• 한국광물학회지
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• 제25권4호
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• pp.271-282
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• 2012

비정질 실리카겔은 Si와 O로 이루어진 가장 간단한 화합물로서, 표면에 다양한 구조의 물과 수산기, 그리고 합성과정에서 형성된 유기 리간드(ligand)를 함유하고 있어, 지권, 수권, 그리고 생물권의 상호작용을 이해하는 모델 시스템으로서 의미를 갖는다. 본 연구에서는 $^{17}O$ NMR 분광분석을 통해 비정질 실리카겔의 Si-O-Si와 Si-OH 산소 원자환경의 차이를 규명하고자 하였다. 이를 위해 $SiCl_4$의 수화반응을 통해 $^{17}O$이 집적된 비정질 실리카겔을 합성하였다. $^1H$과 $^{29}Si$ NMR 분광분석 결과, 비정질 실리카겔 표면에는 다양한 수소결합 세기를 가진 물과 수산기 이외에, Si-$O{\cdots}R$ 형태의 유기 리간드가 존재함을 확인하였다. 이와 같은 유기 리간드는 에탄올 또는 증류수를 이용해 비정질 실리카겔을 초음파 세척함으로써 상당부분 제거 가능하다. $^{17}O$ NMR 분광분석 결과, 짧은 펄스 길이($0.175{\mu}s$)를 이용한 $^{17}O$ NMR 스펙트럼에서 Si-O-Si와 Si-OH 산소원자 환경이 거의 구분되지 않고 나타나는 반면, 특정 실험조건($2{\mu}s$ 펄스길이)의 $^{17}O$ NMR 스펙트럼에서는 약 0 ppm에서 빠른 동역학적 특성을 가지는 Si-OH로 추정되는 피크가 관찰되었다. 이 피크는 비정질 실리카겔 표면의 유기 리간드가 제거됨에 따라 더 뚜렷하게 관찰되며, 이는 유기 리간드와 비정질 실리카의 산소원자 사이의 상호작용이 존재함을 지시한다. 이와 같은 상호작용은 비정질 실리카겔 표면의 수산기의 원자구조에 대한 정보를 제공하며, 이를 통해 규산염 지구물질의 탈수반응 기작에 대한 이해를 고양시킬 수 있다. 따라서 궁극적으로 지구물질의 탈수반응에 기인하여 일어나는 섭입대의 중간깊이(약 70~300 km)에서 일어나는 지진의 미시적인 원인에 대한 실마리를 제시할 것으로 기대된다.

• Bulletin of the Korean Chemical Society
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• 제25권7호
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• pp.965-968
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• 2004

H-montmorillonite was modified by interlayer surface silylation using 3-aminopropyltriethoxysilane and dodecylamine in ethanol without a pre-swelling step. Dodecylamine acts as a gallery expander and silylation catalyst. The evaporation of ethanol from the dispersion yields well-ordered silylated montmorillonites with large basal spacing between 1.50 and 4.20 nm. Solid-state $^29Si$ CP MAS NMR of the silylated samples showed $Q^2\;and\;Q^3$ signals as well as $T^2\;and\;T^3$ signals. The increase in the relative intensity of $Q^3\;for\;Q^2$ and the appearance of $T^2\;and\;T^3$ signals was attributed to the grafting of 3-aminopropyltriethoxysilane to the interlayer surface silanol groups.

• 한국환경과학회지
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• 제12권4호
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• pp.481-485
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• 2003

Two types of polyimide/silica composite films were prepared using sol-gel method through hydrolysis and polycondensation of tetraethoxysilane (TEOS) with the polyamic acid (PAA) and end-capped PAA solution. Samples were characterized by the means of differential thermogravimetry, X-ray diffractometry, scanning electron microscopy, universal test, impedance analyzer, chemical resistance test, etc. All of the PAA/silanol solutions heat-treated at 300$^{\circ}C$ for 6h were transformed to polyimide/silica composites. It has been demonstrated that the properties of polyimide/silica composites were affected by the amount of silica addition and the bend type existed between polyimide and silica.

• 한국분말재료학회지
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• 제9권5호
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• pp.365-369
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• 2002

Silica hydrogel was synthesized by the reaction of liquid sodium silicate with sulfuric acid. The condensation polymerization of the synthesized hydrogel was carried out via an aging process under the acidic or alkaline conditions. Nano porous silica with the pore size below 3 nm and surface area of $715m^2/g$, was obtained by the above processes in acidic ranges(pH : 3~5). The pore size and surface area of the silica varied with pH, and in alkaline ranges(pH : 8~10), those were 21 nm and $300m^2/g$ respectively. The characteristics of the silica varied with the thermal treatment which caused the change of surface area, pore volume and pore diameter.

• 한국세라믹학회지
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• 제40권10호
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• pp.1021-1026
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• 2003

탄소재의 수지함침은 탄소재 표면 상태에 영향을 받는다. Coupling처리에 의한 탄소재 표면처리는 수지와의 호환성과 젖음성을 개선시켜 함침효율과 물성을 향상시킨다. 본 연구에서는 표면개질을 위해 탄소재를 실란 coupling 처리하였다. FT-IR 관찰결과 실라놀은 탄소재 표면에 단층으로 코팅되었음을 확인하였다. 탄소재의 coupling 처리는 함침효율을 향상시켜 기공율, 기계적 강도, 밀도, 마찰거동이 개선되었다.

