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A kind of preparation method of calcium-doped silicon nitride graphene paste electrode sensor

An electrode sensor, silicon nitride technology, applied in the field of electrochemical analysis, can solve the problems of poor conductivity, low sensitivity, poor stability, etc., and achieve the effects of low cost, improved sensitivity, and easy surface

Active Publication Date: 2021-05-04
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, carbon paste electrodes also have some disadvantages, such as poor conductivity, low sensitivity, poor stability, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Preparation of gold-modified silicon nitride: In the reactor, add ethanol: 68 mL, 3-mercaptopropyltriethoxysilane: 26 g, stir well, then add nano-silicon nitride: 20 g, in 50±2℃ constant temperature, stirring, reflux reaction for 5h, after cooling, separate the solid and liquid, wash with deionized water until neutral, dry, put the solid into 0.01mol / L gold solution according to the solid-liquid ratio of 1g:15~25mL Soak for 6 h, separate solid and liquid, wash with deionized water until neutral, and dry to obtain gold-modified silicon nitride;

[0027] (2) Calcium-doped carbon-containing quantum dot adhesive: In the reaction kettle, add 1-butyl-3-methylimidazole p-toluenesulfonate: 69g, calcium gluconate: 9g, absorbent cotton: 22g, Stir evenly, seal, place in an oven at 110±2°C, react at a constant temperature for 9 hours, and cool to room temperature to obtain a light yellow viscous liquid that is calcium-doped carbon-containing quantum dot adhesive;

[0028] (3) ...

Embodiment 2

[0031](1) Preparation of gold-modified silicon nitride: In the reactor, add ethanol: 66 mL, 3-mercaptopropyltriethoxysilane: 27 g, stir well, then add nano-silicon nitride: 21 g, in 50±2℃ constant temperature, stirring, reflux reaction for 5h, after cooling, separate the solid and liquid, wash with deionized water until neutral, dry, put the solid into 0.01mol / L gold solution according to the solid-liquid ratio of 1g:15~25mL Soak for 6 h, separate solid and liquid, wash with deionized water until neutral, and dry to obtain gold-modified silicon nitride;

[0032] (2) Calcium-doped carbon-containing quantum dot adhesive: In the reaction kettle, add 1-butyl-3-methylimidazole p-toluenesulfonate: 70g, calcium gluconate: 10g, absorbent cotton: 20g, Stir evenly, seal, place in an oven at 110±2°C, react at a constant temperature for 8 hours, and cool to room temperature to obtain a light yellow viscous liquid that is calcium-doped carbon-containing quantum dot adhesive;

[0033] (3) ...

Embodiment 3

[0036] (1) Preparation of gold-modified silicon nitride: In the reactor, add ethanol: 71 mL, 3-mercaptopropyltriethoxysilane: 24 g, stir well, then add nano-silicon nitride: 20 g, in 50±2℃ constant temperature, stirring, reflux reaction for 5h, after cooling, separate the solid and liquid, wash with deionized water until neutral, dry, put the solid into 0.01mol / L gold solution according to the solid-liquid ratio of 1g:15~25mL Soak for 6 h, separate solid and liquid, wash with deionized water until neutral, and dry to obtain gold-modified silicon nitride;

[0037] (2) Calcium-doped carbon-containing quantum dot adhesive: In the reaction kettle, add 1-butyl-3-methylimidazole p-toluenesulfonate: 68g, calcium gluconate: 8g, absorbent cotton: 24g, Stir evenly, seal, place in an oven at 110±2°C, react at a constant temperature for 10 hours, and cool to room temperature to obtain a light yellow viscous liquid that is calcium-doped carbon-containing quantum dot adhesive;

[0038] (3)...

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Abstract

The invention discloses a preparation method of a calcium-doped silicon nitride graphene paste electrode sensor, which is characterized in that, firstly, 1-butyl-3-methylimidazole p-toluenesulfonate is used to dissolve calcium gluconate and absorbent cotton to prepare The light yellow viscous liquid obtained is calcium-doped carbon-containing quantum dot adhesive; in an agate mortar, gold-modified silicon nitride: 34-38%, graphene oxide: 28-32%, calcium-doped carbon-containing Quantum dot adhesive: 10~14%, ammonium polyacrylate: 3~5%, ethanol: 14~20%, grind evenly, put it into a glass tube with an inner diameter of Φ5mm connected with a wire, and then get calcium doped nitriding Silicon graphene paste electrode sensor. The electrode prepared by this application has the advantages of 4-6 times higher conductivity than ordinary carbon paste electrodes, wide electrochemical window, simple preparation method, easy surface renewal, and small residual current. High detection sensitivity and good selectivity.

Description

technical field [0001] The invention relates to a preparation method of an electrochemical sensor, in particular to a preparation method and application of a calcium-doped silicon nitride graphene paste electrode sensor. It belongs to the field of electrochemical analysis. Background technique [0002] The electrochemical analysis sensor is the core and most reliable technology of the current analysis and quantitative detection technology, and it occupies a very prominent position. The advantages of this sensor are as follows: simple operation of the instrument, low cost, high sensitivity, high degree of automation of the instrument, and the use of samples The amount is small, the analysis and detection time is fast, and the detection signal is converted into an intuitive and easy-to-read concentration value at the same time, which is convenient for non-professionals to use. It has been widely used in environmental science, pharmacology, and food science. The chemically mod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/30G01N27/26
CPCG01N27/26G01N27/308
Inventor 李慧芝赵淑英李志英
Owner UNIV OF JINAN
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