• Journal of the Korean Chemical Society
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• v.51 no.3
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• pp.232-239
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• 2007

The reaction of 1,1'-bis(dimethylsilyl)ferrocene with various aldehydes in the presence of a catalytic amount of Ni(PEt3)4 lead to the acyclic products by monohydrosilylation. The same reaction in the presence of a catalytic amount of (C2H4)Pt(PPh3)2 leads to the different cyclic six membered ring compound by double silylation. Platinum catalyzed double silylation of 4-cyanobenzaldehyde was generated 5,6-ferrocenylene-1,1,4,4,-tetramethyl-2-oxa-2- cyanophenyl-1,4-disylacyclehexane which was crystallized to have crystal structure.

• Journal of the Microelectronics and Packaging Society
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• v.26 no.4
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• pp.127-132
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• 2019

In this study, barium strontium titanate (BSTO) with high dielectric perovskite structure was synthesized by liquid-solid solution synthesis and the surface was modified using trimethylsilyl chloride (TMCS) as a silylation agent. Silylation surface modification is a method of reacting -OH ligand on the surface of BSTO nanoparticles with Cl in TMCS to generate HCl and replacing the ligand on the surface of nanoparticles with -Si, -CH₃. Silylation was optimized by varying the concentration of TMCS, and the structure of the silicon network was confirmed by Fourier-transform infrared spectroscopy. In addition, the crystallinity of BSTO nanoparticles was confirmed by X-ray diffractometer and the size of the nanoparticles was calculated using Scherrer equation. The field emission scanning electron microscopic image observed the change of the surface-modified BSTO particle size, and the contact angle measurement confirmed the hydrophobic property of the contact angle of 120.9° in the optimized nanoparticles. Finally, the surface-modified BSTO dispersion experiment in de-ionized water confirmed the hydrophobic degree of the nanoparticles.

• Analytical Science and Technology
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• v.5 no.4
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• pp.455-464
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• 1992

Using FT-IR, we determined the depth of silylated layers produced from various gas-phase-silylation conditions was proposed by using Fourier Transform Infrared (FT-IR) spectroscopic analysis. The depth of silylated layer was determined from absorbance measurments of the significant peaks (Si-O-ph, Si-C, Si-H) of FT-IR spectra with background spectrum subtraction method. And the results were compared with thickness measurments of SEM. The results were well agree with SEM. It found to be well suited for determining silylation process window.

• Proceedings of the IEEK Conference
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• 1999.06a
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• pp.922-925
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• 1999

The Silylation photo-resist etch process was tested by Enhanced-ICP dry etcher. The comparison of the two process results of micro pattern etching with 0.25${\mu}{\textrm}{m}$ CD by E-ICP and ICP reveals that E-ICP has better quality than ICP The etch rate and the microloading effect was improved in E-ICP Especially, the problem of the lateral etch was improved in E-ICP.

• Bulletin of the Korean Chemical Society
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• v.25 no.7
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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.

• Journal of Food Hygiene and Safety
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• v.10 no.4
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• pp.239-247
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• 1995

Analytical method for saccharin in foods was developed using gas chromatography/mass spectrometry(GC/MS). Methylation with diazomethane, acetylation with MBTFA, and silylation with MSTFA and MTBSTFA were compared. Methylation of saccharin produced N-methylated saccharin as the major product and O-methylated saccharin as the minor one. Silylation of saccharin with MSTFA and MTBSTFA reasulted in the formation of the correponding O-silylated products, respectively. The derivatization of saccharin was optimized with MSTFA. The ions at m/z 240, 255, and 166 were monitored to characterize saccharin.

• Journal of the Korean Chemical Society
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• v.46 no.2
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• pp.139-144
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• 2002

The nickel-catalyzed reation of 1,1'-bis(dimethysilyl)ferrocene[1] with carbonyls such as benzaldehyde, 4-cyaonbezaldehyde, trimethylacetaldehyde, acethon, and benzophenone afforded 3-oxa-2,5-disilacyclo-1,1'-ferrocene. In contrast, the reation of [1] with isobutyraldehyde under the same reation condition yielded the diinsertion products formed via the insertion of two aldehyde ligands into the Si-H bond of 1,1'-bis(dimethy)ferrocene.

