• 접착 및 계면
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• 제7권4호
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• pp.39-44
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• 2006

A new kind of silicone-epoxy composite is reported in this research. The silicone-epoxy resin was synthesized by the hydrosilylation of tetramethycyclotetrasiloxane and 4-vinyl-1-cyclohexene 1,2-epoxy with a high reaction yield. It was found that the obtained silicone-epoxy resin shows a high reactive activity to the aluminum complex-silanol catalyst. The resin could be cured under the catalysis of $(Al(acac)_3/Ph_2Si(OH)_2$ at a concentration below 0.1 wt% to give a hard cured resin showing excellent optical clarity, UV resistance and thermal stability. It was also found that the Si-H groups facilitated the curing reaction and the silicone-epoxy resin bearing Si-H group could be cured effectively even if $Ph_2Si(OH)_2h$ was absent. Moreover, the UV resistance and thermal stability were improved significantly by the introduction of Si-H groups. This is possibly due to the reductive property of Si-H groups which can annihilate radical and peroxide effectively. This kind of silicone-containing epoxy composite might have very promising applications as optical resin, optical adhesive and encapsulation materials for electronic devices.

• 한국세라믹학회지
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• 제45권2호
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• pp.119-125
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• 2008

The FAS(Fluoroalkylsilane)/Nafion inorganic-organic composite electrolyte membrane was successfully fabricated through sol-gel method. The FAS having hydrophobic functional group and silanol ligands is impregnated in $Nafion^{(R)}$ membrane to reduce methanol crossover. The prepared FAS/Nafion inorganic-organic composite electrolyte membrane consist of the hydrophobic FAS-derived silicate nano-particles and $Nafion^{(R)}$ matrix showed decrease of methanol crossover and reduction of humidity dependence without large sacrifice of proton conductivity. The microstructural analysis of the composite membranes was performed using FESEM and FTIR. And the effect of the incorporation of the hydrophobic FAS-derived silicate nano-particles into $Nafion^{(R)}$ membrane was investigated via solvent uptake, membrane expansion rate, humidity dependency of proton conductivity and contact angle measurement.

• 폴리머
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• 제28권2호
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• pp.170-176
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• 2004

반응조건에 따른 실록산으로 코팅된 마그네타이트 나노입자의 크기 및 분포를 동적광산란을 이용하여 조사하였다. FT-IR로부터 마그네타이트의 표면에 히드록시기가 존재함을 확인하였고 이 히드록시기는 코팅된 실록산의 실란올과 수소결합을 이루고 있음이 확인되었다. 제조된 나노입자의 크기는 반응온도가 증가함에 따라 입자크기는 증가하였고 단량체 함량과 교반 속도의 증가에 따라서는 감소하였다. 입자 크기 분포는 반응조건에 따라서 약간의 변화는 있지만 전체적으로 14∼41nm 크기의 범위를 나타냈다. 제조된 마그네타이트의 자성특성은 vibrating sample magnetometer를 이용하여 초상자성임이 확인되었고 실록산으로 코팅된 나노입자 역시 초상자성을 나타냄을 확인하였다. 반응조건에 따라서는 반응온도가 증가할수록 포화자화강도는 증가하였고 단량체 함량과 교반 속도가 증가함에 따라서 포화자화강도가 감소하는 것을 나타내었다.

• Elastomers and Composites
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• 제55권3호
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• pp.215-221
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• 2020

Silica/SBR (styrene-butadiene rubber) compounds are the primary constituents of tire treads. Furthermore, the excellent dynamic viscoelastic properties of silica lead to good fuel efficiencies. However, the silanol group on the surface of silica does not mix well with non-polar rubber because of its polarity. This incompatibility causes aggregation due to the occurrence of hydrogen bonding between the hydroxyl groups, thereby reducing the dispersibility of silica. Recently, the wet master batch (WMB) process has been applied to overcome these disadvantages, and research on silica dispersants that can be used in the WMB process has been increasing. In this study, we prepared silica/SBR compounds by using three types of eco-friendly cellulose-based dispersants in the WMB process, namely: cellulose-, sodium carboxymethyl cellulose, and nanocellulose-based dispersants. Subsequently, we compared the vulcanization characteristics, viscoelastic properties, and mechanical properties of the compounds. The silica dispersibility in the rubber compounds was improved with the addition of the nano-cellulose dispersant, resulting in the enhancement of the workability, hardness, tensile strength, and wear resistance of the SBR compound.

