CN101122575A - Complex film modified nickel electrode preparation method - Google Patents
Complex film modified nickel electrode preparation method Download PDFInfo
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- CN101122575A CN101122575A CNA2007101394301A CN200710139430A CN101122575A CN 101122575 A CN101122575 A CN 101122575A CN A2007101394301 A CNA2007101394301 A CN A2007101394301A CN 200710139430 A CN200710139430 A CN 200710139430A CN 101122575 A CN101122575 A CN 101122575A
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Abstract
A composite membrane modified nickel electrode preparation method takes a nickel electrode as a modified basement, a platinum wire as a counter electrode and Ag/AgCl as a reference electrode. The nickel electrode, the platinum wire and Ag/AgCl are immersed in 0.1-2.0mol/L sodium hydroxide solution at the same time at room temperature and are modified through a cyclic voltammetry method. An ethanol solution containing five percent of Nafion is added with anhydrous alcohol for dilution. And a solution containing 0.1-0.5 percent of Nafion is obtained. 0.2-0.3mg carbon nano-tube is weighted and added into the solution. Ultrasonic vibration is implemented on the solution for 20-40min. Then, a micro-sampler is used to fetch a drop of 8-12Mu L to be coated on the finished nickel electrode surface, which is dried under a infrared lamp. And a composite membrane modified nickel electrode is obtained. A methane electrochemical sensor assembled with the electrode has the advantages of good stability and high flexibility. And the methane can be detected in solution.
Description
Technical field
The present invention relates to electrode, specifically belong to a kind of method at nickel electrode finishing composite membrane.
Background technology
Methane is the principal ingredient of mine gas, but is the distinctive flammable explosive gas in colliery, is the significant threat of Safety of Coal Mine Production.At present, the coal mine safety monitoring system of China's equipment mostly adopts principle of catalyst combustion to detect methane, exists weak point in serviceable life, poor work stability and adjustment to proofread and correct frequent shortcoming always.For this reason, press for the product and the method for the new control gas disaster of development.
It is little, highly sensitive, simple to operate, cheap and can be used for advantage such as field monitoring that electrochemical sensor has a volume, so in existing all kinds of gas detection equipments at present, electrochemical sensor occupies very consequence.
Electrochemistry Communications in 2003 5 volume 184-188 pages or leaves have reported that the nickel electrode of having modified nickel hydroxide can catalytic oxidation methane in alkaline solution, but the remolding sensitivity of this electrode detection methane is lower, poor stability.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of complex film modified nickel electrode, the modified nickel electrode of this method preparation will have advantages of high catalytic activity to methane, and it is highly sensitive to be used to measure methane, good stability.
The preparation method of a kind of complex film modified nickel electrode provided by the invention comprises the steps:
(1) be to modify substrate with the nickel electrode, platinum filament is to electrode, Ag/AgCl is a contrast electrode, at room temperature they are immersed in the sodium hydroxide solution of 0.1-2.0mol/L simultaneously, modify with cyclic voltammetry, condition is: potential windows 0.1V-0.6V, sweep velocity 0.1V/s, continuous sweep 20-60 minute, take out nickel electrode and wash with redistilled water, dry naturally;
(2) ethanolic solution of 5%Nafion is added the absolute ethyl alcohol dilution and obtain 0.1%-0.5%Nafion solution, taking by weighing 0.2-0.3 milligram carbon nano-tube adds in the above-mentioned solution, sonic oscillation 20-40 minute, getting 8-12 μ L with microsyringe then drips and is coated in the nickel electrode surface that step (1) is finished, under infrared lamp, dry, obtain stable complex film modified nickel electrode.
The concentration of described sodium hydroxide solution is preferably 1.0mol/L.The described continuous sweep time is preferably 30-60 minute.Described preparation process is at room temperature carried out.
The present invention utilizes the high-efficiency catalytic activity of high price nickel ion to methane, the characteristic and the effect of Nafion selective enrichment of structure, chemical property and the adsorbed gas that the combined carbon nanotube is peculiar simultaneously greatly improved the sensitivity and the stability of assay determination methane.The resulting complex film modified electrode pair methane of the present invention has advantages of high catalytic activity.This electrode is placed in the 1.0mol/L sodium hydroxide solution, just can realizes two electronics oxidations of methane.
Complex film modified nickel electrode of the present invention surface, the preparation method is simple, quick, easy to operate, modifies mild condition, and required medicine is commercially available, and raw material is easy to get.And the composite membrane of modifying is highly stable, can realize two electronics oxidations to methane.It is highly sensitive to measure methane with this modified electrode, good stability.
Description of drawings:
Fig. 1 surveys the comparison diagram of the cyclic voltammogram of methane for nickel electrode of modifying nickel hydroxide and the nickel electrode of modifying composite membrane.A modifies the cyclic voltammogram that the nickel electrode of nickel hydroxide is surveyed methane for pressing document among the figure, and b modifies the cyclic voltammogram of the nickel electrode survey methane of composite membrane for the present invention.