• Korean Chemical Engineering Research
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• v.55 no.3
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• pp.401-408
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• 2017

In preparation of self-repairing polymer-modified waterproofing asphalt-montmorillonite (MMT) composite, silylation-modification characteristics of cation ($Na^+$) exchanged K-10 (Na-MMT-K) using 3-aminopropyltriethoxysilane (APS) were studied and the optimal conditions of its silylation-modification process were proposed by use of the results of XRD analysis on silylation-modified Na-MMT-K (S-Na-MMT-K) under various conditions. According to XRD results, it was confirmed that peaks of Na-MMT-K were simultaneously consistent with those of K-10 and natural or Ca-MMT modified Na-MMT. Similarly, S-Na-MMT-K was observed to have two basal spacings ($d_{001}$), among which the area-ratio of a secondary (001) peak ($2{\theta}=3.9{\sim}4.2^{\circ}$) to a primary (001) peak ($2{\theta}{\sim}8.838^{\circ}$) was suggested to be a criterion to represent a degree of APS silylation-modification. Then, the optimal conditions on APS-stirring period prior to APS-MMT reaction, APS-MMT reaction period, APS concentration and reaction temperature at the highest area-ratio were turned out to be 20 min, 2~3 hr, 7.5 w/v% and $50^{\circ}C$, respectively.

• Korean Chemical Engineering Research
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• v.55 no.3
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• pp.409-418
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• 2017

In preparation of self-repairing polymer-modified waterproofing asphalt-montmorillonite (MMT) composite, silylation-modification characteristics of cation ($Na^+$) exchanged K-10 (Na-MMT-K) using 3-aminopropyltriethoxysilane (APS) were studied and the optimal conditions of its silylation-modification process were proposed by use of the results of instrumental analysis, including FTIR, XRD, NMR and TGA, on silylation-modified Na-MMT-K (S-Na-MMT-K) under various conditions. According to FTIR analysis on S-Na-MMT-K, its peak-strengths of Si-O, -$NH_2$, -$CH_2$- and -OH, correlated with APS silylation-modification reaction, were compared each other. As a result, its optimal conditions including APS-MMT reacting period, APS-stirring period prior to APS-MMT reaction, APS concentration and reaction temperature were turned out to be 2~3 h, 20 min, 7.5 w/v% and $50^{\circ}C$, respectively. In addition, the optimal conditions induced from the results of TGA were also nearly consistent to those according to the results of FTIR analyses. These optimal conditions were turned out to be almost consistent to those drawn according to a criterion from XRD results suggested previously by Lee et al., by which the criterion was validated.

• Clean Technology
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• v.16 no.3
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• pp.191-197
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• 2010

Repair reaction of plasma damaged porous methyl doped SiOCH films was carried out with silylation agents dissolved in supercritical carbon dioxide ($scCO_2$) at various reaction time, pressure, and temperature. While a decrease in the characteristic bands at $3150{\sim}3560cm^{-1}$ was detectable, the difference of methyl peaks was not identified apparently in the FT-IR spectra. The surface hydrophobicity was rapidly recovered by the silylation. In order to induce effective repair in bulk phase, the wafer was heat treated before reaction under vacuum or ambient condition. The contact angle was slightly increased after the treatment and completely recovered after the subsequent silylation. Methyl groups were decreased after the plasma damage, but their recovery was not identified apparently from the FT-IR, spectroscopic ellipsometry, and secondary ion mass spectroscopy analyses. Furthermore, Ti evaporator was performed in a vacuum chamber to evaluate the pore sealing effect. The GDS analysis revealed that the open pores in the plasma damaged films were efficiently sealed with the silylation in $scCO_2$.