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p-type semiconductor metal oxide doped ordered mesoporous tungsten oxide gas sensing material and preparation method thereof

A technology of gas-sensing materials and oxides, applied in the direction of nickel oxide/nickel hydroxide, cobalt oxide/cobalt hydroxide, copper oxide/copper hydroxide, etc., can solve the influence of mesopore disorder, uncontrollable pore structure, Complicated synthesis steps and other problems, to achieve the effect suitable for scale-up production, good sensitivity and selectivity, simple and controllable steps

Active Publication Date: 2022-07-22
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis steps of mesoporous n-type semiconductor metal oxides doped with p-type semiconductor metal oxides reported so far are complicated, and the carrier needs to be prepared in advance; at the same time, the pore structure of the carrier is uncontrollable, and its stability is poor. Difficult to apply to mass production
In addition, the disorder of mesopores in most of the synthesized materials negatively affects mass transport

Method used

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  • p-type semiconductor metal oxide doped ordered mesoporous tungsten oxide gas sensing material and preparation method thereof
  • p-type semiconductor metal oxide doped ordered mesoporous tungsten oxide gas sensing material and preparation method thereof
  • p-type semiconductor metal oxide doped ordered mesoporous tungsten oxide gas sensing material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0025] (1) The amphiphilic block copolymer polyethylene oxide- b - Polystyrene (PEO 114 - b -PS 336 , M n =36948 gmol -1 ) was dissolved in tetrahydrofuran (THF) solution and stirred to obtain a uniform solution A (the mass percentage of the polymer was 2.0 wt%); anhydrous tungsten hexachloride (WCl) was added to ethanol 6 ) and acetylacetone (AcAc), stirred until the solid was completely dissolved to obtain a homogeneous solution B, A and B were mixed and stirred for 2 h, and the solution turned dark green. Add 2.0 mg of copper acetylacetonate (copper source) and stir for 10 min. The mass ratio of block copolymer: tetrahydrofuran: ethanol: anhydrous tungsten hexachloride: acetylacetone: copper source is 0.1:5:1:0.4:0.4:0.02;

[0026] (2) The solution was transferred to a petri dish with a diameter of 15 cm, volatilized at 25 °C for 1 h, and turned into a dark blue film. The petri dish was transferred to a 40 °C oven for 48 h to further evaporate the solvent, and then tr...

Embodiment 2

[0029] (1) The amphiphilic block copolymer polyethylene oxide- b - Polystyrene (PEO 108 - b -PS 112 , Mn=16689 gmol -1 ) in chloroform (CHCl) 3 ) solution, stir to obtain a uniform solution A (the mass percentage of the polymer is 2.0 wt%); add anhydrous tungsten hexachloride (WCl 6 ) and acetylacetone (AcAc), stirred until the solid was completely dissolved to obtain a homogeneous solution B, A and B were mixed and stirred for 2 h, and the solution turned dark green. Add nickel acetylacetonate (nickel source) and stir for 10 min. The mass ratio of block copolymer: chloroform: ethanol: anhydrous tungsten hexachloride: acetylacetone: nickel source is 0.1:5:1:0.4:0.4:0.02;

[0030] (2) The solution was coated on a quartz substrate by spin-coating, volatilized at 25 °C for 2 h to become a dark blue film, transferred to a 70 °C oven for 24 h to further evaporate the solvent, and then transferred Cured at 150 °C for 24 h to obtain a brown composite film;

[0031] (3) The fr...

Embodiment 3

[0033] (1) The amphiphilic block copolymer poly-(4-vinylpyridine)- b - Polystyrene (P4VP 76 - b -PS 96 , Mn≈18000 g mol -1 ) in dichloromethane (CH 2 Cl 2 ) solution, stir to obtain a uniform solution A (the mass percentage of the polymer is 2.0 wt%); add anhydrous tungsten hexachloride (WCl 6 ) and acetylacetone (AcAc), stirred until the solid was completely dissolved to obtain a homogeneous solution B, A and B were mixed and stirred for 2 h, and the solution turned dark green. Add cobalt(II) acetylacetonate (cobalt source) and stir for 10 min. The block copolymer: dichloromethane: ethanol: anhydrous tungsten hexachloride: acetylacetone: cobalt source mass ratio of 0.1:5:1:0.4:0.4:0.02;

[0034] (2) The solution was coated on a quartz substrate by a dip-coating method, volatilized at 25 °C for 1 h, and turned into a dark blue film, which was transferred to a 40 °C oven for 24 h to further evaporate the solvent, and then transferred Cured at 100 °C for 24 h to obtain a...

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Abstract

The invention belongs to the technical field of advanced nanomaterials, in particular to a p-type semiconductor metal oxide doped ordered mesoporous tungsten oxide gas sensing material and a preparation method thereof. The present invention adopts the sol-gel chemical synthesis method, uses the amphiphilic block copolymer as the structure directing agent, and the hydrophilic block interacts with the p-type semiconductor transition metal oxide and tungsten oxide precursor species through hydrogen bonding and coordination. Assembled in a solution, through solvent volatilization-induced co-assembly and high-temperature heat treatment, a p-type semiconductor metal oxide-doped ordered mesoporous tungsten oxide material is obtained. The material has a highly ordered mesoporous structure, high specific surface area and large pore size, its unique mesoporous structure and the role of p-n semiconductor heterojunction, can be used for the preparation of gas sensors, and has a strong effect on hydrogen sulfide gas. Excellent sensitivity and selectivity, ultra-fast response and recovery time. The method of the invention is simple and controllable, is suitable for enlarged production, and has broad application prospects in the field of gas sensing.

Description

technical field [0001] The invention belongs to the technical field of advanced nanomaterials, and in particular relates to a p-type semiconductor metal oxide doped ordered mesoporous tungsten oxide gas-sensing material and a preparation method thereof. Background technique [0002] With the rapid development of Internet of Things technology, various sensor technologies are widely used in practical life, making important contributions to industrial production, environmental monitoring and the improvement of life quality. Among many types of sensors, gas sensors based on semiconductor metal oxide materials (tungsten oxide, tin oxide, zinc oxide, and indium oxide, etc.) have extremely superior performance, including better long-term stability and lower production costs. , and easy to achieve real-time control. These advantages enable it to be widely used in various aspects such as food safety, air quality detection and medical diagnosis. [0003] Since the gas sensing proces...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/02C01G3/02C01G51/04C01G53/04G01N27/12B82Y30/00B82Y40/00
CPCC01G41/02C01G3/02C01G53/04C01G51/04G01N27/127B82Y30/00B82Y40/00C01P2006/16C01P2006/12C01P2004/03C01P2004/04C01P2006/14C01P2006/17
Inventor 邓勇辉肖杏宇周欣然马俊豪
Owner FUDAN UNIV
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