Highly dispersed noble metal-loaded ordered mesoporous tungsten oxide gas-sensitive material and preparation method thereof

A precious metal and tungsten oxide technology, which is applied to the analysis of materials, tungsten oxide/tungsten hydroxide, and gas mixture analysis. It can solve the problems of poor stability and dispersion of precious metal particles, complicated synthesis steps, and uncontrollable pore structure. Fast response and recovery time, suitable for scale-up production, simple method effect

Inactive Publication Date: 2018-06-29
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, the synthesis steps of mesoporous metal oxides loaded with precious metals are complicated, and the carrier or noble metal particles need to be prepared in advance; at the same time, the pore structure of the carrier is uncontrollable, and the stability and dispersion of the noble metal particles are poor. Difficult to mass produce
In addition, most of the synthesized materials have disordered mesopores, which have certain deficiencies in material transport.

Method used

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  • Highly dispersed noble metal-loaded ordered mesoporous tungsten oxide gas-sensitive material and preparation method thereof
  • Highly dispersed noble metal-loaded ordered mesoporous tungsten oxide gas-sensitive material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Amphiphilic block copolymer polyethylene oxide- b - Polystyrene (PEO 108 - b -PS 210 , Mn= 26544 g mol -1 ) was dissolved in tetrahydrofuran (THF) solution, and stirred to obtain a homogeneous solution A (the polymer mass percentage was 2.0 wt%); anhydrous tungsten hexachloride (WCl 6 ) and acetylacetone (AcAc), stirred until the solid was completely dissolved to obtain a uniform solution B, mixed A and B and stirred for 2 h, and the solution turned dark green. Add 2.0 mg (1,5-cyclooctadiene) dimethyl platinum (II) (platinum source), and stir for 10 min. Wherein the mass ratio of block copolymer: tetrahydrofuran: ethanol: anhydrous tungsten hexachloride: acetylacetone: platinum source is 0.1:5:1:0.4:0.4:0.002;

[0024] (2) Transfer the solution to a petri dish with a diameter of 15 cm, volatilize at 25 °C for 1 h, and turn into a dark blue film, transfer the petri dish to a 40 °C oven for 48 h to further volatilize the solvent, and then transfer to 100 °C Afte...

Embodiment 2

[0027] (1) Amphiphilic block copolymer polyethylene oxide- b - Polystyrene (PEO 108 - b -PS 112 , Mn= 16689 g mol -1 ) dissolved in chloroform (CHCl 3 ) solution, stirred to obtain a homogeneous solution A (the polymer mass percentage is 2.0 wt%); anhydrous tungsten hexachloride (WCl 6 ) and acetylacetone (AcAc), stirred until the solid was completely dissolved to obtain a uniform solution B, mixed A and B and stirred for 2 h, and the solution turned dark green. Add (1,5-cyclooctadiene) dimethyl platinum (II) (platinum source) and triphenyl (phenylethynyl) lead (IV), and stir for 10 min. Wherein block copolymer: tetrahydrofuran: ethanol: anhydrous tungsten hexachloride: acetylacetone: platinum source: lead source mass ratio is 0.1:5:1:0.4:0.4:0.002:0.003;

[0028] (2) The solution was coated on a quartz substrate by spin-coating method, volatilized at 23 °C for 2 h, and turned into a dark blue film, which was transferred to an oven at 70 °C for 24 h to further volatilize...

Embodiment 3

[0031] (1) Amphiphilic block copolymer polyethylene oxide- b - Polystyrene (PEO 108 - b -PS 297 , Mn= 35975 g mol -1 ) dissolved in dichloromethane (CH 2 Cl 2 ) solution, stirred to obtain a homogeneous solution A (the polymer mass percentage is 2.0 wt%); anhydrous tungsten hexachloride (WCl 6 ) and acetylacetone (AcAc), stirred until the solid was completely dissolved to obtain a uniform solution B, mixed A and B and stirred for 2 h, and the solution turned dark green. Add (1,5-cyclooctadiene) dimethyl platinum (II) (platinum source), and stir for 10 min. Wherein block copolymer: tetrahydrofuran: ethanol: anhydrous tungsten hexachloride: acetylacetone: platinum source mass ratio is 0.1:5:1:0.4:0.4:0.02;

[0032] (2) Apply the solution on a quartz substrate by dip-coating method, volatilize at 25 °C for 1 h, and turn into a dark blue film, transfer it to a 40 °C oven for 24 h to further volatilize the solvent, and then transfer Cured at 100 °C for 24 h to obtain a brow...

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Abstract

The invention belongs to the technical field of advanced nanocomposite materials, and in particular to a highly dispersed noble metal-loaded ordered mesoporous tungsten oxide gas-sensitive material and a preparation method thereof. By a sol-gel chemical synthesis method, the invention utilizes an amphiphilic block copolymer as a structure-directing agent, hydrophilic blocks are assembled with a metallic oxide precursor in solution by hydrogen bonds and coordination, hydrophobic blocks wrap an oil-soluble noble metal precursor by a hydrophobic effect, and after solvent evaporation-induced co-assembly and high-temperature heat treatment, the noble metal-loaded ordered mesoporous tungsten oxide material is directly obtained. The composite material has a highly ordered mesoporous structure, large specific surface area and highly dispersed, stable noble metal particles with uniform size, and can be used in the preparation of gas sensors, the composite material has excellent sensitivity andselectivity on carbon monoxide, and response and recovery times are extremely short. The method disclosed by the invention is simple, the complexity of multi-step synthesis is overcome, the method issimple, controllable and suitable for enlarged production, and the invention has a broad application prospect in the field of gas sensing.

Description

technical field [0001] The invention belongs to the technical field of advanced nanocomposite materials, and in particular relates to a highly dispersed noble metal-loaded ordered mesoporous tungsten oxide gas-sensing material and a preparation method thereof. technical background [0002] In recent years, with the rapid development of the Internet of Things, sensors, as an important device for real-time information collection, have attracted widespread attention and research. A gas sensor is a converter that converts a certain gas volume fraction into a corresponding electrical signal, which can reflect the type, concentration and other information of the gas in time, so it is widely used in industrial production, medical and health, food safety, home life and other fields. And important applications. [0003] Resistive sensors based on semiconductor metal oxides are cheap, simple in structure, sensitive and fast in response, and easy to mass-produce, so they have become t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/02B22F9/30G01N33/00B82Y30/00
CPCC01G41/02B22F9/30B82Y30/00C01P2004/80C01P2006/12C01P2006/16G01N33/004
Inventor 邓勇辉马俊豪
Owner FUDAN UNIV
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