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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-sensitive substrates, such as semiconductors, thin metal film substrates, and organic materials.
[0027] In summary, no matter which method is used, although the organic matter in the pores can be removed eventually, it does not fully solve the particle aggregation and prevent the generation of film cracks.

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

Embodiment 1

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

[0058] Adsorb 60nm Silicalite-1 seeds with MFI structure on the surface of the cleaned α-alumina, and then put 5 parts of TPAOH: 25 parts of SiO 2 : 480 H 2 O: 100 parts of EtOH (TPAOH: tetrapropylamine hydroxide, EtOH: ethanol, SiO 2 : ethyl orthosilicate) mixed solution, crystallized at 100°C, took it out after 3 days, washed the surface of the film with deionized water, and dried it naturally in the air. XRD diffraction pattern s...

Embodiment 2

[0062] Put the cleaned ceramic sheet into 0.14-0.3 parts of CTAB: 7.4-15 parts of NH 4 OH: 1.0 parts of SiO 2 : 70-100 parts of H 2 O(CTAB: cetyltrimethylammonium bromide, SiO 2 : tetraethyl orthosilicate) in the synthetic ratio solution, crystallize at 20-40°C for 10-200 minutes, and obtain a transparent film on the silicon chip. The XRD diffraction spectrum shows that it is MCM-41 with a two-dimensional hexagonal structure (in 1992, Mobil researchers used alkyl quaternary ammonium salt type cationic surfactants as templates for the first time, and synthesized a compound with a single pore size under alkaline conditions. Mesoporous silicate materials, collectively referred to as M41S, including hexagonal MCM-41, cubic MCM-48 and layered MCM-50) mesoporous films.

[0063] Take two pieces of MCM-41 mesoporous membranes with a size of 2×2 cm, put one piece into a horse boiling furnace for calcination, raise the temperature from room temperature to 550 ℃ at a heating rate of 0...

Embodiment 3

[0066] 8.0 parts (TMA) 2 O: 0.22 parts of Na 2 O:Al 2 o3 : 5.0 parts of SiO 2 : 400 copies of H 2 O(TMAOH: Tetramethylamine Hydroxide, SiO 2 : ethyl orthosilicate) mixed solution was hydrolyzed for 12-48 hours under stirring; then placed in a water bath at 60°C for 3-5 days to obtain a white powder. The XRD diffraction pattern shows that it is A-type molecular sieve with LTA structure, and the average particle size is 130nm.

[0067] According to the literature report, adsorb 130nm A-type molecular sieve seed crystals on the surface of the cleaned α-alumina, then put it into the same solution as the above-mentioned synthetic seed crystals, take it out after crystallization at 100°C for 3 days, and wash the film with deionized water Surface, dry naturally in the air. The XRD diffraction pattern shows that the film is a type A molecular sieve with LTA structure.

[0068] Take two pieces of A-type molecular sieves with a size of 2×2cm, and put one piece into a horse boilin...

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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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