Method for manufacturing flawless millipore/mesoporous film by adopting mould plate technique and film thereof

A manufacturing method and crack-free technology, which is applied in the field of crack-free micro/mesoporous film and crack-free micro/mesoporous film, can solve the problems of long roasting stage, inapplicability, and unsolved particle aggregation, etc. Achieve the effect of low temperature and avoid cracks

Inactive Publication Date: 2008-05-07
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0026] In addition, a complex firing temperature program can produce crack-free films, but these processes usually require long firing stages and special sample pretreatment
Moreover, the high-temperature calcination process cannot be applied to the removal of templating agents for temperature-sensit

Method used

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  • Method for manufacturing flawless millipore/mesoporous film by adopting mould plate technique and film thereof
  • Method for manufacturing flawless millipore/mesoporous film by adopting mould plate technique and film thereof
  • Method for manufacturing flawless millipore/mesoporous film by adopting mould plate technique and film thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0056] Example one

[0057] 9 (mole, the same below) parts of TPAOH: 25 parts of SiO 2 : 480 parts H 2 O: 100 parts of EtOH (TPAOH: tetrapropyl ammonium hydroxide, EtOH: ethanol, SiO 2 :Ethyl orthosilicate) mixed solution is hydrolyzed for 12-48 hours under stirring; then placed in a 60°C water bath to crystallize for 10-15 days, fully washed with deionized water 4 times, freeze-dried to obtain a white powder. The XRD diffraction spectrum showed that the white powder was pure silicon Silicalite-1 nanocrystals with MFI structure, and the average particle size was 60 nm.

[0058] Adsorb 60nm Silicalite-1 seed crystal with MFI structure on the cleaned α alumina surface, and then put 5 parts TPAOH: 25 parts SiO 2 : 480 parts H 2 O: 100 parts of EtOH (TPAOH: tetrapropyl ammonium hydroxide, EtOH: ethanol, SiO 2 : Ethyl orthosilicate) in a mixed solution, crystallize at 100°C, take it out after 3 days, wash the surface of the film with deionized water, and dry it naturally in the air. Th...

Example Embodiment

[0061] Example two

[0062] Put the washed ceramic pieces into 0.14-0.3 parts CTAB: 7.4-15 parts NH 4 OH: 1.0 part of SiO 2 : 70-100 parts H 2 O(CTAB: Cetyl trimethyl amine bromide, SiO 2 : Ethyl orthosilicate) in a synthetic solution, crystallize at 20-40°C for 10-200 minutes to obtain a transparent film on the silicon chip. The XRD diffraction pattern shows that it is MCM-41 with a two-dimensional hexagonal structure (in 1992, researchers from Mobil Company used alkyl quaternary ammonium salt type cationic surfactant as a template for the first time, and synthesized it with a single pore size under alkaline conditions. The mesoporous silicate materials, collectively referred to as M41S, include hexagonal crystal system MCM-41, cubic crystal system MCM-48 and layered structure MCM-50) mesoporous film.

[0063] Take two 2×2cm MCM-41 mesoporous membranes, and put one into a horse boiling furnace for calcining. After raising the temperature from room temperature to 550°C at a heatin...

Example Embodiment

[0065] Example three

[0066] 8.0 copies (TMA) 2 O: 0.22 parts Na 2 O: Al 2 O3 : 5.0 parts SiO 2 : 400 parts H 2 O(TMAOH: Tetramethylammonium hydroxide, SiO 2 : Ethyl orthosilicate) mixed solution is hydrolyzed for 12-48 hours under stirring; then placed in a water bath at 60°C for crystallization for 3-5 days to obtain a white powder. The XRD diffraction pattern shows that it is an A-type molecular sieve with an LTA structure, with an average particle size of 130 nm.

[0067] According to literature reports, 130nm A molecular sieve seed crystals were adsorbed on the cleaned α alumina surface, and then placed in the same solution as the above synthetic seed crystals. After crystallization at 100°C for 3 days, they were taken out, and the film was washed with deionized water. The surface is naturally dry in the air. The XRD diffraction pattern shows that the film is a type A molecular sieve with LTA structure.

[0068] Take two 2×2cm size A molecular sieves, one piece is calcined i...

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Abstract

The invention provides a production method of non-crack micro or a meso pore membrane used for eliminating a template agent with the adoption of an ultraviolet photolysis technology, and the non-crack micro or the meso pore membrane thereof. Non-crack micro or the meso pore membrane is prepared by eliminating an organic matter (including a guiding agent, a template agent, a surfactant, and an organic matter in creatures, etc.) which is mainly composed of an organic template agent in the pore channel of the non-crack micro or the meso pore membrane, with the adoption of the ultraviolet photolysis technology. The technology not only avoids the generation of crack in the micro or the meso pore membrane, but also operates conveniently and saves the energy, thereby greatly shortening the time to remove the organic template agent.

Description

technical field [0001] The present invention relates to a method for manufacturing a micro / mesoporous film and the micro / mesoporous film thereof. Specifically, the present invention relates to a method for manufacturing a crack-free micro / mesoporous film using template technology and a crack-free micro / mesoporous film. Porous film. Background technique [0002] According to the pore size, porous materials can be divided into: Microporous (pore diameter<2nm), mesoporous (Mesoporous, pore diameter 2-50nm) and macroporous (Macroporous, pore diameter>50nm) materials. Due to the large internal surface area of ​​porous materials, they are widely used in catalysts and adsorption carriers. Due to the application of micro / mesoporous materials in high-tech aspects such as optoelectronics and sensing (such as sensors, separation membranes, low-electronic continuous materials and laser media), their status is becoming more and more important. There has been considerable interest...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 李庆华袁昊解丽丽王利军
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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