enhance the strength of the diamond electrode with multi-channel sandwich structure. Make sure that the deposition temperature is around 800°C. in CH 4 / H 2 nucleation in an atmosphere with a flow ratio of 7% for 2 h, followed by the reduction of CH 4 Ratio to CH 4 / H 2 The flow ratio is 5% for diamond growth, and the carrier H of the boron source is introduced at the same time 2 Gas flow as a percentage of total H 2 The proportion of gas flow is 10%. And the lower surface of the composite electrode ...

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Abstract

The invention relates to a method for preparing a cage multilayer structure boron-doped diamond electrode, which belongs to the field of semiconductor material preparation. Firstly, TiNb metal mesh and boron-doped diamond powder with a particle size of 1 μm-100 μm are placed alternately layer by layer, and processed by hot isostatic pressing at a pressure of 100-300 MPa and a temperature of 1000-1400 ° C for 30 min-5 h . Then, the diamond / TiNb composite electrode is deposited on the upper and lower sides of the diamond composite electrode by microwave plasma or DC arc plasma chemical vapor deposition technology to respectively deposit boron-doped diamond protective layers to strengthen the cage multi-layer boron-doped diamond electrode. Strength of. Subsequently, the electrode is heat-treated at 800-1000°C for 2-10 hours to finally form a stable high-performance cage multilayer structure boron-doped diamond electrode with a higher effective reaction surface area. The invention is suitable for preparing diamond electrodes.

Description

technical field [0001] The invention relates to a method for preparing a cage multilayer structure boron-doped diamond electrode, which belongs to the field of semiconductor material preparation. Background technique [0002] In recent years, 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 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 with better performance than traditional electrodes, pyrolytic graphite and other forms of electrodes. Materials have incomparable advantages over many electrode materials, so they have attracted extensive attention from scientists from all over the world. [0003] BDD electrodes have a wide potential window, sma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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