• Applied Microscopy
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• v.26 no.4
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• pp.447-456
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• 1996

Fracture surfaces of materials contain useful information ranging from crack path to the mechanism of fracture. Since limitation of electron transparency requires a sample in the form of thin foil for TEM observations, it is impossible to extract such information directly from the fracture surfaces. In this study, the method of surface replication from the ceramic fracture surface is employed to characterize the process of crack propagation in ceramic matrix composites using TEM analysis. The surface replica from the fracture surface in ceramic materials provides detailed surface morphology and more importantly, loosened particles on the fracture surface are collected. Electron diffraction and chemical composition analyses of these particles reveal crack path in the specimen. Furthermore, one can determine the mode of fracture by observing the fracture surface morphology from the image of replica. Two examples are given to illustrate the potential of the surface replication technique. In the first example, apparent toughness increase in $B_{4}C-Al$ composites at high strain rate is investigated by surface replication to elucidate the mechanism of fracture at different strain rates. The polytypes of SiC formed during the sintering of SiC-AlN composite and their effect on the fracture behavior of SiC-AlN composite are analyzed in the second example.

• Bulletin of the Korean Chemical Society
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• v.35 no.1
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• pp.189-196
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• 2014

Water dispersible ZnS based nanocrystals: ZnS (blue), ZnS:Cu (green) and ZnS:Mn (yellow-orange) were synthesized by capping the surface of the nanocrystals with a mercaptopropionic acid (MPA) molecule. The MPA capped ZnS based nanocrystal powders were characterized by using XRD, HR-TEM, EDXS, FT-IR, and FT-Raman spectroscopy. The optical properties of the colloidal nanocrystals were also measured by UV/Vis and photoluminescence (PL) spectroscopies in aqueous solvents. The PL spectra showed broad emission peaks at 440 nm (ZnS), 510 nm (ZnS:Cu) and 600 nm (ZnS:Mn), with relative PL efficiencies in the range of 4.38% to 7.20% compared to a reference organic dye. The measured average particle sizes from the HR-TEM images were in the range of 4.5 to 5.0 nm. White light emission was obtained by mixing these three nanocrystals at a molar ratio of 20 (ZnS):1 (ZnS:Cu):2 (ZnS:Mn) in water. The measured color coordinate of the white light was (0.31, 0.34) in the CIE chromaticity diagram, and the color temperature was 5527 K.

• Bulletin of the Korean Chemical Society
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• v.35 no.2
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• pp.431-435
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• 2014

Zinc peroxide nanoparticles ($ZnO_2$ NPs) were prepared by reacting zinc(II) isobutylcarbamate, as an organometallic precursor, with hydrogen peroxide ($H_2O_2$) at $60^{\circ}C$. Polyethylene glycol and polyvinylpyrrolidone were used as stabilizers, which suppressed aggregation of the $ZnO_2$ NPs. Conditions such as concentrations of $H_2O_2$ and the stabilizer were systemically controlled to determine their effect on the formation of nano-sized $ZnO_2$ NPs. The formation of stable $ZnO_2$ NPs was confirmed by UV-vis, Raman spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction. The TEM images revealed that polyvinylpyrrolidone-stabilized $ZnO_2$ NPs (diameter, 10-30 nm) were well dispersed in the organic solvent. Quite pure ZnO NPs were obtained from the peroxide powder by simple heat treatment of $ZnO_2$. The transition temperature of $170^{\circ}C$ was determined by differential scanning calorimetry.

• Current Photovoltaic Research
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• v.1 no.1
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• pp.27-32
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• 2013

We investigated the growth mechanism of amorphous-phase Si thin films in order to improve the film characteristics and circumvent photo-degradation effects by implementation of hot-wire chemical vapor deposition. Amorphous silicon thin films grown in a silane/hydrogen mixture can be decomposed by a resistive heat filament. The structural properties were observed by Raman spectroscopy, FTIR, SEM, and TEM. The electrical properties of the films were measured by photo-conductivity, dark-conductivity, and photo-sensitivity. The contents of Si-H and $Si-H_n$ bonds were measured to be 19.79 and 9.96% respectively, at a hydrogen flow rate of 5.5 sccm, respectively. The thin film has photo-sensitivity of $2.2{\times}10^5$ without a crystalline volume fraction. The catalyst behavior of the hot-wire to decompose the chemical precursors by an electron tunneling effect depends strongly on the hydrogen mixture rate and an amorphous Si thin film is formed from atomic relaxation.

• Bulletin of the Korean Chemical Society
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• v.32 no.3
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• pp.815-820
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• 2011

Three kinds of organometallic compounds (chromium acetylacetonate, magnesium acetate and vanadyl acetylacetonate) were used as transition metal precursor, titanium n-butoxide and multi-walled carbon nanotube as titanium and carbon precursor to prepare metal oxide-CNT/$TiO^2$ composites. The surface properties and morphology of metal oxide-CNT/$TiO^2$ composites were by Brauer-Emett-Teller (BET) surface area measurement, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive X-ray (EDX) analysis. The photocatalytic activity of prepared metal oxide-CNT/$TiO^2$ composites was determined by the degradation effect of methylene blue in an aqueous solution under irradiation of visible light.

