• Korean Journal of Materials Research
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• v.29 no.4
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• pp.221-227
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• 2019

This study examines the role of the nano- and micro-particle ratio in dispersion stability and mechanical properties of composite resins for SLA(stereolithography) 3D printing technology. VTES(vinyltriethoxysilane)-coated $ZrO_2$ ceramic particles with different nano- and micro-particle ratios are prepared by a hydrolysis and condensation reaction and then dispersed in commercial photopolymer (High-temp) based on interpenetrating networks(IPNs). The coating characteristics of VTES-coated $ZrO_2$ particles are observed by FE-TEM and FT-IR. The rheological properties of VTES-coated $ZrO_2/High-temp$ composite solution with different particle ratios are investigated by rheometer, and the dispersion properties of the composite solution are confirmed by relaxation NMR and Turbiscan. The mechanical properties of 3D-printed objects are measured by a tensile test and nanoindenter. To investigate the aggregation and dispersion properties of VTES-coated $ZrO_2$ ceramic particles with different particle ratios, we observe the cross-sectional images of 3D printed objects using FE-SEM. The 3D printed objects of the composite solution with nano-particles of 80 % demonstrate improved mechanical characteristics.

• Economic and Environmental Geology
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• v.46 no.1
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• pp.51-61
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• 2013

Researches on the oil recovery enhancement using the nanotechnology has recently been studied in the United States. The previous researches has focused mainly on the flow characteristics of nanoparticles in porous media, and the stability of the nano-emulsion itself. However, the analysis did not deal with the size effects between a nano-emulsion and the pore size which has an important role when nano-emulsion flows in the porous media. In this research, nano-based emulsion was fabricated which is able to be applied for the enhanced oil recovery techniques and its characteristics was analyzed. In addition, in order to identify the characteristics of nano-emulsions flowing through the porous media, the size effect was analysed by filtering test. According to the results, when the emulsion was fabricated, SCA(Silane Coupling Agent) or PVA(Poly Vinyl Alcohol) are added to improve the stability of emulsion. As the ratio of the decane to water increased, the viscosity of emulsion and the droplet size also increased. For the filtering test at the atmospheric conditions, the droplet did not go through the filter; only the separated water from the emulsion was able to be filtered. This phenomenon occurred because the droplet was not able to overcome the capillary pressure. At the filtering test by suction pressure, most of the emulsion was filtered over the filter size of $60{\mu}m$. However, the ratio of filtration was rapidly degraded at less than $45{\mu}m$ filters. This is caused due to deformation and destruction of the droplet by strong shear stress when passing through the pore. The results from the study on the basic characteristic of nano-emulsion and filtering test will be expected to play as the important role for the fabrication of the stable nano-emulsion or the research on the recovery of residual oil in porous media.

• The Korean Journal of Rheology
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• v.11 no.1
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• pp.34-43
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• 1999

Flow-induced voids during resin impregnation and poor fiber wetting have known to be highly detrimental to the performance of composite parts manufactured by resin transfer molding(RTM) process. In this study, in order to overcome these serious problems encountered in RTM, the effects of surface modification by using silane coupling agent as a surface modifier on the flow characteristics, the wetting between resin and fiber, and void content were investigated. For the experiments of microscopic flow visualization and curing in a beam mold, glass fiber mats having plain weaving structure and epoxy resin were used. Modifying the fiber surface was found to result in a significant decrease of dynamic contact angle between resin and fiber and increase of wicking rate. Therefore, it was confirmed that the surface modification employed in this study could improve the wettability of reinforcing fibers as well as micro flow behavior. In addition, It was revealed that high temperature and low penetration rate of the resin are more favorable processing conditions to reduce the dynamic contact angle. However, surface modified fiber mat was found to have lower permeability than the unmodified one, which may be explained in terms of the decrease of contact time between resin and fiber owing to improvement of wetting. It was also exhibited that surface modification had a significant influence on void formation in RTM process, resulting in a decrease of overall void content due to the improvement of wetting in cured composite parts.

