Preparation method of nanometer VN/graphene composite paste electrode sensor

A graphene composite and electrode sensor technology, applied in the field of electrochemical analysis, can solve the problems of low sensitivity, unsatisfactory precision and accuracy, cumbersome operation, etc., and achieve the solution of difficult detection, low cost, and wide electrochemical window Effect

Inactive Publication Date: 2018-11-30
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the operation of the above four determination methods is cumbersome, the sensitivity is not high, and the precision and accuracy are not ideal.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Graphene oxide pretreatment: In the reactor, add deionized water: 72mL, concentrated sulfuric acid: 5.5mL, mix well, cool to room temperature, add graphene oxide: 18g, soak at room temperature for 16h, solid-liquid Separation, washing with deionized water without sulfate radicals, drying, and grinding to powder to obtain pretreated graphene oxide;

[0026] (2) Preparation of nano-VN / graphene composite paste electrode: In an agate mortar, add nano-VN: 43g, pretreated graphene oxide: 22g, N-ethyl-3-methylpyridine hexafluorophosphate : 15g, liquid paraffin: 11mL, petroleum ether: 15mL, grind evenly to get nano-VN / graphene / N-ethyl-3-methylpyridine hexafluorophosphate mixture carbon paste; then put the carbon paste into the In a glass tube with an inner diameter of Φ5mm, compact it, dry it, grind it with metallographic sandpaper, polish it, and wash it with deionized water to obtain a nano-VN / graphene composite paste electrode.

Embodiment 2

[0028] (1) Graphene oxide pretreatment: In the reactor, add deionized water: 75mL, concentrated sulfuric acid: 4.5mL, mix well, cool to room temperature, add graphene oxide: 17g, soak at room temperature for 17h, solid-liquid Separation, washing with deionized water without sulfate radicals, drying, and grinding to powder to obtain pretreated graphene oxide;

[0029] (2) Preparation of nano-VN / graphene composite paste electrode: In an agate mortar, add nano-VN: 45g, pretreated graphene oxide: 20g, N-ethyl-3-methylpyridine hexafluorophosphate : 18g, liquid paraffin: 9mL, petroleum ether: 14mL, grind evenly to get nano-VN / graphene / N-ethyl-3-methylpyridine hexafluorophosphate mixture carbon paste; then put the carbon paste into the connection In a glass tube with an inner diameter of Φ5mm, compact it, dry it, grind it with metallographic sandpaper, polish it, and wash it with deionized water to obtain a nano-VN / graphene composite paste electrode.

Embodiment 3

[0031] (1) Graphene oxide pretreatment: In the reactor, add deionized water: 70mL, concentrated sulfuric acid: 6mL, mix well, cool to room temperature, add graphene oxide: 19g, soak at room temperature for 15h, and separate solid and liquid , wash with deionized water without sulfate radicals, dry, grind to powder, and obtain pretreated graphene oxide;

[0032] (2) Preparation of nano-VN / graphene composite paste electrode: In an agate mortar, add nano-VN: 42g, pretreated graphene oxide: 25g, N-ethyl-3-methylpyridine hexafluorophosphate : 13g, liquid paraffin: 13mL, petroleum ether: 12mL, grind evenly to get nano-VN / graphene / N-ethyl-3-methylpyridine hexafluorophosphate mixture carbon paste; then put the carbon paste into the In a glass tube with an inner diameter of Φ5mm, compact it, dry it, grind it with metallographic sandpaper, polish it, and wash it with deionized water to obtain a nano-VN / graphene composite paste electrode.

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Abstract

The invention discloses a preparation method of a nanometer VN / graphene composite paste electrode sensor. The preparation method comprises following steps: firstly, sulfuric acid is adopted for pre-treatment of oxidized graphene so as to obtain pre-treated oxidized graphene; by mass, 42 to 45% of nanometer VN, 20 to 25% of the pre-treated oxidized graphene, 12 to 18% of N-ethyl-3-methylpyridine hexafluorophosphate, 8 to 12% of liquid paraffin, and 6 to 10% of petroleum ether are introduced into a agate mortar for uniform grinding, an obtained carbon paste is introduced into a glass tube connected with a wire, compressing, drying, polishing with abrasive paper for metallograph, polishing, and deionized water washing are carried out so as to obtain a nanometer VN / graphene composite paste electrode, wherein the internal diameter of the glass tube is 5mm. The electric conductivity of the nanometer VN / graphene composite paste electrode is increased by 2 to 4 times of that of common paste electrode; the electrochemical window is wide; the preparation method is simple; cost is low; surface replacing is convenient; residual current is low; the sensitivity and the selectivity in detection of luteolin are high.

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 nano VN / graphene composite paste electrode sensor. It belongs to the field of electrochemical analysis. Background technique [0002] Vanadium nitride (VN) is a multifunctional metal nitride with a face-centered cubic crystal structure, which has high electrical conductivity (conductivity is about 10 6 / (Ω•m) and high electrochemical activity hexagonal crystal structure, high hardness, microhardness is about 1520HV, VN density is 6.13. Relative molecular mass is 64.95. The melting point is 2360 degrees. They all have high wear resistance. It is a class of noble metal catalysts with high catalytic activity and high-capacity electrochemical energy storage electrode materials. Graphene is a two-dimensional crystal with only one atomic thickness assembled by carbon six-membered rings. As a new class of electrode materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30B82Y30/00
CPCG01N27/308B82Y30/00
Inventor 李慧芝翟玉博李志英
Owner UNIV OF JINAN
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