• 접착 및 계면
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• 제7권4호
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• pp.32-38
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• 2006

A series of organic-inorganic hybrids, PCL/EP/$SiO_2$, involving epoxy resin and triethoxysilane-terminated polycaprolactone elastomer (PCL-TESi) were prepared via polymerization of diglycidyl ether of bisphenol A (DGEBA) with amine curing agent KB-2 and sol-gel process of PCL-TESi. The curing reactions were started from the initially homogeneous mixture of DGEBA, KB-2 and the PCL-TESi. The organicinorganic hybrids containing up to 4.95% (wt) of $SiO_2$ were obtained and characterized by FT-IR, transmission electron microscopy (TEM), differential scanning calorimetry (DSC) and thermogravimetry analysis (TGA). It was experimentally shown that the swelling property in toluene, morphologies and thermal properties of the resulting hybrids were quite dependent on the contents of $SiO_2$. The crosslink network density decreases with increasing of the PCL-TESi. And in TEM, the phase separated morphology of these hybrids was found, which resulted from the coagulation of Si-O-Si networks resulting from $-Si(OC_2H_5)_3$ of PCL-TESi self-curing by hydrolytic silanol condensation, with the advancement of the curing reaction in the modified epoxy resin systems. Meanwhile, the change of the $SiO_2$ content made the morphologies changed from aggregated particles of Si-O-Si in the hybrid to nanocluster of interconnected Si-O-Si particles, then to aggregated Si-O-Si dispersing in the continuous cured epoxy phase again, and last to co-continuous interpenetrating network. The glass transition behavior of the hybrid material was cooperative motion of large chain segments, which were hindered by the inorganic Si-O-Si network. And in TG analysis, the characteristic temperature at 5% of weight loss was evidently increased from $120.5^{\circ}C$ of pure cured epoxy to $277.6^{\circ}C$ of 3.84% (wt) of $SiO_2$ modified epoxy due to the existence of Si-O-Si when PCL-TESi was added in the hybrid.

• Bulletin of the Korean Chemical Society
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• 제25권5호
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• pp.681-686
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• 2004

Ti-ZSM-5 prepared by secondary synthesis, from the reaction of H-ZSM-5 with vapor phase $TiCl_4$, was characterized with several physicochemical techniques including FT-IR and UV/VIS-DRS. It was found that zeolite structure, surface area and pore volume did not change, and the framework aluminum could not be replaced by titanium atom during the secondary synthesis of Ti-ZSM-5. The incorporation of titanium into the framework might be due to reaction of $TiCl_4$with the silanol groups associated with defects or surface sites. The formation of extra-framework titanium could not be avoided, unless the samples were further treated by water vapor at 550 $^{\circ}C$ or higher temperature. High temperature steam treatment of Ti-ZSM-5 prepared by chemical vapor deposition with $TiCl_4$was efficient to prevent the formation of non-framework titanium species. Ti-ZSM-5 zeolites prepared in this work contained only framework titanium species and exhibited improved catalytic property close to TS-1 prepared by hydrothermal synthesis.

• 한국재료학회지
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• 제22권8호
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• pp.433-438
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• 2012

A chemical process involves polymerization within microspheres, whereas a physical process involves the dispersion of polymer in a nonsolvent. Nano-sized monodisperse microspheres are usually prepared by chemical processes such as water-based emulsions, seed suspension polymerization, nonaqueous dispersion polymerization, and precipitation polymerizations. Polymerization was performed in a four-necked, separate-type flask equipped with a stirrer, a condenser, a nitrogen inlet, and a rubber stopper for adding the initiator with a syringe. Nitrogen was bubbled through the mixture of reagents for 1 hr. before elevating the temperature. Functional silane (3-mercaptopropyl)trimethoxysilane (MPTMS) was used for the modification of silica nanoparticles and the self-assembled monolayers obtained were characterized by X-ray photoelectron spectroscopy (XPS), laser scattering system (LSS), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), elemental analysis (EA), and thermogravimetric analysis (TGA). In addition, polymer microspheres were polymerized by radical polymerization of ${\gamma}$-mercaptopropyl modified silica nanoparticles (MPSN) and acrylamide monomer via precipitation polymerization; then, their characteristics were investigated. From the elemental analysis results, it can be concluded that the conversion rate of acrylamide monomer was 93% and that polyacrylamide grafted to MPSN nanospheres via the radical precipitation polymerization with AAm in ethanol solvent. The microspheres were successfully polymerized by the 'graft from' method.