Embodiment
Embodiment 1:
(1) be to modify substrate with the nickel electrode, platinum filament is to electrode, Ag/AgCl is a contrast electrode, at room temperature they are immersed in the sodium hydroxide solution of 1.0mol/L simultaneously, modify with cyclic voltammetry, condition is: potential windows 0.1V-0.6V, sweep velocity 0.1V/s, continuous sweep 30 minutes is taken out nickel electrode and is washed with redistilled water, dries naturally;
(2) ethanolic solution of 5%Nafion is added the absolute ethyl alcohol dilution and obtain 0.1%Nafion solution, taking by weighing 0.2 milligram of carbon nano-tube adds in the above-mentioned solution, sonic oscillation 20 minutes, getting 8 μ L with microsyringe then drips and is coated in the nickel electrode surface that step (1) is finished, under infrared lamp, dry, obtain stable complex film modified nickel electrode.
The peak current that utilizes complex film modified nickel electrode to detect methane increases greatly, has improved the sensitivity (see figure 1) that detects methane.After electrode was placed a week, the peak current that detects methane did not have to change substantially.
Embodiment 2:
(1) continuous sweep is 40 minutes, and other is with embodiment 1;
(2) ethanolic solution of 5%Nafion is added the absolute ethyl alcohol dilution and obtain 0.2%Nafion solution, taking by weighing 0.2 milligram of carbon nano-tube adds in the above-mentioned solution, sonic oscillation 20 minutes, getting 9 μ L with microsyringe then drips and is coated in the nickel electrode surface that step (1) is finished, under infrared lamp, dry, obtain stable complex film modified nickel electrode.
Embodiment 3:
(1) continuous sweep is 50 minutes, and other is with embodiment 1;
(2) ethanolic solution of 5%Nafion is added the absolute ethyl alcohol dilution and obtain 0.4%Nafion solution, taking by weighing 0.3 milligram of carbon nano-tube adds in the above-mentioned solution, sonic oscillation 25 minutes, getting 10 μ L with microsyringe then drips and is coated in the nickel electrode surface that step (1) is finished, under infrared lamp, dry, obtain stable complex film modified nickel electrode.
Embodiment 4:
(1) continuous sweep is 35 minutes, and other is with embodiment 1;
(2) ethanolic solution of 5%Nafion is added the absolute ethyl alcohol dilution and obtain 0.2%Nafion solution, taking by weighing 0.3 milligram of carbon nano-tube adds in the above-mentioned solution, sonic oscillation 30 minutes, getting 11 μ L with microsyringe then drips and is coated in the nickel electrode surface that step (1) is finished, under infrared lamp, dry, obtain stable complex film modified nickel electrode.
Claims (4)
1. the preparation method of a complex film modified nickel electrode is characterized in that, comprises the steps:
(1) be to modify substrate with the nickel electrode, platinum filament is to electrode, Ag/AgCl is a contrast electrode, at room temperature they are immersed in the sodium hydroxide solution of 0.1-2.0mol/L simultaneously, modify with cyclic voltammetry, condition is: potential windows 0.1V-0.6V, sweep velocity 0.1V/s, continuous sweep 20-60 minute, take out nickel electrode and wash with redistilled water, dry naturally;
(2) ethanolic solution of 5%Nafion is added the absolute ethyl alcohol dilution and obtain 0.1%-0.5%Nafion solution, taking by weighing 0.2-0.3 milligram carbon nano-tube adds in the above-mentioned solution, sonic oscillation 20-40 minute, getting 8-12 μ L with microsyringe then drips and is coated in the nickel electrode surface that step (1) is finished, under infrared lamp, dry, obtain stable complex film modified nickel electrode.
2. the preparation method of electrode according to claim 1 is characterized in that the concentration of described sodium hydroxide solution is 1.0mol/L.
3. the preparation method of electrode according to claim 1 is characterized in that the described continuous sweep time is 30-60 minute.
4. the preparation method of electrode according to claim 1 is characterized in that described preparation process is at room temperature carried out.
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CN200710139430A CN100580441C (en) | 2007-09-13 | 2007-09-13 | Complex film modified nickel electrode preparation method |
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CN200710139430A CN100580441C (en) | 2007-09-13 | 2007-09-13 | Complex film modified nickel electrode preparation method |
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CN100580441C CN100580441C (en) | 2010-01-13 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105712448A (en) * | 2016-02-26 | 2016-06-29 | 东华大学 | Preparation method of Nafion/porous carbon composite electrode material for capacitive adsorption desalting |
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2007
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105712448A (en) * | 2016-02-26 | 2016-06-29 | 东华大学 | Preparation method of Nafion/porous carbon composite electrode material for capacitive adsorption desalting |
CN105712448B (en) * | 2016-02-26 | 2018-10-23 | 东华大学 | A kind of preparation method of the capacitive adsorption desalination porous carbon composite electrode materials of Nafion/ |
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