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Method for synthesizing large-aperture mesoporous bimetallic oxide semiconductor gas-sensitive material

A technology of double metal oxide and synthesis method, applied in zirconia, tungsten oxide/tungsten hydroxide, nanotechnology, etc., can solve the problems of poor stability, difficult industrial production, difficult control of synthesis process, etc., and achieve good sensitivity and Effects of selectivity, fast response and recovery time

Active Publication Date: 2019-11-15
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, so far, there are few reports on the synthesis of mesoporous double metal oxide semiconductor materials. This is because the hydrolysis and condensation rates of different metal precursors are different, and the synthesis process of mesoporous double metal oxides is difficult to control. In the post-treatment process of removing the template and crystallizing the pore walls of mesoporous metal oxides, the metal oxides will cause the collapse of the pore structure due to severe structural reformation, and the poor stability makes it difficult to carry out large-scale industrial production

Method used

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  • Method for synthesizing large-aperture mesoporous bimetallic oxide semiconductor gas-sensitive material
  • Method for synthesizing large-aperture mesoporous bimetallic oxide semiconductor gas-sensitive material

Examples

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Effect test

Embodiment 1

[0024] (1) Add 0.10 g amphiphilic block copolymer polyethylene oxide- b- Polystyrene (PEO 112 - b -PS 236 ,M n =27948 gmol -1 ) was dissolved in 5 g tetrahydrofuran, and stirred at room temperature for 0.5 h to obtain solution A; 0.10 g tungsten chloride and 0.20 g n-propoxide zirconium were dissolved in 2.0 g ethanol, and stirred at room temperature for 0.5 h to obtain solution B; solution A was mixed with B is mixed evenly, and after stirring for 2 hours at room temperature, a homogeneous mixed solution is finally obtained;

[0025] (2) The homogeneous solution was transferred to a watch glass and volatilized at room temperature for 24 h; then the watch glass was transferred to a 40°C oven to further evaporate the solvent for 24 h, and then transferred to a 100°C oven for curing for 24 h. Finally, the composite film is scraped off from the watch glass and ground to obtain a solid powder;

[0026] (3) The obtained solid powder was placed in a tube furnace, and calcined ...

Embodiment 2

[0028] (1) Add 0.10 g amphiphilic block copolymer polyethylene oxide- b -Polymethylmethacrylate (PEO 123 - b -PMMA 184 ,M n =35729 gmol -1 ) was dissolved in 5 g tetrahydrofuran, and stirred at room temperature for 0.5 h to obtain solution A; 0.15 g cobalt chloride and 0.3 g n-propoxide zirconium were dissolved in 2.0 g ethanol, and stirred at room temperature for 0.5 h to obtain solution B; solution A was mixed with B is mixed evenly, and after stirring for 2 hours at room temperature, a homogeneous mixed solution is finally obtained;

[0029] (2) The homogeneous solution was coated on a quartz plate by spin coating, and volatilized at room temperature for 24 h; then transferred to a 40°C oven to further volatilize the solvent for 24 h, and then transferred to a 100°C oven for curing 24 h. Finally, the composite film is scraped off from the quartz plate and ground to obtain a solid powder;

[0030] (3) The obtained solid powder was placed in a tube furnace, and calcine...

Embodiment 3

[0032] (1) Add 0.10 g amphiphilic block copolymer poly-(4-vinylpyridine)- b - Polystyrene (P4VP 84 - b -PS 113 , Mn=19356 g mol -1 ) was dissolved in 5 g of dichloromethane solution, stirred at room temperature for 0.5 h to obtain solution A; 0.125 g of tin tetrachloride and 0.25 g of titanium isopropoxide were dissolved in 2.0 g of ethanol, and stirred at room temperature for 0.5 h to obtain solution B; Mix solutions A and B evenly, and stir at room temperature for 2 hours to finally obtain a homogeneous mixed solution;

[0033] (2) Apply the homogeneous solution on the quartz plate by pulling method, and volatilize at room temperature for 24 h; then transfer it to a 40°C oven to further volatilize the solvent for 24 h, and then transfer to a 100°C oven for curing 24 h. Finally, the composite film is scraped off from the quartz plate and ground to obtain a solid powder;

[0034] (3) The obtained solid powder sample was placed in a tube furnace, and calcined in a nitroge...

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Abstract

The invention belongs to the technical field of advanced nano materials and in particular discloses a method for synthesizing a large-aperture mesoporous bimetallic oxide semiconductor gas-sensitive material on the basis of acid-base pairs. The method comprises the following steps: by taking an amphiphilic block copolymer as a template agent, and a metal alkoxide and a metal chloride as two metaloxide precursors, enabling the precursors to react with a hydrophilic segment of the template agent through hydrogen bonds under a coordination function in a synthesis system of a polar organic solvent, and performing solvent volatilization induction co-assembling and calcining at different steps with an inert atmosphere firstly and an air atmosphere later, so as to obtain a large-aperture mesoporous bimetallic oxide semiconductor material. By adopting the method, materials such as a p-n junction semiconductor, a p-p junction semiconductor and an n-n junction semiconductor can be synthesized,and in addition, the synthetic materials have highly ordered mesoporous structures, large apertures and large specific surface areas. The method can be applied to gas sensation, and has very good sensitivity and selectivity and very short response and recover time upon small molecule gases such as CO, H2 and CH4 or one or more of VOCs (volatile organic compounds) such as ethanol, acetone and methylbenzene.

Description

technical field [0001] The invention belongs to the technical field of advanced nanometer materials, and specifically relates to a method for synthesizing a large-aperture mesoporous double-metal oxide semiconductor gas-sensing material based on the concept of an acid-base pair. Background technique [0002] Metal oxide semiconductor nanomaterials have a wide range of applications in the fields of catalysis, sensing and energy storage due to their unique micro-nano structure and special optical and electronic properties. In terms of gas sensing, the rapid diffusion of guest molecules and the large exposure of active sites will greatly improve the performance of gas sensing devices based on metal oxide semiconductor materials. Therefore, compared with non-porous bulk metal oxide semiconductors, ordered mesoporous metal oxide semiconductors rely on their highly crystalline pore walls, higher specific surface area, larger pore volume, rich, orderly and connected The characteri...

Claims

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Application Information

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IPC IPC(8): C01G25/02C01G41/02B82Y40/00
CPCC01G25/02C01G41/02B82Y40/00C01P2004/03C01P2006/12C01P2006/16C01P2006/14
Inventor 邓勇辉高美琪马俊豪
Owner FUDAN UNIV
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