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A method for preparing metal homogenous and hybrid ultrafine electrodes by carbon template and electroplating

A technology of ultra-micro electrodes and carbon templates, applied in the field of analytical chemistry, can solve the problems of poor preparation repeatability, single signal, and obstacles to wide application, and achieve the effect of simple method and high success rate

Active Publication Date: 2022-06-07
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A method for preparing metal homogenous and hybrid ultrafine electrodes by carbon template and electroplating
  • A method for preparing metal homogenous and hybrid ultrafine electrodes by carbon template and electroplating
  • A method for preparing metal homogenous and hybrid ultrafine electrodes by carbon template and electroplating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Preparation of silanized carbon deposition templates.

[0044] Pull the quartz double tube into an empty tube of the desired size, fix it at the end of the butane tube, fill the tube with butane gas (purity 99.9%, butane gas pressure 0.03 MP), and then Insert into the quartz protective sleeve (quartz single tube) on the opposite side, and 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 alcohol burner is used for heating for 60 s~200 s. The specific heating time depends on the size of the pipe diameter, that is, the tip required in the first step is not The fully plugged ultrafine carbon electrode is called a carbon template, and subsequent electrodeposition experiments are completed on this template.

[0045] In order to prevent the random growth of nanoparticles to the outer wall, the DCE solution of trim...

Embodiment 2

[0047] The above silanized carbon template was inserted into a potassium chloride solution containing 1 mM chloroauric acid, and AuCl was determined by cyclic voltammetry 4 ‒ the reduction potential (such as image 3 a), the results show that AuCl 4 ‒ It begins to reduce to gold when it is lower than 0 V. like image 3 As shown in b, during the potentiostatic plating process, the first AuCl 4 ‒ It is reduced to gold on the carbon layer, and as the gold gradually covers the carbon layer, the AuCl diffuses to the surface of the gold. 4 ‒ It began to grow gradually on the gold element, and after a period of time, the gold nanoparticles filled the entire pore channel; when the electrodeposition continued, the current increased rapidly as the nanoparticles grew outward, indicating that the gold nanoparticles just filled the pipe completely. on both sides of the double tube figure 2 The electroplating process shown, after the electroplating is finished, the preparation is ...

Embodiment 3

[0051] Pull the quartz double tube into an empty tube of the required size, fix it at the end of the butane pipe, fill the pipe with butane gas, and then insert it into the quartz protective sleeve on the opposite side, at this time It is not necessary to pass nitrogen gas into the protective sleeve of the tube, and it is heated with the outer flame of an alcohol lamp or an alcohol burner for 60 s~200 s. The specific heating time depends on the size of the tube diameter, that is, the carbon blank at the tip required for the first step is prepared. Template and silanization of the outer wall.

[0052] The above preparation process is as figure 1 shown.

[0053] The electrode prepared above was inserted into a potassium chloride solution containing 2 mM chloroplatinic acid, and the electroplating potential was determined according to its reduction potential in the solution, at which the chloroplatinate ion in the solution would be reduced to platinum nanoparticles. The particl...

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Abstract

The invention discloses a method for preparing metal hybrid and homogeneous ultramicro electrodes by using carbon template and electroplating method. The method can prepare single-tube ultrafine metal electrodes including gold, platinum, mercury, etc., and double-channel hybrid and homogeneous ultrafine metal electrodes with different (or the same) metal materials on both sides. Firstly, micro-nano-scale quartz double tubes are drawn according to the needs of the experiment, and then high-temperature cracking and deposition of butane is performed on the dual channels of the quartz tubes to prepare incompletely sealed carbon templates. Since no special attention to nitrogen protection is required, the method has greatly reduced requirements on operation and environment. On this basis, we inserted it into a metal electrolyte containing a certain concentration, determined the reduction potential and performed constant potential electroplating, and finally obtained various metal ultramicro electrodes with dense and flat filling tips. Since the outer wall is silanized, metal growth outside the tube is prevented. Electrochemical techniques and surface analysis techniques were used to characterize the prepared electrodes.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for preparing ultra-micro homogeneous and hybrid electrodes by using a carbon template method and an electroplating method. Background technique [0002] Since the late 1970s, ultra-micro electrodes (UMEs, also known as micro-nano electrodes) have been introduced into the field of electroanalytical chemistry, which has led to revolutionary changes in the field. Not only can it be used to obtain kinetic parameters of electrochemical reactions, but its size characteristics enable many studies in biological systems that would otherwise be impossible. For example, ultrafine electrodes 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, the preparation of ultrafine electrodes is usually difficult, which cannot be mass-produced, and the repeatability of p...

Claims

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Application Information

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Patent Type & Authority Patents(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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