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Method for preparing SnO2 micro-nanofiber

A technology of micro-nano fiber and polyvinylpyrrolidone, which is applied in the field of preparation of SnO2 micro-nano fiber, achieves good gas-sensing performance, controllable reaction parameters, and easy operation

Inactive Publication Date: 2017-06-09
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the two-step synthesis of SnO at home and abroad 2 The work on micro-nanofibers is still in its infancy, and the setting of related process parameters urgently needs further exploration

Method used

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  • Method for preparing SnO2 micro-nanofiber
  • Method for preparing SnO2 micro-nanofiber
  • Method for preparing SnO2 micro-nanofiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1.1 Mix 4.321 g of tin tetrachloride pentahydrate (SnCl 4 ∙5H 2 O) and 2.067 g of hexamethylenetetramine (HMT) were added to a mixed solvent of 18.0 mL of deionized water and 9.0 mL of glycerol, and stirred to obtain a transparent solution, which was transferred to a reaction kettle and placed in a After reacting at 120 °C for 3 h, place it in a constant temperature water bath at 90 °C and stir for 4 h to obtain a precursor solution;

[0037] 1.2 Dissolve 1.998 g of PVP and 1.552 g of stearic acid (SA) in a mixed solvent of 6.0 mL of deionized water and 3.0 mL of DMF, slowly add it to the precursor solution obtained in 1.1, and stir for 6 h to obtain the precursor The body spinning solution was used to obtain precursor fibers by electrospinning. The spinning parameters were as follows: positive voltage 15 KV, negative voltage 0.5 KV, receiving distance 14 cm, and syringe advancing speed 0.001 mm / s.

[0038] 1.3 Place the precursor fiber in a muffle furnace, raise the ...

Embodiment 2

[0041] 2.1 Add 3.315 g of SnCl 4 ∙5H 2 O and 1.392 g of HMT were added to a mixed solvent of 20.0 mL of deionized water and 6.0 mL of glycerol, and stirred to obtain a transparent solution. The solution was transferred to a reaction kettle, and after reacting at 110 °C for 6 h, set Stir in a constant temperature water bath at 80°C for 8 h to obtain a precursor solution;

[0042] 2.2 After dissolving 1.376 g of PVP and 0.784 g of SA in a mixed solvent of 5.0 mL of deionized water and 3.0 mL of DMF, they were slowly added to the precursor solution obtained in 2.1, and stirred for 2 h to obtain a precursor spinning solution. The precursor fibers were obtained by electrospinning. The spinning parameters were as follows: positive voltage 10 KV, negative voltage 0.5 KV, receiving distance 15 cm, and syringe advancing speed 0.002 mm / s.

[0043] 2.3 Place the precursor fiber in a muffle furnace, raise the temperature from room temperature to 300 °C at a rate of 2 °C / min, keep it for...

Embodiment 3

[0045] 3.1 Add 4.887 g of SnCl 4 ∙5H 2 O and 2.832 g of HMT were added to a mixed solvent of 16.0 mL of deionized water and 9.6 mL of glycerol, and stirred to obtain a transparent solution. The solution was transferred to a reaction kettle and reacted at 120 °C for 1 h. Stir in a constant temperature water bath at 90°C for 1 h to obtain a precursor solution;

[0046] 3.2 After dissolving 1.987 g of PVP and 1.954 g of SA in a mixed solvent of 5.0 mL of deionized water and 1.5 mL of DMF, they were slowly added to the precursor solution obtained in 3.1, and stirred for 7 h to obtain a precursor spinning solution. Precursor fibers were obtained by electrospinning. The spinning parameters were as follows: positive voltage 16 KV, negative voltage 0.5 KV, receiving distance 10 cm, and syringe advancing speed 0.001 mm / s.

[0047] 3.3 Place the precursor fiber in a muffle furnace, raise the temperature from room temperature to 300 °C at a rate of 1 °C / min, keep it warm for 4 h, then ...

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Abstract

The invention discloses a method for preparing an SnO2 micro-nanofiber. The method comprises the following steps: adding tin salt and hexamethylenetetramine into a water and glycerin mixed solution, performing stirring to obtain a transparent solution, and after solvothermal reaction treatment, performing stirring and heat preservation at 80-90 DEG C to obtain a precursor solution; and after dissolving PVP and stearic acid in a water and DMF mixed solvent, slowly adding the obtained solution into the precursor solution to obtain a precursor spinning solution, selecting appropriate electrospinning parameters to obtain a precursor fiber, and performing heat treatment to obtain the final product. According to the method, the solvothermal method and the electrospinning method are combined to prepare the size-adjustable SnO2 micro-nanofiber formed by stacking of SnO2 micro-nanoparticles. The preparation process is simple and convenient, the reaction parameters are controllable, and the product appearance is obviously different from a fiber structure obtained by use of the pure electrospinning method. The obtained SnO2 micro-nanofiber has a broad application prospect in the fields of catalysis, gas sensitivity and the like.

Description

technical field [0001] The present invention relates to a kind of SnO 2 A method for preparing micro-nano fibers, specifically related to a spherical or spherical SnO 2 Size-tunable SnO stacked by micro-nanoparticles 2 Preparation method of micro-nanofibers. Background technique [0002] Gas sensors based on metal oxide semiconductor materials have the advantages of simple crystal structure, small particle size, good stability, high sensitivity, fast response time, real-time monitoring, and low cost, and have been widely used in environmental monitoring, food industry, health care, etc. field. Metal oxides with different micromorphologies such as TiO 2 , ZnO, In 2 o 3 , Fe 2 o 3 , CuO, SnO 2 Such micro-nano materials can show excellent gas sensing properties, and have attracted great attention from researchers at home and abroad. [0003] SnO 2 It is a typical n-type semiconductor with a direct band gap of 3.6 eV. It has the advantages of high electrical conductiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/08
CPCD01F9/08
Inventor 马谦李绘陈迎车全德王俊鹏王刚杨萍
Owner UNIV OF JINAN
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