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Preparation method of titanium nitride/carbon nano tube composite paste electrode sensor

A carbon nanotube composite, electrode sensor technology, applied in the field of electrochemical analysis, can solve the problems of poor electrical conductivity, poor stability, low sensitivity, etc., and achieve the effects of low cost, easy surface, and improved sensitivity

Inactive Publication Date: 2019-11-12
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

[0025] (1) Carbon nanotube pretreatment: In the reactor, add 6mol / L sulfuric acid: 84 mL, potassium periodate: 6g, stir to dissolve, add carbon nanotube: 10g, soak at room temperature for 11h, then boil for 30min , Cool to room temperature, separate solid and liquid, wash with deionized water to neutrality, dry, and grind to powder to obtain pretreated carbon nanotubes;

[0026] (2) Preparation of composite adhesive: In the reactor, add 1-butyl-1-methylpyrrole trifluoromethanesulfonate: 75g, cellulose: 25g, close the sealing cap, and place in a thermostat. In the medium, the temperature is kept at 120±2℃, and the reaction is 22h to obtain a viscous light yellow transparent liquid, which is a composite adhesive;

[0027] (3) Preparation of titanium nitride / carbon nanotube composite paste electrode sensor: In an agate mortar, add nanometer titanium nitride: 38g, pretreated carbon nanotube: 30g, composite adhesive: 14g, liquid paraffin. :18g, grind evenly into a carbon paste, then pu...

Embodiment 2

[0029] (1) Pretreatment of carbon nanotubes: In the reactor, add 6mol / L sulfuric acid: 86mL, potassium periodate: 5g, stir to dissolve, add carbon nanotubes: 8g, soak at room temperature for 10h, then boil for 30min, Cool to room temperature, separate solid and liquid, wash with deionized water until neutral, dry, and grind to powder to obtain pretreated carbon nanotubes;

[0030] (2) Preparation of composite adhesive: In the reaction kettle, add 1-butyl-1-methylpyrrole trifluoromethanesulfonate: 72g, cellulose: 28g, close the sealing lid, and place in a thermostat. In the medium, the temperature is kept at 120±2℃, the reaction is 21h, and the viscous light yellow transparent liquid is obtained, which is a composite adhesive;

[0031] (3) Preparation of titanium nitride / carbon nanotube composite paste electrode sensor: In an agate mortar, add nanometer titanium nitride: 42g, pretreated carbon nanotube: 28g, composite adhesive: 15g, liquid paraffin. : 15g, grind evenly into a carbo...

Embodiment 3

[0033] (1) Carbon nanotube pretreatment: In the reactor, add 6mol / L sulfuric acid: 83mL, potassium periodate: 4g, stir to dissolve, add carbon nanotube: 12g, soak at room temperature for 12h, then boil for 30min, Cool to room temperature, separate solid and liquid, wash with deionized water until neutral, dry, and grind to powder to obtain pretreated carbon nanotubes;

[0034] (2) Preparation of composite adhesive: In the reactor, add 1-butyl-1-methylpyrrole trifluoromethanesulfonate: 76g, cellulose: 24g, close the sealing cap, and place in a thermostat. In the medium, the temperature is kept at 120±2℃, and the reaction is 20h to obtain a viscous light yellow transparent liquid, which is a composite adhesive;

[0035] (3) Preparation of titanium nitride / carbon nanotube composite paste electrode sensor: In an agate mortar, add nanometer titanium nitride: 36g, pretreated carbon nanotube: 32g, composite adhesive: 16g, liquid paraffin. : 16g, grind evenly into a carbon paste, then put...

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Abstract

The invention discloses a preparation method of a titanium nitride / carbon nano tube composite paste electrode sensor. The preparation method is characterized by comprising the steps of: processing a carbon nano tube by using sulphuric acid and periodate potassium, so that a pre-processed carbon nano tube is obtained; preparing a composite adhesive by adopting 1-butyl-1-methyl pyrrole trifluoromethylsulfonate and cellulose; and then, adding the following components into an agate mortar in percentage by weight: 36-42% of nano titanium nitride, 28-32% of the pre-processed carbon nano tube, 12-16%of the composite adhesive, and 15-18% of liquid paraffin, uniformly grinding to form a carbon paste, putting the carbon paste into a glass tube, wherein the glass tube is connected to a conducting wire; the inside diameter of the glass tube is phi5 mm; and thus, the titanium nitride / carbon nano tube composite paste electrode sensor is prepared. Compared with the ordinary carbon paste electrode, the electrical conductivity of the carbon paste electrode prepared in the invention is increased by 6-8 times; the carbon paste electrode prepared in the invention has the advantages of being wide in electrochemical window, simple in preparation method, low in cost, easy to update the surface, low in residual current, high in paracetamol detection sensivity, good in selectivity and the like.

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 titanium nitride / carbon nanotube composite paste electrode sensor. It belongs to the field of electrochemical analysis. Background technique [0002] Titanium nitride (TiN) has a typical NaCl-type structure, which is a face-centered cubic lattice, with a lattice constant a=0.4241nm, in which titanium atoms are located at the corners of the face-centered cubic. TiN is a non-stoichiometric compound, and its stable composition range is TiN0.37-TiN1.16, and the nitrogen content can be changed within a certain range without causing changes in the TiN structure. TiN powder is generally yellowish brown, and ultrafine TiN powder is black. TiN has a melting point of 2950°C, a density of 5.43-5.44g / cm3, a Mohs hardness of 8-9, and good thermal shock resistance. The melting point of TiN is higher than that of most transition metal n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30G01N27/26
CPCG01N27/26G01N27/308
Inventor 李慧芝翟玉博朱学英
Owner UNIV OF JINAN
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