• Journal of the Korean Applied Science and Technology
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• v.34 no.1
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• pp.152-162
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• 2017

A hydrophilic coating solution was prepared by adding a silane coupling agent and a nano-inorganic oxide in aqueous surfactant solution to increase the efficiency of photovoltaic power generation due to the introduction of antifogging and antifouling properties on the glass surface of the solar cell module. Addition of $Ludox^{(R)}$, a nano-inorganic oxide, to 1% hydrophilic coating solution showed improved hydrophilicity and excellent antifogging effect regardless of $Ludox^{(R)}$ concentration. However, the antifouling effect on the glass surface was showed only when Ludox was added more than 10%. In the case of addition of 0.7% of hydrolyzed TEOS at pH 4, the antifogging effect was maintained as a result of the steam test as well as the antifouling effect even after the coated glass surface was rubbed 100 times with a wet Kimwipe. In addition, from the surface roughness ($R_q$) calculated using AFM data, the higher surface roughness with irregular surface shape was obtained with the higher concentration of TEOS. The addition of 0.7% of TEOS showed relatively high surface roughness and well organized surface condition which can help to improve transmittance of light. In conclusion, $Ludox^{(R)}$ is not required only for the antifogging property. However, at least 10% of Ludox should be added to show antifouling effect and 0.7% of TEOS should be added for good durability.

• Journal of the Korean Applied Science and Technology
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• v.35 no.3
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• pp.595-605
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• 2018

In recent years, researches on organic-inorganic coating films have conducted a nanocomposite system composed of organic resin matrices having excellent flexibility and chemical stability and inorganic materials having excellent mechanical properties. The o-phenylphenoxyethyl acrylate (OPPEA) used as the acrylate monomer has a high refractive index of 1.58, and the bisphenol A ethoxylate diacrylate (BAEDA) has a low refractive index but improves the chemical stability of the organic resin. In addition, zirconia used as an inorganic material exhibits excellent durability and optical properties. In this study, the BAEDA contents in acrylate monomer were controlled to produce a film with suitable optical transparency. And optimum conditions were established by comparing the changes in surface properties of PET films detected with pencil hardness tester, Abbe's refractometer, and UV-vis spectrophotometer. The hydrophobicity and the dispersibility of zirconia in acrylate monomer were much improved after modification with ${\gamma}$-methacryloxypropyltrimethoxysilane (MPS), which is a silane coupling agent. And the existence of ester C=O bond peak at $1716cm^{-1}$ introduced by MPS through FT-IR ATR spectrophotometer confirmed the completion of surface modification of zirconia with MPS. In addition, the presence of silicon atom on the surface modified zirconia was also proved using X-ray fluorescence spectrometer. When the photocurable hybrid coating was prepared by introducing chemically modified zirconia into acrylate monomer, the refractive index of this coated PET film was improved by 1.2%, compared to the only acrylate coated PET film. The homogeneous distribution of zirconia in acrylate coating layer on PET film was also identified through SEM/EDS mapping analysis technique.

• Polymer(Korea)
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• v.37 no.3
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• pp.308-315
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• 2013

In this study, we performed surface modification of silica nanoparticles with bis[3-(triethoxysilylpropyl)]tetrasulfide (TESPT) silane coupling agent to study the effects of treatment temperature, treatment time, and amount of TESPT used on the silanization degree with Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), elemental analysis (EA) and solid state $^{13}C$ and $^{29}Si$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR). We found peak area of isolated silanol groups at $3747cm^{-1}$ decreased, but peak area of $-CH_2$ asymmetric stretching of TESPT at $2938cm^{-1}$ increased with the amount of TESPT from FTIR measurements. We also used universal testing machine (UTM) to study mechanical properties of styrene butadiene rubber (SBR) nanocomposites with 20 phr (parts per hundred of rubber) of pristine and TESPT modified silicas, respectively. The tensile strength and 100% modulus of modified silica/SBR nanocomposite were enhanced from 5.65 to 9.38MPa, from 1.62 to 2.73 MPa, respectively, compared to those of pristine silica/SBR nanocomposite.

• Polymer(Korea)
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• v.38 no.2
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• pp.257-264
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• 2014

In this study, we modified silica nanoparticles with bis[3-(trimethoxysilyl)propyl]ethylenediamine (BTPED) silane coupling agent, which has two secondary amino groups in a molecule, to introduce amino groups on the silica surface. After modification of silica, we used acrylate group containing 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) to introduce polymerizable methacrylate groups by Michael addition reaction. We used Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and liquid and solid state cross polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to understand the reactions between N-H groups of BTPED modified silica surface and acrylate groups of AHM monomer. We confirmed Michael addition reaction between BTPED modified silica and AHM completed in 2 hr reaction time. We also found increased methacrylate group introduction with increase of mol ratio of the acrylate group of AHM to N-H group of BTPED modified silica by increase of C=O peak area of measured FTIR spectra. These results were also supported by EA and solid state $^{13}C$ and $^{29}Si$ NMR results.

