Method for preparing size-controllable nanoneedle type electrode

A nano-electrode and nano-needle technology, which is applied in the field of electrode preparation and electroanalytical chemistry, can solve the problems of numerous operation steps and uncontrollable nano-electrode size, and achieve the effects of simple operation, low cost and extended service life

Pending Publication Date: 2022-01-04
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing preparation method has many steps, and the size of the prepared nano-electrode is uncontrollable. Therefore, it is of great application significance to develop a new preparation method of nano-needle electrodes.

Method used

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  • Method for preparing size-controllable nanoneedle type electrode
  • Method for preparing size-controllable nanoneedle type electrode
  • Method for preparing size-controllable nanoneedle type electrode

Examples

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Embodiment 1

[0031] A method for preparing a size-controllable gold nanometer needle electrode, comprising the steps of:

[0032] 1) Place the borosilicate capillary in ethanol solution to remove impurities in the tube by ultrasonic. The inner diameter of the capillary is 0.2mm and the outer diameter is 1.0mm. Use a gold wire with a purity of 99.95%, a diameter of 50 μm, and a length of 2 cm. It penetrates into a borosilicate capillary with a length of 10 cm. The position of the gold wire is in the middle of the capillary. The smaller the size difference between the selected gold wire and the inner diameter of the capillary, the better the gold wire in the drawing process. The better the fit with the capillary.

[0033] 2) Install the capillary with gold wire in step 1) in a Sutter-P2000 laser drawing machine for pre-drawing operation, the purpose is to thin the middle part of the capillary so that the gap between it and the internal gold wire becomes smaller. The pre-drawing program is: ...

Embodiment 2

[0043] A method for preparing size-controllable platinum nano-needle electrodes, comprising the steps of:

[0044] 1) Borosilicate capillary inner diameter = 0.6 mm, outer diameter = 1.0 mm. A platinum wire with a purity of 99.95%, a diameter of 50 μm, and a length of 2 cm is used to penetrate into a borosilicate capillary with a length of 10 cm, and the platinum wire is located in the middle of the capillary.

[0045] 2) Pre-draw the capillary tube with platinum wire in step 1, the pre-drawing procedure is: HEAT=450W, FIL=4, VEL=15, DEL=120, PULL=0, the laser signal light flashes 3 times and then turns off Program, natural cooling for 60 seconds.

[0046] 3) The fusion program is: HEAT=400, FIL=4, VEL=15, DEL=120, PULL=0. Stop the program after timing 7s after starting, and cool down naturally for 60 seconds.

[0047] 4) Perform hard pulling operation on the capillary in step 3), hard pulling procedure: HEAT=400, FIL=4, VEL=33, DEL=120, PULL=90.

[0048] 5) Perform precis...

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Abstract

The invention provides a method for preparing the size-controllable nanoneedle type electrode, a laser drawing instrument is used for preparation, and compared with an existing nanoelectrode preparation technology, the size of a glass tube, drawing parameters, the drawing process and the electrode polishing end point are selected and designed. And the gold and platinum nano electrode with controllable electrode size is obtained by using a simpler and more effective method. And the fitting and melting conditions of the metal wire in the capillary tube in each drawing step are observed through a metallographic microscope, an electrode polishing end point feedback circuit is designed, and the polishing size of the electrode is accurately monitored. A piranha solution is used for treating the surface of the polished electrode, a scanning electron microscope (SEM) is combined for characterizing the accurately polished electrode, the apparent size of the nanoelectrode is tested through limiting current cyclic voltammetry, and the electrode with the minimum size of 6.4 nm can be prepared. And the size of the electrode is not changed after multiple cyclic voltammetry tests, so that the electrode prepared by the method has relatively high stability.

Description

technical field [0001] The invention relates to the field of electroanalytical chemistry and electrode preparation, in particular to a nano-needle electrode and a preparation method thereof. Background technique [0002] Electrochemistry is a special field. In theory, electrochemistry itself is a nanoscience, which studies the surface / interface process of the electric double layer with a thickness of nanometer and subnanometer. The small size of nanoelectrodes determines their specific electrochemical properties, which are quite different from the electrochemical behavior observed on macroscopic electrodes. Nanoelectrodes have a very high electrochemical response speed, and can quantitatively study the kinetics of heterogeneous electron transfer reactions without the limitation of mass transfer, which provides a new way for the study of nanoscale electrochemical properties and processes. [0003] Nanoelectrodes are increasingly used in electrochemical scanning probe techniq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30
CPCG01N27/30
Inventor 张香平王宗旭白璐董海峰李紫欣江重阳
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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