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A kind of nano material and its preparation method and application

A nano-reaction technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of solute time difference, long time-consuming, high energy consumption, etc., and achieve short time and reliable process control, low energy consumption

Inactive Publication Date: 2017-05-31
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the conventional hydrothermal or solvothermal method usually takes more than ten hours or even dozens of hours for holding time, which takes a long time, consumes a lot of energy, and has the disadvantages of time difference in heating the solute.

Method used

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  • A kind of nano material and its preparation method and application
  • A kind of nano material and its preparation method and application
  • A kind of nano material and its preparation method and application

Examples

Experimental program
Comparison scheme
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preparation example Construction

[0029] a. Gear-shaped nano-WO 3 Precursor preparation:

[0030] Use a small container to measure a certain amount of ethylene glycol, and accurately weigh a certain amount of WCl 6 Dissolved in ethylene glycol, fully stirred on a magnetic stirrer, the solution is dark green, then put it into a reaction tank, add ammonia water and deionized water to the outer wall of a small container, put it into a microwave reactor for reaction, and obtain a dark brown viscous A thick precipitate was obtained after drying at 105°C to obtain a black powder precursor sample, and the SEM image showed a gear-like substance.

[0031] b. Dimple-shaped nano-WO with intermediate pores 3 Preparation of:

[0032] After calcining the black precursor sample at 450-550 ° C in the air for 2 hours, the sample is a light yellow powder, and the obtained nano-WO is dimpled with a hole in the middle. 3 .

[0033] Application of the present invention in the preparation of xylene gas sensor; its manufacturin...

Embodiment 1

[0035] Take 40ml of ethylene glycol (EG) in a 50ml beaker and accurately weigh 1.7850g of WCl 6 Dissolve in ethylene glycol, stir for 1h, the solution is dark green, then put it into the reaction tank, add 1.8ml of ammonia water and 15ml of deionized water outside the beaker and into the reaction tank, put it into the microwave reactor and heat up to within 20min After reacting at 170°C for 80 minutes, cool naturally. The solution in the beaker is tan, with obvious uniform flocculent precipitation, centrifuged and washed and dried, the sample is black powder, and the XRD pattern of the obtained powder is as follows: figure 1 As shown in the spectrum of the precursor, it is consistent with the phase of PDF card No. 85-2459 after jade6.5 phase retrieval, which is hexagonal crystal phase WO 3 , good crystallinity, calculated by Scherrer formula WO 3 The grain size is 19.37nm. The resulting scanning electron microscope images are figure 2 As shown, it is in the shape of a gea...

Embodiment 2

[0037] After the precursor composite material was calcined at 550°C in the air for 2 hours, the sample completely turned into a light yellow powder, and the XRD pattern was as follows: figure 1 As shown in the spectrum of the product after calcination, the jade6.5 phase search is consistent with the PDF card number 83-0950, which is WO 3 Monoclinic crystal phase, good crystallinity, WO calculated by Scherrer formula 3 The grain size is 28.82nm. The resulting scanning electron microscope images are image 3 As shown, it is a dimple-shaped substance with a hole in the middle; the powder is evenly mixed with water, coated into a side-heated gas sensor, dried, calcined at 550°C for 2 hours, naturally cooled and taken out, and tested for gas-sensing performance after aging for 5 days. The relationship curve between its response sensitivity to 100ppm xylene and working temperature is as follows Figure 4b As shown, the best working temperature is 80°C, at 80°C, its sensitivity to...

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Abstract

The invention relates to a nanometer material and its preparation method and application. The material, that is, the nano-WO3 precursor and the sintered body exhibit excellent gas-sensing properties to xylene gas. In the present invention, tungsten hexachloride is used as a tungsten source and dissolved in ethylene glycol solvent, ammonia water is used as a precipitant, and microwave heating is adopted at 170-190°C for 50-80 minutes at the gas-liquid interface under stirring conditions to obtain a gear-shaped The nano-WO3 precursor, after the precursor is calcined at 450-550°C for 2 hours in the air, the sintered product of nano-WO3 with intermediate pores is obtained, and both the precursor and the sintered product exhibit excellent gas Sensitivity, the method has the advantages of fast response, energy saving and cost reduction, and the prepared xylene gas sensor has the advantages of low operating temperature, high sensitivity, good selectivity, and short response / recovery time.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular to a nanomaterial and its preparation method and application. Background technique [0002] Nano tungsten trioxide (WO 3 ) as a wide-bandgap semiconductor has attracted extensive attention due to its unique physical and chemical properties (such as for gas sensors, photocatalysis, electrochromic devices, and optoelectronic devices, etc.). Nano WO 3 The structure itself is complex and the phases are diverse. For nano-WO 3 The morphology design and controlled synthesis of the compound have aroused people's widespread interest. WO 3 Nanosheet, WO 3 Nanowires and WO 3 Nanotubes have been reported. The national invention patent (CN201410110388) reported the amino-functionalized NH 2 -SBA-15 as a template, phosphotungstic acid as a tungsten source, stirred in an alcohol solution and sintered to obtain hexagonal flaky tungsten trioxide with regular morphology, the prepared tu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/02B82Y40/00B82Y30/00
CPCC01G41/02C01P2002/72C01P2004/03
Inventor 桂阳海赵建波郭智荣
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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