A kind of preparation method of ultrasensitive nitrogen dioxide sensing material

A technology of nitrogen dioxide and sensing materials, applied in tin oxide, nanotechnology, etc., can solve the problems of poor selectivity, low response, high working temperature, etc., and achieve the effects of easy deviceization, increased output, and good permeability

Active Publication Date: 2016-08-24
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing an ultra-sensitive nitrogen dioxide sensing material for the current gas-sensitive materials with low response, high working temperature and poor selectivity. Preparation of tin seeds and hydrothermal growth of tin dioxide nanoflowers

Method used

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  • A kind of preparation method of ultrasensitive nitrogen dioxide sensing material
  • A kind of preparation method of ultrasensitive nitrogen dioxide sensing material
  • A kind of preparation method of ultrasensitive nitrogen dioxide sensing material

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Experimental program
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Effect test

Embodiment 1

[0033] a. Use a pipette gun to inject 20 μl of tin tetrachloride into 30ml of deionized water frozen ice. After the ice is completely melted, move the solution to a water bath at a temperature of 50°C and stir for 40 hours to make it completely hydrolyzed, and the white precipitate After being collected by centrifugation, it was calcined in an air atmosphere in a tube furnace at a temperature of 500°C for 2 hours to generate tin dioxide nanoparticle crystal seeds;

[0034] b. Grind the seed crystal obtained in step a for 5 minutes with a mortar, then disperse into 30ml deionized ice water and stir, control the temperature of deionized water to 0°C, then add 0.8475g sodium hydroxide and 240μl tin tetrachloride in sequence (the molar ratio is 10.5: 1, wherein the mol ratio of tin tetrachloride in step a and tin tetrachloride in step b is 1: 12), stirred for 30min to form a mixed solution;

[0035] c. Transfer the mixed solution obtained in step b into a Teflon hydrothermal kettl...

Embodiment 2

[0038]a. Inject 20 μl of tin tetrachloride into the ice of deionized water with a pipette gun. After the ice is completely melted, move the solution to a water bath with a temperature of 50°C, stir for 40 hours, and completely hydrolyze. The white precipitate is collected by centrifugation. Finally, calcining in an air atmosphere in a tube furnace at a temperature of 500°C for 2 hours to generate tin dioxide nanoparticle crystal seeds;

[0039] B, grind the seed crystal obtained in step a for 5 minutes with a mortar, then disperse into deionized water and stir, control the temperature of deionized water to be 70°C, then add 0.8475g sodium hydroxide and 240 μl tin tetrachloride (mol Ratio is 10.5: 1, wherein tin tetrachloride in step a and tin tetrachloride mol ratio in step b are 1: 12), stirred 30min to form mixed solution;

[0040] c. Transfer the mixed solution obtained in step b into a Teflon hydrothermal kettle, and place it in an oven at a temperature of 200° C. for 20 h...

Embodiment 3

[0043] a. Use a pipette gun to inject 20 μl of tin tetrachloride into 30ml of deionized water frozen ice. After the ice is completely melted, move the solution to a water bath at a temperature of 30°C and stir for 40 hours to make it completely hydrolyzed, and the white precipitate After being collected by centrifugation, it was calcined in an air atmosphere in a tube furnace at a temperature of 350°C for 2 hours to generate tin dioxide nanoparticle seeds;

[0044] b. Grind the seed crystal obtained in step a for 5 minutes with a mortar, then disperse into 30ml of deionized ice water and stir, control the temperature of deionized water to 0°C, then add 0.5470g of sodium hydroxide and 200μl of tin tetrachloride in sequence (the molar ratio is 8: 1, wherein the mol ratio of tin tetrachloride in step a and tin tetrachloride in step b is 1: 10), stirred for 30min to form a mixed solution;

[0045] c. Transfer the mixed solution obtained in step b into a Teflon hydrothermal kettle,...

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Abstract

The invention relates to a preparation method of a supersensitive nitrogen dioxide sensing material. The method adopts a two-step process, including preparation of a tin dioxide crystal seed and hydrothermal growth of a tin dioxide nanometer flower. The preparation method comprises the following steps: step 1, by taking stannic chloride of which the hydrolysis rate is extremely sensitive to temperature as a raw material, dispersing the stannic chloride in water and calcining to obtain the tin dioxide crystal seed; step 2, grinding the obtained crystal seed; dispersing in ice water; adding sodium hydroxide and the stannic chloride; stirring under an ice bath condition to form a mixed solution; performing hydrothermal synthesis of the tin dioxide nanometer flower; centrifugally washing, collecting and drying to obtain the supersensitive nitrogen dioxide gas-sensitive material. A new generation of supersensitive ppb-grade nitrogen dioxide gas-sensitive material can be obtained by controlling the external temperature of the supersensitive nitrogen dioxide gas-sensitive material during hydrolysis. The supersensitive nitrogen dioxide sensing material obtained by the method disclosed by the invention has the characteristics of being highly sensitive, stable for a long time, good in selectivity, capable of work at room temperature and the like, so the practicability of the material is greatly improved.

Description

technical field [0001] The invention relates to the field of functional material science, in particular to a preparation method of an ultrasensitive nitrogen dioxide sensing material. Background technique [0002] The well-known tin dioxide (SnO 2 ) Main features of gas-sensitive materials: Tin dioxide has a series of excellent gas-sensing properties and physical and chemical properties. By reducing the size of tin dioxide and changing the morphology of tin dioxide, various gas-sensitive sensors can be obtained, which are suitable for low-concentration Gas detection has the advantages of adjustable, good electrical conductivity, and stable chemical properties. The superiority of tin dioxide as a sensitive material has been widely recognized, making it the most studied metal oxide gas sensitive material. The gas-sensing performance is remarkable in the concentration range of ppm (one part per million). [0003] The currently known simple tin dioxide gas-sensing material ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/02B82Y40/00
Inventor 窦新存李予祥
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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