• Journal of Hydrogen and New Energy
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• v.16 no.4
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• pp.343-349
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• 2005

In this study, We had surface-treated single-walled carbon nanotubes (SWNTs) for improving hydrogen storage capacity. The SWNTs were treated by heat treatment, acid treatment and fluorinated at various temperatures. The SWNTs were characterized by Raman spectroscopy and TEM and estimated hydrogen storage capacities at 303K. As shown Raman spectra and TEM images, the structure of fluorinated SWNTs were stable at 423K but changed to the MWNTs-like structure or onion structure over 523K. Hydrogen storage capacity of SWNTs fluorinated at 423K was remarkably increased 2.6 times than that of pristine SWNTs. For SWNTs fluorinated at 573K, the amount of hydrogen adsorbed wasn't increased compared with SWNTs fluorinated at 423K. Therefore, high hydrogen storage capacity of SWNTs could be archived by fluorinated condition at 423K, which was not changed SWNT structure.

• Transactions of the Korean Society of Mechanical Engineers A
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• v.31 no.2 s.257
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• pp.205-210
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• 2007

SiC/SiC composites and monolithic SiC materials have been fabricated by the melt infiltration process, through the creation of crystallized SiC phase by the chemical reaction of C and Si. The reinforcing material used in this system was a braided Hi-Nicalon SiC fiber with double interphases of BN and SiC. The microstructures and the mechanical properties of RS-SiC based materials were investigated through means of SEM, TEM, EDS and three point bending test. The matrix morphology of RS-SiS/SiC composites was greatly composed of the SiC phases that the chemical composition of Si and C is different. The TEM analysis showed that the crystallized SiC phases were finely distributed in the matrix region of RS-SiC/SiC composites. RS-SiC/SiC composites also represented a good flexural strength and a high density, accompanying a pseudo failure behavior.

• Bulletin of the Korean Chemical Society
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• v.33 no.12
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• pp.3981-3986
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• 2012

Anatase nanocrystalline and its tungsten-doped (0.4, 2, and 4 mol %) powders have been synthesized by microwave irradiation through hydrolysis of titanium tetra-isopropoxide (TIP) in aqueous solution. The materials are characterized by XRD, Raman, SEM-EDX, TEM, FT-IR and UV-vis techniques. The nanocrystalline $TiO_2$ particles are 30 nm in nature and doping of tungsten ion decreases their size. As seen in TEM images, the crystallites of W (4 mol %) doped $TiO_2$ are small with a size of about 10 nm. The photocatalytic activity was tested on the degradation of 4-nitrophenol (4-NP). Catalytic activities of W-doped and pure $TiO_2$ were also compared. The results show that the photocatalytic activity of the W-doped $TiO_2$ photocatalyst is much higher than that of pure $TiO_2$. Degradation decreases from 96 to 50%, during 115 min, when the initial 4-NP concentration increases from 10 to 120 ppm. Maximum degradation was obtained at 35 mg of photocatalyst.

• Bulletin of the Korean Chemical Society
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• v.30 no.11
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• pp.2637-2642
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• 2009

In this present paper, we prepared $MWCNT/TiO_2$ composites by using pre-oxidized multi-walled carbon nanotubes (MWCNTs) with different titanium alkoxide precursors in benzene solvent. The composites were comprehensively characterized by BET surface area, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX) and UV-Vis absorption spectroscopy. The photoactivity of the prepared materials, under UV irradiation, was tested using methylene blue (MB) in aqueous solution. Finally, according to the results of MB removal experiment, it can be considered that the MB degradation infect mainly caused by photocatalytic effect of $TiO_2$. Furthermore, the bactericidal test of the composites was also determined. It was indicated that $MWCNT/TiO_2$ composites with sunlight had greater effectiveness for B. cereus, S. aureus and E. coli than any other experimental conditions.

• Polymer(Korea)
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• v.27 no.1
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• pp.17-25
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• 2003

Using atom transfer radical polymerization (ATRP), polystyrene macroinitiators and polystyrene-b-poly(t-butyl acrylate) (PS-b-P(tBA) block copolymers were synthesized by CuBr/PMDETA catalyst system in solution. After hydrolysis, polystyrene-b-poly(acrylic acid), amphiphilic block copolymers, were formed. Subsequent neutralization of polyacid block led to the block ionomers. The molecular weight of the synthesized PS-b-P(tBA) block copolymers was easily-controlled to 5000-10000 and their distributions were less than 1.2. The chemical structures of the synthesized block copolymers were characterized by $^1$H-NMR and FT-IR. In the DSC thermograms, $T_g$ appeared in the vicinity of 100 $^{\circ}C$ because of higher styrene content. In addition, the phase separation of the block ionomers was observed by TEM.