• Macromolecular Research
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• 제16권5호
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• pp.399-403
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• 2008

Monodisperse, micron-sized, hybrid particles having a core-shell structure were prepared by coating the surface of poly(methyl methacrylate)(PMMA) microspheres with silica and by copolymerizing acrylamide (AAm) to supply the hydrogen bonding effect by means of the amide groups. Tetraethoxysilane (TEOS) was then slowly dropped onto the medium under certain conditions. Because of the hydrogen bonding between the amide of the PMMA particles and the hydroxyl group of the hydrolyzed silanol, a silica shell was generated on the PMMA core particles. The morphology of the hybrid particles was investigated with transmission (TEM) and scanning (SEM) electron microscopy as a function of the medium conditions and the amount of TEOS. Improved thermal properties were observed by TGA analysis.

• Elastomers and Composites
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• 제27권4호
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• pp.255-261
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• 1992

Chlorosulfonated polyethylene(CSM) was moisture-cure after treating them with silane coupling agents such as ${\gamma}-mercapto$ propyl trimethoxy silane, ${\gamma}-glycidoxy$ propyl triethoxy silane and methyl triethoxy silane, 3-(trimethoxy silyl) propyl methacrylate and 3-thiocyanopropyl triethoxy silane. The cure reaction is composed two steps. The first is the reaction between chlorosulfonyl groups of CSM and silane coupling agents. The second is the formation of cross-links which are siloxane linkage. The linkage is formed by the condensation of silanol groups which are produced by the hydrolysis of alkoxysilyl groups. CSM was mixed with MPS etc., and dilaurate dilaurate as catalyst on two open mill and the compounds were lured in hot water at $70^{\circ}C$ Physical properties of moisture-cured CSM was measured. CSM was effectively moisture-cured and r-mercapto propyl trimethoxy silane and r-glycidoxy propyl trimethoxy silane were capable of the vulcanizing agents.

• 대한화장품학회지
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• 제13권1호
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• pp.15-28
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• 1987

Silica spheres were prepared by interfacial reaction method. Factors in-fluencing to the mean particle size and specific surface area of silica spheres were investigated. The experiment about the surface modification of silica spheres was carried out. It was observed that silica spheres have characteristics of the spherical shape with the vacancy in the inner side, high surface area, and reaction tendency by many silanol group. The mean particle size of silica spheres is dependent on the surfactant concentration and W/O ratio. The specific surface area is influenced by SiO2/Na2O mole ratio in sodium silicate. Silica spheres coated with titanium dioxide or zirconium dioxide improve the UV protection effect. Titanate and silane coupling agent make chemical bond with silica surface and improve the organophile and the dispersibility of silica spheres.

• Bulletin of the Korean Chemical Society
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• 제17권8호
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• pp.696-699
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• 1996

Silicate and borosilicate gels were prepared by the sol-gel process and thermally treated in the 150-850 ℃ temperature range. Solid-state 1H MAS and 29Si CP/MAS NMR spectroscopy were used to investigate the effects of heat treatments on the silicate gel to glass conversion process. The 1H NMR isotropic chemical shifts and the relative intensities of hydrogen bonded and isolated silanol groups have been used to access the information concerning the dehydration process on the silicate gel surface. The 29Si NMR isotropic chemical shifts affected by the local silicon environment have been used to determine the degree of crosslinking, i.e. the number of siloxane bonds. These NMR results suggest that the silicate gel to glass conversion process is occurred by two stages which are dependent on the temperature; (1) the formation of particles up to 450 ℃ and (2) the formation of large particles by aggregation of each separated single particle above 450 ℃. In addition, the effects of B atom on the formation of borosiloxane bonds in borosilicates have been discussed.

• Bulletin of the Korean Chemical Society
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• 제20권6호
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• pp.715-719
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• 1999

The incorporation of cobalt into mesoporous molecular sieves MCM-41 and MCM-48 was carried out. Co-PO/MCM41 and Co-PO/MCM48 were prepared using Co(II) acetate solution adjusted to pH = 3.0 with phosphoric acid by the incipient wetness method. Photoacoustic spectroscopy (PAS) was used to study the local environments of Co(II) incorporated into mesopores. The band around 500 nm in PAS of as-prepared Co-PO/MCM41 and Co-PO/MCM48 with Co(II) acetate solution was changed to triplet bands around 600 nm. This could be assigned to the 4 A2(F)-> 4T1(P) transition of Co(II) surrounded tetrahedrally by oxygen ions after calcination. It may be attributable to that the octahedral cobalt species containing phosphate ligands in coordination sphere reacting with framework's silanol groups to be dispersed atomically onto the surface of mesoporous molecular sieves as a tetrahedral species. This is unlike that the Co in Co-Cl/MCM41 and direct-synthesized Co-MCM41 transforms to Co oxide phase upon calcination. Co-PO/MCM41 and Co-PO/MCM48 were stable while treated with water.