• Journal of the Mineralogical Society of Korea
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• v.22 no.3
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• pp.241-248
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• 2009

Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.

• Journal of Korea Foundry Society
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• v.17 no.6
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• pp.560-568
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• 1997

The dissolution behavior of secondary solidification phases in squeeze cast Al-3.9wt%Cu-1.5wt%Si-1.0wt%Mg has been studied using a combination of optical microscope, image analyzer, scanning electron microscope(SEM), energy dispersive spectrometer(EDS), X-ray diffractometer(XRD) and differential thermal analyzer (DTA). Special emphasis was placed on the investigation of the effects of the nonequilibrium heat treatment on the dissolution of the second solidification phases. Ascast microstructure consisted of primary solidification product of ${\alpha}-Al$ and secondary solidification products of $Al_2Cu$, $Mg_2Si$ and $Al_2CuMg$. Equilibrium and non-equilibrium solution treatments were carried out at the temperatures of $495^{\circ}C$, $502^{\circ}C$ and $515^{\circ}C$ for 3 to 5 hours. The amount of the dissolved secondary phases increased with increasing solution treatment temperature, for example, area fractions of $Al_2Cu$, $Mg_2Si$ and $Al_2CuMg$ were approximately 0%, 1.6% and 4.2% after solution treatment at $495^{\circ}C$ for 5hours, and were approximately 0%, 0.36% and 2% after solution treatment at $515^{\circ}C$ for 5hours. The best combination of tensile properties was obtained when the as-cast alloy was solution treated at $515^{\circ}C$ for 3hours followed by aging at $180^{\circ}C$ for 10 hours. Detailed DTA and TEM study showed that the strengthening behavior during aging was due to enhanced precipitation of the platelet type fine ${\theta}'$ phase.

• Korean Journal of Materials Research
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• v.22 no.6
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• pp.298-302
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• 2012

Fe/$SiO_2$ core-shell type composite nanoparticles have been synthesized using a reverse micelle process combined with metal alkoxide hydrolysis and condensation. Nano-sized $SiO_2$ composite particles with a core-shell structure were prepared by arrested precipitation of Fe clusters in reverse micelles, followed by hydrolysis and condensation of organometallic precursors in micro-emulsion matrices. Microstructural and chemical analyses of Fe/$SiO_2$ core-shell type composite nanoparticles were carried out by TEM and EDS. The size of the particles and the thickness of the coating could be controlled by manipulating the relative rates of the hydrolysis and condensation reaction of TEOS within the micro-emulsion. The water/surfactant molar ratio influenced the Fe particle distribution of the core-shell composite particles, and the distribution of Fe particles was broadened as R increased. The particle size of Fe increased linearly with increasing $FeNO_3$ solution concentration. The average size of the cluster was found to depend on the micelle size, the nature of the solvent, and the concentration of the reagent. The average size of synthesized Fe/$SiO_2$ core-shell type composite nanoparticles was in a range of 10-30 nm and Fe particles were 1.5-7 nm in size. The effects of synthesis parameters, such as the molar ratio of water to TEOS and the molar ratio of water to surfactant, are discussed.

• Journal of the Korean Ceramic Society
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• v.53 no.1
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• pp.110-115
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• 2016

We prepared a working electrode (WE) coated with 0 ~ 50 nm-thick indium gallium zinc oxide(IGZO) by using RF sputtering to improve the energy conversion efficiency (ECE) of a dye sensitized solar cell (DSSC). Transmission electron microscope (TEM) and energy dispersive spectroscopy (EDS) were used to analyze the microstructure and composition of the IGZO layer. UV-VIS-NIR spectroscopy was used to determine the transparency of the WE with IGZO layers. A solar simulator and a potentiostat were used to confirm the photovoltaic properties of the DSSC with IGZO layer. From the results of the microstructural analysis, we were able to confirm the successful deposition of an amorphous IGZO layer with the expected thickness and composition. From the UV-VIS-NIR analysis, we were able to verify that the transparency decreased when the thickness of IGZO increased, while the transparency was over 90% for all thicknesses. The photovoltaic results show that the ECE became 4.30% with the IGZO layer compared to 3.93% without the IGZO layer. As the results show that electron mobility increased when an IGZO layer was coated on the $TiO_2$ layer, it is confirmed that the ECE of a DSSC can be enhanced by employing an appropriate thickness of IGZO on the $TiO_2$ layer.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.46 no.4
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• pp.28-36
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• 2014

We studied the green synthesis and antibacterial activity of paper coated with chitosan-silver (Ag) green nanocomposites for packaging applications. Green synthesis of Ag nanoparticles (AgNPs) was achieved by a chemical reaction involving a mixture of chitosan-silver nitrate ($AgNO_3$) in an autoclave at 15 psi, $121^{\circ}C$, for 30 min. AgNPs and their formation in chitosan was confirmed by UV-Vis spectroscopy, transmission electron microscopy (TEM) and dynamic light scattering (DLS). As-prepared chitosan-AgNPs composite materials were coated on manila paper using Meyer rod. Surface morphology and Ag contents in coating layer were characterized by field emission scanning electron microscopy (FESEM) and energy dispersive spectroscopy (EDS). The mechanical properties such as tensile strength and elongation were significantly affected by coating with chitosan-AgNPs. The antibacterial test of coated paper was performed qualitatively and quantitatively against Escherichia coli (E. coli). It was shown to be effective in suppressing the growth of E. coli with increasing Ag contents on the surface of coated paper and more than 95 R (%) of antimicrobial rate was obtained at chitosan-AgNPs coated papers.