• 폴리머
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• 제25권4호
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• pp.512-520
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• 2001

섬유강화 복합재료의 물성을 결정하는 주요 인자중 하나는 계면결합력이다. 본 연구에서는 유리섬유와 PC/SAN 블렌드를 대상으로 하여 계면결합력을 측정하였으며 SAN함량을 0-30 wt%까지 변화시켜 실험하였다. 계면결합력 측정에는 Single Fiber Fragmentation Test법을 사용하였는데 SAN 함량이 증가할수록 계면결합력이 증가하였다. 한편 계면결합력을 증가시키기 위해 PC/SAN 혼련물을 개질하고자 소량의 SMA를 혼합하였으며, 유리섬유 표면을 실란 커플링제로 처리하여 관능기를 도입하였다. 계면결합력은 SAN/SMA계의 상용성에 크게 영향을 받았으며, 비상용성 SAN/SMA계보다 상용성 SAN/SMA계에서 계면결합력이 증가하였다. 또한 상용성 SAN/SMA계에서는 계면결합력이 SMA 내의 MA 함량이 아닌 전체 계내의 MA 함량에 의존하였으며 그 최적 함량은 0.4wt%였다.

• Elastomers and Composites
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• 제50권2호
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• pp.110-118
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• 2015

In this study, diethylaminoethyl methacrylate-styrene-butadiene terpolymer (DEAEMA-SBR), in which diethylaminoethyl methacrylate (DEAEMA) was introduced to the SBR molecule as a third monomer, was synthesized by cold emulsion polymerization. It is expected that amine group introduced to a rubber molecule would improve dispersion of silica by the formation of hydrogen bond (or ionic coupling) between the amine group and silanol groups of silica surface. The chemical structure of DEAEMA-SBR was analyzed using proton nuclear magnetic resonance spectroscopy (H-NMR), Fourier transform infrared spectroscopy (FTIR), gel permeation chromatography (GPC) and differential scanning calorimetry (DSC). Then, various properties of DEAEMA-SBR/silica composite such as crosslink density, bound rubber content, abrasion resistance, and mechanical properties were evaluated. As a result, bound rubber content and crosslink density of DEAEMA-SBR/silica compound were higher than those of the SBR 1721 composite. Abrasion resistance and moduli at 300% elongation of the DEAEMA-SBR/silica composite were better than those of SBR 1721 composite due to the high bound rubber content and crosslink density. These results are attributed to high affinity between DEAEMA-SBR and silica. The proposed study suggests that DEAEMA-SBR can help to improve mechanical properties and abrasion resistance of the tire tread part.

• 한국광물학회지
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• 제13권4호
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• pp.186-195
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• 2000

To study phosphate adsorption on kaolinite, $^{31}$ P MAS NMR(magic angle spinning nuclear magnetic resonance spectroscopy)has been used for kaolinite reacted in 0.1 M phosphate solutions at pH’s from 3 to 11. There are at least 3 different forms of phosphate on kaolinite. One is the phosphate physically adsorbed on kaolinite surface (outer-sphere complexes) or species left after vacuum-filtering. The second is the phosphate adsorbed by ligand exchange (inner-sphere complexes), and the third is Al-phosphate precipitates which are pH dependent. Most of the inner-spherer complexes and surface precipitates are mainly on hydroxided Al(aluminol) rather than hydroxided Si(silanol). These are pertinent with the results obtained from the phosphate adsorption experiments on silica gel and ${\gamma}$-Al$_2$O$_3$ as model compounds, respectively. The two peaks with more negative chemical shifts(more shielded) than the ortho-phosphate peak (positive chemical shift) are assigned to be the inner-sphere complexes and surface precipitates. The $^{31}$ P chemical shifts of the Al-phosphate precipitates are more negative than those of inner-sphere complexes at a given pH due to the larger number of P-O-Al linkages per tetrahedron. The chemical shifts of both the inner-sphere complexes and surface precipitates are more negative than those of inner-sphere complexes at a given pH due to the larger number of P-O-Al linkages per tetrahedron. The chemical shifts of both the inner-sphere complexes and surface precipitates become progressively less shielded with increasing pH. For the inner-sphere complexes, decreasing phosphate protonation combined with peak averaging by rapid proton exchange among phosphate tetrahedra with different numbers of protons is though to be the reason for the peak change. The decreasing shielding with increasing pH for surface precipitates is probably due to the decreasing average number of P-O-Al linkages per tetrahedron combined with decreasing protonation like inner-sphere complexes.