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Self-supporting boron-doped diamond electrochemical sensor and preparation method and application thereof

A diamond and boron doping technology, applied in electrochemical variables of materials, scientific instruments, gaseous chemical plating, etc. Reproducible results

Active Publication Date: 2020-11-17
CHINA UNIV OF GEOSCIENCES (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a self-supporting boron-doped diamond (Freestanding boron-doped diamond, FBDD) electrochemical sensor to solve the problem of the prior art When the BDD film sensor detects heavy metals in water, it cannot meet the requirements of accurate and long-term application

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  • Self-supporting boron-doped diamond electrochemical sensor and preparation method and application thereof
  • Self-supporting boron-doped diamond electrochemical sensor and preparation method and application thereof
  • Self-supporting boron-doped diamond electrochemical sensor and preparation method and application thereof

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Embodiment 1

[0045] The present embodiment provides a kind of preparation method of FBDD electrochemical sensor, comprises the following steps:

[0046] (1) Pretreatment: Polish the surface of the metal molybdenum disc to remove the oxide layer, and use W0.5 diamond polishing agent to polish it into a mirror surface, place it in acetone for ultrasonic cleaning for 10 minutes, transfer to ethanol for ultrasonic cleaning for 5 minutes, and dry it for later use;

[0047] (2) Substrate seed crystal: 1 g of nano-diamond powder (50 nm in particle size) was uniformly densely spread on the surface of a metal molybdenum disc with a diameter of 10 cm, mechanically ground for 5 min, and then the surface was blown clean with nitrogen gas for later use.

[0048] (3) CVD coating: put the base material after the above seed crystal into the reaction chamber, reduce the vacuum degree in the furnace to 10 -4 Below Pa, start to feed the reaction gas for coating. The heat source is provided by tungsten wire,...

Embodiment 2

[0061] The present embodiment provides a kind of preparation method of FBDD electrochemical sensor, comprises the following steps:

[0062](1) Pretreatment: Polish the surface of the metal molybdenum disc to remove the oxide layer, and use W0.5 diamond polishing agent to polish it into a mirror surface, place it in acetone for ultrasonic cleaning for 10 minutes, transfer to ethanol for ultrasonic cleaning for 5 minutes, and dry it for later use;

[0063] (2) Substrate seed crystal: 1 g of nano-diamond powder (60 nm in particle size) was evenly and densely spread on the surface of a metal molybdenum disc with a diameter of 10 cm, mechanically ground for 5 min, and then the surface was blown clean with nitrogen gas for later use.

[0064] (3) CVD coating: put the base material after the above seed crystal into the reaction chamber, reduce the vacuum degree in the furnace to 10 -4 Below Pa, start to feed the reaction gas for coating. The heat source is provided by tungsten wire,...

Embodiment 3

[0069] The present embodiment provides a kind of preparation method of FBDD electrochemical sensor, comprises the following steps:

[0070] (1) Pretreatment: Polish the surface of the metal molybdenum disc to remove the oxide layer, and use W0.5 diamond polishing agent to polish it into a mirror surface, place it in acetone for ultrasonic cleaning for 10 minutes, transfer to ethanol for ultrasonic cleaning for 5 minutes, and dry it for later use;

[0071] (2) Substrate seed crystal: 1g of nano-diamond powder (particle size: 40nm) was evenly and densely spread on the surface of metal molybdenum disk with a diameter of 10cm, mechanically ground for 5min, and then the surface was blown clean with nitrogen gas for later use.

[0072] (3) CVD coating: put the base material after the above seed crystal into the reaction chamber, reduce the vacuum degree in the furnace to 10 -4 Below Pa, start to feed the reaction gas for coating. The heat source is provided by tungsten wire, (CH 3...

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Abstract

The invention provides a self-supporting boron-doped diamond electrochemical sensor and a preparation method and application thereof. The preparation method of the self-supporting boron-doped diamondelectrochemical sensor comprises the following steps: 1) taking nano-diamond powder as a seed crystal seed material, uniformly paving the seed crystal seed material on the surface of a pretreated metal substrate, and mechanically performing grinding to obtain a seed-crystallized metal substrate; (2) coating a film on the metal base material subjected to seed crystal by utilizing a hot wire chemical vapor deposition technology, wherein in the diamond nucleation stage, methane is used as a carbon source, and hydrogen is used as etching gas; in the diamond growth stage, ethanol is used as a carbon source, and trimethyl borate is used as a boron source; and 3) performing demolding and packaging to obtain the self-supporting boron-doped diamond electrochemical sensor. The self-supporting boron-doped diamond electrochemical sensor provided by the invention can meet the accurate long-acting detection requirement of an online monitoring system on the sensor, effectively overcomes the defect ofshort service life of a BDD film sensor, and has the application potential of online monitoring of heavy metal ions, especially Pb < 2 + >, in a water body.

Description

technical field [0001] The invention relates to the technical field of water body monitoring, and more specifically, to a self-supporting boron-doped diamond electrochemical sensor, a preparation method and application thereof. Background technique [0002] Pb in aquatic ecosystems 2+ The risk of pollution continues to increase, requiring detection and sensing devices to meet the performance requirements of accurate and long-term detection to achieve online monitoring of heavy metal pollutants. Compared with other heavy metal ions, Pb 2+ Because of its rapid enrichment process and serious toxicity characteristics, it has become the focus of water quality environment monitoring. Pb 2+ It will also accumulate in aquatic organisms and endanger human health through the action of the food chain. [0003] Online monitoring of Pb in water by anodic stripping voltammetry 2+ It is the only way to prevent water pollution. Unfortunately, the BDD film electrodes used in the current...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30G01N27/333G01N27/48C23C16/27
CPCG01N27/333G01N27/48C23C16/27Y02A20/20
Inventor 于翔裴敬轩赵斌杨成武刘兴举
Owner CHINA UNIV OF GEOSCIENCES (BEIJING)
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