• 대한금속재료학회지
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• 제47권8호
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• pp.516-521
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• 2009

In this study we report a rapid synthesis of nanoporous organo-functional silica (OFS) with unimodal and bimodal pore structures encompassing pores ranging from meso-to macroscale. The problems of tediousness and high production cost in the conventional syntheses are overcome by co-condensation of an inexpensive inorganic precursor, sodium silicate with an organosilane containing trimethyl groups. The insitu covalent anchoring of the non-polar trimethyl groups to the inner pore walls prohibits irreversible shrinkage of the wet-gel during microwave drying at ambient pressure and thus larger size pores (from ca. 20 to ca. 100 nm) can be retained in the dried silica. The drying process of the silylated wet-gels at an ambient pressure can be greatly accelerated upon microwave exposure instead of drying in an oven or furnace. Using this approach, anoporous and superhydrophobic silicas showing a wide variation in texture and morphology can be readily synthesized in roughly two hours. The effects of various sol-gel parameters solely on the textural properties of the organo-functional silica (OFS) have been investigated and discussed.

• 한국재료학회지
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• 제22권6호
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• pp.275-279
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• 2012

(3-mercaptopropyl)trimethoxysilane (MPTMS) was used as a silylation agent, and modified silica nanoparticles were prepared by solution polymerization. 2.0 g of silica nanoparticles, 150 ml of toluene, and 20 ml of MPTMS were put into a 300 ml flask, and these mixtures were dispersed with ultrasonic vibration for 60 min. 0.2 g of hydroquinone as an inhibitor and 1 to 2 drops of 2,6-dimethylpyridine as a catalyst were added into the mixture. The mixture was then stirred with a magnetic stirrer for 8 hrs. at room temperature. After the reaction, the mixture was centrifuged for 1 hr. at 6000rpm. After precipitation, 150 ml of ethanol was added, and ultrasonic vibration was applied for 30 min. After the ultrasonic vibration, centrifugation was carried out again for 1 hr. at 6000rpm. Organo-modification of silica nanoparticles with a ${\gamma}$-methacryloxypropyl functional group was successfully achieved by solution polymerization in the ethanol solution. The characteristics of the ${\gamma}$-mercaptopropyl modified silica nanoparticles (MPSN) were examined using X-ray photoelectron spectroscopy (XPS, THERMO VG SCIENTIFIC, MultiLab 2000), a laser scattering system (LSS, TOPCON Co., GLS-1000), Fourier transform infrared spectroscopy (FTIR, JASCO INTERNATIONL CO., FT/IR-4200), scanning electron microscopy (SEM, HITACHI, S-2400), an elemental analysis (EA, Elementar, Vario macro/micro) and a thermogravimetric analysis (TGA, Perkin Elmer, TGA 7, Pyris 1). From the analysis results, the content of the methacryloxypropyl group was 0.98 mmol/g and the conversion rate of acrylamide monomer was 93%. SEM analysis results showed that the organo-modification of ultra-fine particles effectively prevented their agglomeration and improved their dispensability.