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Preparation method of silicon oxide uniwafer material with ordered hole

A mesoporous silicon oxide, monolithic technology, applied in the direction of silicon oxide, silicon dioxide, etc., can solve the problems of long time, harsh equipment requirements, unfavorable industrial production of materials, etc., and achieve the effect of wide application

Inactive Publication Date: 2004-11-10
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods are generally demanding on equipment and require a very long time (8-12 weeks), which is very unfavorable for the industrial production of such materials, and it is difficult to obtain a single piece of mesoporous silicon oxide without cracks

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1, 1 gram of Pluronic 123 (P123, EO 20 PO 70 EO 20 ) was dissolved in a solution composed of 5 grams of ethanol and 0.2 grams of 1mol / L hydrochloric acid, stirred to dissolve, then added 2.08 grams of TEOS, and continued to stir for about 10 minutes. Move the sol into a container with a certain shape (usually a porcelain crucible), and let it stand for a period of time (the specific time depends on the temperature, humidity and ventilation at the time, generally 20-48 hours) to fully age it. Then cover the gel with a layer of liquid paraffin, place it in an oil bath and heat it at 60°C for 24 hours, take it out, and wipe off the surface liquid paraffin to obtain a single piece. Then the temperature was raised to 550°C at a speed of 0.5°C / min and fired for 6 hours to completely remove the surfactant, and a highly ordered mesoporous monolithic material was obtained. Analysis and tests by PXRD, BET, TEM, etc. show that the obtained is a high-quality two-dimen...

Embodiment 2

[0018] Embodiment 2, 1 gram of Pluronic 123 (P123, EO 20 PO 70 EO 20 ) was dissolved in a solution composed of 5 grams of ethanol and 0.2 grams of 1mol / L hydrochloric acid, stirred to dissolve, then added 2.08 grams of TEOS, and continued to stir for about 10 minutes. Move the sol into a container with a certain shape (usually a porcelain crucible), and let it stand for a period of time (the specific time depends on the temperature, humidity and ventilation at the time, generally 20-48 hours) to fully age it. Then cover the gel with a layer of liquid paraffin, place it in an oil bath and heat it at 90°C for 8-24 hours, take it out, and wipe off the surface liquid paraffin to obtain a single piece. Then the temperature was raised to 550°C at a speed of 0.5°C / min and fired for 6 hours to completely remove the surfactant, and a highly ordered mesoporous monolithic material was obtained. PXRD, BET, TEM and other analysis tests show that the obtained is a high-quality three-dime...

Embodiment 3

[0019] Example 3, 0.6 g of Brij 97 was dissolved in a solution composed of 5 g of ethanol and 0.2 g of 1 mol / L hydrochloric acid, stirred to dissolve, then 2.08 g of TEOS was added, and the stirring was continued for about 10 minutes. Move the sol into a container with a certain shape (usually a porcelain crucible), and let it stand for a period of time (the specific time depends on the temperature, humidity and ventilation at the time, generally 20-48 hours) to fully age it. Then cover the gel with a layer of liquid paraffin, place it in an oil bath and heat it at 60°C for 24 hours, take it out, and wipe off the surface liquid paraffin to obtain a single piece. Then the temperature was raised to 550°C at a speed of 0.5°C / min and fired for 6 hours to completely remove the surfactant, and a highly ordered mesoporous monolithic material was obtained. Analysis and tests by PXRD, BET, TEM, etc. show that the obtained is a high-quality two-dimensional hexagonal structure (space gro...

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Abstract

The invention relates to a process for preparing ordered porous silicon oxide single sheet material with large scale and no fracture, wherein the conventional sol-gal process is improved by introducing inert medium liquid as shape protecting agent, and solvent volatilization is realized at high temperature.

Description

technical field [0001] The invention belongs to the technical field of mesoporous silicon oxide materials, in particular to a rapid preparation method of a large-sized, crack-free mesoporous silicon oxide monolithic material. Background technique [0002] Inorganic monolithic materials prepared by the sol-gel process have great potential application value in the field of optics. Such materials have high light transmittance, are easy to be chemically doped and modified, and can be used as lenses, monochromators, and nonlinear optical media. Wait. Mesoporous molecular sieves have highly ordered pore structure, high specific surface area and excellent thermal stability, and have important practical significance in catalysis, separation, optical materials and synthesis of ordered nanostructures as hard templates. In addition to these characteristics, the mesoporous monolithic material also has a small external area, a high degree of orientation, and a large-scale continuous por...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12C01B33/14
Inventor 杨海峰施奇惠屠波赵东元
Owner FUDAN UNIV
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