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Method for preparing iridium/iridium oxide pH electrode through supercritical treatment

A supercritical, iridium oxide technology, applied in the direction of material electrochemical variables, material analysis by electromagnetic means, instruments, etc., can solve problems such as insufficient hydration degree, electrode potential drift, limited application, etc., to achieve reproducibility and Enhanced sensitivity, stable electrode performance, and good thermal stability

Inactive Publication Date: 2020-03-17
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional hydration process is to immerse the electrode in water at room temperature, but the cycle of the traditional method is relatively long, the degree of hydration is not sufficient in a short period of time, the electrode potential drifts seriously, and the reproducibility of multiple tests is poor and it is easy to detach. film, thus greatly limiting its practical application

Method used

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  • Method for preparing iridium/iridium oxide pH electrode through supercritical treatment
  • Method for preparing iridium/iridium oxide pH electrode through supercritical treatment
  • Method for preparing iridium/iridium oxide pH electrode through supercritical treatment

Examples

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Effect test

Embodiment 1

[0016] Step 1: Polish a section of 2cm long iridium wire with sandpaper, and ultrasonically clean it in 2M hydrochloric acid solution, acetone and ultrapure water respectively; then, immerse the iridium wire in potassium nitrate and In the powder of sodium nitrate, the temperature was programmed to rise to 800°C at 5°C / min in a tube furnace, and the temperature was kept constant for 45 minutes;

[0017] Step 2: Put the iridium / iridium oxide pH electrode prepared in step 1 into a supercritical device, and treat it in a supercritical environment at 300°C and 30Mpa for 5 hours. Scrape off the oxide film with a length of about 1 mm at one end of the obtained electrode to obtain an iridium / iridium oxide pH electrode.

Embodiment 2

[0019] Step 1: A section of 3cm long iridium wire was polished bright with sandpaper, and ultrasonically cleaned in 4M hydrochloric acid solution, acetone and ultrapure water respectively; subsequently, the iridium wire was immersed in potassium nitrate and In the powder of sodium nitrate, the temperature was programmed to rise to 600°C at 3°C / min in a tube furnace, and the temperature was kept constant for 45min;

[0020] Step 2: Put the iridium / iridium oxide pH electrode prepared in step 1 into a supercritical device, and treat it in a supercritical environment at 300°C and 30Mpa for 5 hours. The oxide film with a length of about 2 mm was scraped off one end of the obtained electrode to obtain an iridium / iridium oxide pH electrode.

Embodiment 3

[0022] Step 1: A section of 4cm long iridium wire is polished bright with sandpaper, and ultrasonically cleaned in 3M hydrochloric acid solution, acetone and ultrapure water respectively; subsequently, the iridium wire is placed in potassium nitrate and Cover with sodium nitrate powder; program the temperature to 800°C at 5°C / min in a tube furnace, and keep the temperature constant for 45min;

[0023] Step 2: Put the iridium / iridium oxide pH electrode prepared in step 1 into a supercritical device, and treat it in a supercritical environment at 400°C and 40Mpa for 3 hours. The oxide film with a length of about 2 mm was scraped off one end of the obtained electrode to obtain an iridium / iridium oxide pH electrode.

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Abstract

The invention discloses a method for preparing an iridium / iridium oxide pH electrode through supercritical treatment. The method comprises the following steps: preparing the iridium / iridium oxide pH electrode through thermal oxidation, and treating for 3-5 hours in a supercritical environment of 300-400 DEG C and 30-40 MPa. The electrode subjected to supercritical treatment has the advantages of high sensitivity, fast response, good reproducibility, low hysteresis quality, high stability and the like. The problems of long hydration time, low efficiency, poor stability, demolding and the like of the iridium / iridium oxide pH electrode for a long time are effectively solved. The electrode improved by the method can be well applied under the condition of normal temperature, and the stability of the electrode can also be kept under the conditions of high temperature such as supercritical conditions and hot liquid ports.

Description

technical field [0001] The invention relates to the technical field of sensor analysis and testing, in particular to a method for preparing an iridium / iridium oxide pH electrode by supercritical treatment. Background technique [0002] The iridium / iridium oxide pH electrode has attracted wide attention because of its small size, easy fabrication, wide pH response range, good response stability, and can be used in corrosive environments. Common methods for preparing iridium / iridium oxide pH electrodes include electrochemical cyclic voltammetry, electrodeposition, sputtering, and thermal oxidation. Among them, the thermal oxidation method is widely used because of its simple preparation process, low cost, dense oxide, good adhesion of the oxide film layer, and convenience for mass production. However, for electrodes prepared by thermal oxidation, the surface oxide film is a dry film, and some even have mud-like cracks, surface stress and defects, which are common phenomena in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30
CPCG01N27/302
Inventor 李强戴梦婷王冰李鑫缪佳燕王文慧衡月容于翠艳
Owner EAST CHINA NORMAL UNIV
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