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A kind of precious metal ultramicro electrode and preparation method thereof

A technology of ultra-micro electrodes and precious metals, applied in the field of electrochemistry, can solve the problems of uncontrollable electrode size and shape, cumbersome preparation process of ultra-micro electrodes, etc., and achieve the effects of promoting and applying, low cost, and reducing preparation costs

Inactive Publication Date: 2016-06-22
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the defects of cumbersome preparation process and uncontrollable electrode size and morphology in the prior art, a noble metal ultramicro electrode and its preparation method are provided to obtain a noble metal ultramicro electrode with controllable size, shape and yield

Method used

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  • A kind of precious metal ultramicro electrode and preparation method thereof
  • A kind of precious metal ultramicro electrode and preparation method thereof

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preparation example Construction

[0029] The preparation method of the precious metal ultramicro electrode of the present invention includes the following steps:

[0030] S1. A clean borax glass tube with a length of 100mm, an inner diameter of 1mm, and an outer diameter of 2mm is vertically fixed on the needle puller and heated by tungsten wires. The length is 110mm, the inner diameter of the middle part is 40μm-60μm, and the outer diameter is 130μm-150μm. Borax glass tube;

[0031] S2. Use a glass knife to cut the middle of the borax glass tube drawn in step S1 to obtain two capillary glass tubes with an inner diameter of 40 μm-60 μm and an outer diameter of 130 μm-150 μm at the tip. At the same time, place the tip of the capillary glass tube Burn the outer flame of the alcohol lamp for 0.3 seconds to seal the tip end;

[0032] S3. Feed the precious metal wire with a length of 15mm and a diameter of 25μm or 10μm vertically into the bottom end of the needle tip of the capillary glass tube made in (2), and place it ...

Embodiment 1

[0043] The first embodiment is the preparation method of platinum ultramicro electrode. The preparation method of the platinum ultramicro electrode of this embodiment includes the following steps:

[0044] Step 1: Put the borax glass tube with a length of 100mm, an outer diameter of 2mm, and an inner diameter of 1mm in 0.1MHNO 3 The solution, deionized water, acetone solution, and deionized water are sonicated for 30 minutes, and then placed in a vacuum drying oven, and vacuum dried at 80°C for 24 hours;

[0045] Step 2: Fix the clean borax glass tube prepared in step 1 vertically on the needle puller, and ensure that the heating place of the tungsten wire is located in the axial center of the borax glass tube. The borax glass tube adopts a two-step drawing method, the initial drawing temperature is set to 100℃, the second drawing temperature is 90℃, and the stretching distance is 5mm each time. Start the needle drawing instrument and follow the preset program. The glass tube will...

Embodiment 2

[0054] The difference from the first embodiment is that in this embodiment, the method for preparing the platinum ultramicro electrode includes the following steps:

[0055] Step 1: Put the borax glass tube with a length of 100mm, an outer diameter of 2mm, and an inner diameter of 1mm in 0.1MHNO 3 The solution, deionized water, acetone solution, and deionized water are sonicated for 30 minutes, and then placed in a vacuum drying oven and vacuum dried at 80°C for 24 hours;

[0056] Step 2: Fix the clean borax glass tube prepared in step 1 vertically on the needle puller, and ensure that the heating place of the tungsten wire is located in the axial center of the borax glass tube. The borax glass tube adopts a two-step drawing method. The initial drawing temperature is set to 100℃, the second drawing temperature is 90℃, and the stretching distance is 5mm each time. Start the needle drawing instrument and follow the preset program. The glass tube will be drawn into three sections, the...

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Abstract

The invention discloses a noble metal ultramicro electrode and a preparation method thereof. The method comprises: drawing a borax glass tube into a capillary glass tube with the inner diameter of the tip portion being 40-60 [mu]m and carrying out seal processing on a tip mouth the capillary glass tube; putting a noble metal wire to the bottommost end of the needle tip of the capillary glass tube to carry out fusion processing, thereby enabling the lower half portion of the noble metal wire to be fused into one body with the needle tip portion of the capillary glass tube; putting a pure copper wire into the capillary glass tube, the copper wire and the noble metal wire being bonded through silver slurry and being in good conductive contact through the function of the high temperature solidification of the silver slurry; utilizing epoxy resin to seal the other end of the capillary glass tube, reserving 5mm length, extending out of the tip portion of the capillary glass tube, of the copper wire to serve as an electrode pin, and performing drying to obtain the ultramicro electrode; and polishing and grinding the ultramicro electrode to enable the ratio between the radius of the tip portion of the capillary glass tube and the radius of the noble metal to be 10. The preparation method can effectively control the size and shape of the surface of the noble metal ultramicro electrode; the yield of the noble metal ultramicro electrode is improved; and preparation cost is reduced.

Description

Technical field [0001] The invention relates to the technical field of electrochemistry, in particular to a precious metal ultramicro electrode and a preparation method thereof. Background technique [0002] Scanning Electrochemical Microscopy (SECM) is a scanning probe microscope technology proposed and developed by the group of internationally renowned electrochemists A.J. Bard in the late 1980s. It is based on the development of ultramicroelectrodes (UME) in the late 1970s and scanning tunneling microscope (STM) in the early 1980s, a new type of electrochemical field detection with a resolution between ordinary optical microscopes and STM technology. Unlike STM and atomic force microscopy (AFM) technology, SECM makes up for the lack of electrochemical information provided by STM. SECM works based on the principle of electrochemistry. It can measure the electrochemical current given by the oxidation or reduction of substances in the microzone. The samples to be tested can be ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01Q60/60G01N27/30
Inventor 申燕张炳雁张晓凡王鸣魁
Owner HUAZHONG UNIV OF SCI & TECH