• Korean Chemical Engineering Research
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• v.55 no.1
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• pp.60-67
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• 2017

In this study, we performed surface modification of biodegradable microcrystalline cellulose (MCC) to use as a filler in polyethylene (PE) composite in food packaging application. We modified MCC surface with (3-trimethoxysilylpropyl)diethylenetriamine (TPDT) silane coupling agent, which has one primary amino group and two secondary amino groups per molecule, to introduce amino groups with a carbon dioxide adsorption capability in MCC. Effects of each of the reaction conditions such as amount of TPDT introduced, swelling time, reaction temperature, and reaction time on surface modification degree of MCC were investigated by changing a variety of above reaction conditions. The amount of TPDT grafted on MCC surface and formation of chemical bonds were confirmed by Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA) and solid state $^{29}Si$ nuclear magnetic resonance (NMR) spectroscopy. We confirmed increase of grafted amount of TPDT on MCC with increasing reaction time, reaction temperature, and amount of introduced TPDT.

• Polymer(Korea)
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• v.39 no.2
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• pp.329-337
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• 2015

In this study, multi-walled carbon nanotubes (MWCNTs) were oxidized with a mixture of nitric acid and sulfuric acid. After oxidation, oxidized MWCNTs were treated with thionyl chloride ($SOCl_2$) and 1,4-butanediol (BD) in sequence at room temperature to introduce hydroxyl groups on the surface of MWCNTs. The prepared MWCNT-OH was silanized with 3-methacryloxypropyltrimethoxylsilane (MPTMS) to make MWCNT-MPTMS. The MWCNT-MPTMS was used as fillers in emulsion polymerization to make MWCNT-MPTMS/PMMA composite particles with 3 kinds of emulsifiers, hexadecyltrimethylammoniumbromide (CTAB) as a cationic, sodium dodecylbenzene sulfonate (SDBS) as an anionic and polyethylene glycol tert-octylphenyl ether (Triton X-114) as a nonionic emulsifier. Morphologies of composite emulsions were confirmed by a particle size analyzer (PSA) and a scanning electron microscope (SEM). Morphologies of emulsion polymerized MWCNT-MPTMS/PMMA with SDBS showed more uniform particle size distribution compared to those of other two emulsifiers used emulsions. MWCNT-MPTMS/PMMA showed $3.4^{\circ}C$ higher $T_g$ compared to pristine MWCNT/PMMA due to covalent bond formation at interface of MWCNT-MPTMS and PMMA.

• Polymer(Korea)
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• v.24 no.3
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• pp.389-398
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• 2000

Transparent, abrasion resistant coatings with 4~13 ${\mu}{\textrm}{m}$ thickness were prepared by spin-coating on polycarbonates with organic/inorganic hybrid solutions, followed by UV curing and heat treatment at 12$0^{\circ}C$ for 12 hours. The coating solutions were composed of inorganic phase and organic phase in 0:100, 20:80, 30:70, 50:50, 80:20 wt% ratios, respectively, mixed with photoinitiator, senaitizer and surfactant. The inorganic phase was formed by sol-gel reaction of TEOS and silane coupling agent MPTMS in 1 : 2 or 2 : 1 molar ratios, the organic phase consisted of difunctional urethane acrylate oligomeric resin, multifunctional acrylate TMPTA and HDDA in 4 : 3 : 3 wt% ratio. The coating systems were investigated by FT-IR, $^{29}$ Si-NMR spectra. In addition, TGA/DSC for thermal analysis and SEM, AFM observation for coated surface were examined. Gererally, the homogeneity of phases, the surface smoothness of coating and abrasion resistance were improved with the higher content of inorganic component. Namely, coating system with below 10 $\AA$ surface roughness and T$_{g}$ of 15$0^{\circ}C$ showed only 10% decrease in light transmittance after abrasion test, whereas uncoated polycarbonate substrate exhibited 46% decrease..