Method for preparing metal homogeneous and hybrid ultramicro electrode by using carbon template and electroplating method

An ultra-micro electrode and carbon electrode technology, applied in the field of analytical chemistry, can solve the problems of poor preparation repeatability, single signal, and inability to mass-produce, and achieve the effect of high success rate and simple method

Active Publication Date: 2021-09-14
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, ultramicroelectrodes are usually difficult to prepare, cannot be mass-produced, and the repeatability of preparation is poor, which seriously hinders their wide application.
And the traditional ultra-micro electrode is often a single electrode, which can only get a single signal, which also affects the application range of this type of electrode to a large extent.

Method used

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  • Method for preparing metal homogeneous and hybrid ultramicro electrode by using carbon template and electroplating method
  • Method for preparing metal homogeneous and hybrid ultramicro electrode by using carbon template and electroplating method
  • Method for preparing metal homogeneous and hybrid ultramicro electrode by using carbon template and electroplating method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1, the preparation of silanized carbon deposition template

[0043] Draw the quartz double tube into an empty tube of the required size, fix it at the end of the butane pipeline, make the pipeline full of butane gas (purity is 99.9%, butane gas pressure is 0.03MP), and then put it Inserted into the quartz protective sleeve (quartz single tube) on the opposite side, the inserted micro-nano tip accounts for about one-twentieth of the entire micro-nano tube. At this time, nitrogen does not need to be introduced into the protective sleeve, and the outer flame of an alcohol lamp or an alcohol blowtorch is used for heating for 60s to 200s. The specific heating time depends on the diameter of the tube, that is, the tip required for the first step is not completely blocked. The living ultra-fine carbon electrode is called a carbon template, and the subsequent electrodeposition experiments are all completed on this template.

[0044]In order to prevent the irregular ...

Embodiment 2

[0046] The above silanized carbon template was inserted into the potassium chloride solution containing 1mM chloroauric acid, and AuCl was determined by cyclic voltammetry. 4 - The reduction potential (such as image 3 a), the results show that AuCl 4 - When it is lower than 0V, it starts to be reduced to simple gold. Such as image 3 As shown in b, in the constant potential plating process, first AuCl 4 - It is reduced to gold on the carbon layer, and as the gold gradually covers the carbon layer, the AuCl diffused to the surface of the gold 4 - It began to grow gradually on the gold simple substance, and after a period of time, the gold nanoparticles filled the entire channel; continued electrodeposition, and the current increased rapidly as the nanoparticles grew outward, indicating that the gold nanoparticles just completely filled the channel. on both sides of the double tube figure 2 As shown in the electroplating process, after the electroplating is finished, ...

Embodiment 3

[0050] Draw the quartz double tube into an empty tube of the required size, fix it at the end of the butane pipeline, fill the pipeline with butane gas, and then insert it into the quartz protective sleeve on the opposite side, at this time There is no need to feed nitrogen gas into the protective sleeve, and heat it with an alcohol lamp or the outer flame of an alcohol blowtorch for 60s to 200s. The specific heating time depends on the size of the tube diameter, that is, to prepare the blank carbon template at the tip required for the first step and Silanize the outer wall.

[0051] The above preparation process is as figure 1 shown.

[0052] Insert the electrode prepared above into the potassium chloride solution containing 2mM chloroplatinic acid, and determine the electroplating potential according to its reduction potential in the solution, at which potential, the chloroplatinate ions in the solution will be reduced to platinum nanoparticles Inside the quartz tube, stop...

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Abstract

The invention discloses a method for preparing a metal hybrid and homogeneous ultramicro electrode by using a carbon template and an electroplating method. The method can be used for preparing single-tube ultramicro metal electrodes such as gold, platinum, mercury and the like and double-channel hybrid and homogeneous ultramicro metal electrodes made of different (or same) metal materials on the two sides. The method comprises the following steps: firstly, drawing micro-nano quartz double tubes according to experimental requirements, and then carrying out butane high-temperature cracking deposition on double channels of the quartz tubes to prepare an incompletely sealed carbon template. As nitrogen protection does not need to be specially paid attention to, the requirements of the method on operation and environment are greatly reduced. On the basis, the electrode is inserted into a metal electrolyte with a certain concentration, constant-potential electroplating is carried out after the reduction potential is determined, and finally various metal ultramicroelectrodes with compact and flat filling tips are obtained. As the outer wall is silanized, metal is prevented from growing outside the tubes. The prepared electrode is characterized by adopting an electrochemical technology and a surface analysis technology.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for preparing ultramicro homogeneous and hybridized electrodes by using a carbon template method and an electroplating method. Background technique [0002] Since the late 1970s, ultramicroelectrodes (UMEs, also known as micro-nano electrodes) have been introduced into the field of electroanalytical chemistry and have triggered revolutionary changes in this field. It can not only be used to obtain the kinetic parameters of electrochemical reactions, but also make use of its size characteristics to make possible many researches in biological systems that could not be done otherwise. For example, ultra-microelectrodes can be inserted into cells without destroying the physiological activity of cells, so as to dynamically monitor the changes inside cells in real time. However, ultramicroelectrodes are usually difficult to prepare, cannot be mass-produced, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C17/00C03C17/06C03C17/22C03C17/30C03C17/36C03C23/00C25D3/52C25D3/54G01N27/48
CPCC03C17/004C03C17/22C03C23/00C03C17/005C03C17/30C03C17/06C03C17/3607C03C17/3649C25D3/52C25D3/54G01N27/48
Inventor 邵元华聂鑫刘俊杰邵毅詹佶睿
Owner PEKING UNIV
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