• Journal of Sensor Science and Technology
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• v.23 no.6
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• pp.397-401
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• 2014

This paper describes the fabrication and characteristics of $C_2H_2$ gas sensor based on Ag-doped hierarchical ZnO nanostructures. In this work, a pure hierarchical ZnO structure was prepared using a simple hydrothermal method, and Ag nanoparticles doped the hierarchical ZnO structure were uniformly synthesized through photochemical route. The synthesized samples were characterized by SEM, TEM, EDS, XRD and PL spectra. Average size of prepared ZnO structures was around $2{\sim}3{\mu}m$ and showed highly uniform. The average size of Ag nanoparticles was 70 nm. The gas sensing properties of as-prepared products were investigated using resistivity-type gas sensors. 5 at% Ag-doped ZnO based sensors exhibited good performances for $C_2H_2$ gas in comparison with the un-doped one. The sensor based on Ag-doped hierarchical ZnO structures had linear response property from 5~1000 ppm of $C_2H_2$ concentration at working temperature of $200^{\circ}C$. The response values with 100 ppm $C_2H_2$ at $200^{\circ}C$ were 10% and 75% for pure and 5 at% Ag-doped hierarchical ZnO nanostructures, respectively. Moreover, the device showed excellent selectivity towards to $C_2H_2$ gas at optimal working temperature of $200^{\circ}C$.

• Proceedings of the Korean Vacuum Society Conference
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• 2015.08a
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• pp.91-91
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• 2015

반도체 공정의 발전에 의해 최근 생산되는 메모리 등은 십 수 나노미터까지 좁아진 선 폭을 갖게 되었다. 이러한 이유로, 기존에는 큰 문제를 발생시키지 않던 나노미터 영역의 입자들이 박막 증착 공정과 같은 반도체 제조공정 수율을 저감시키게 되었다. 따라서 오염입자의 유입을 막거나 제어하기 위해 transmission electron microscopy (TEM)나 scanning electron microscopy (SEM)과 같은 전자현미경을 활용한 비 실시간 입자 측정 방법 및 광원을 이용하는 in-situ particle monitor (ISPM) 및 전기적 이동도를 이용한 scanning mobility particle sizer (SMPS) 등 다양한 원리를 이용한 실시간 입자 측정방법이 현재 사용중에 있다. 이 중 진공 내 입자의 수농도를 측정하기 위해 개발된 particle beam mass spectrometer (PBMS) 기술은 박막 증착 공정 등 chemical vapor deposition (CVD) 방법을 이용하는 진공공정에서 활용 가능하여 개발이 진행되어 왔다. 본 연구에서는 PBMS의 한계점인 입자 밀도, 형상 등의 특성분석이 용이하도록 PBMS와 scanning electron microscopy (SEM), 그리고 energy dispersive spectroscopy (EDS) 기술을 결합하여 입자의 직경별 개수농도, 각 입자의 형상 및 성분을 함께 측정 가능하도록 하였다. 협소한 반도체 제조공정 내부 공간에 적용 가능하도록 기존 PBMS 대비 크기 또한 소형화 하였다. 각 구성요소인 공기역학 집속렌즈, electron gun, 편향판, 그리고 패러데이 컵의 설치 및 물리적인 교정을 진행한 후 입자발생장치를 통해 발생시킨 sodium chloride 입자를 상압 입자 측정 및 분류장치인 SMPS 장치를 이용하여 크기별로 분류시켜 압력차를 통해 PBMS로 유입시켜 측정을 진행하였다. 나노입자의 입경분포, 형상 및 성분을 측정결과를 토대로 장치의 측정정확도를 교정하였다. 교정된 장치를 이용하여 실제 박막 증착공정 챔버의 배기라인에서 발생하는 입자의 수농도, 형상 및 성분의 복합특성 측정이 가능하였으며, 최종적으로 실제 공정에 적용가능하도록 장치 교정을 완료하였다.

• Journal of Soil and Groundwater Environment
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• v.25 no.1
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• pp.95-105
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• 2020

In this study, iron nanoparticles impregnated hydrochar (FeNPs@HC) was synthesized using lignocellulosic waste and simple one-pot synthetic method. During hydrothermal carbonization (HTC) process, the mixture of lignocellulosic waste and ferric nitrate (0.1~0.5 M) as a precursor of iron nanoparticles was added and heated to 220℃ for 3 h in a teflon sealed autoclave, followed by calcination at 600℃ in N₂ atmosphere for 1 h. For the characterization of the as-prepared materials, X-ray diffraction (XRD), cation exchange capacity (CEC), fourier transform infrared spectrometer (FT-IR), Brunauer-Emmett-Teller (BET), transmission electron microscope (TEM), Energy Dispersive X-ray Spectroscopy (EDS) were used. The change of Fe(III) concentration in the feedstock influenced characteristics of produced FeNPs@HC and removal efficiency towards As(V) and Pb(II). According to the Langmuir isotherm test, maximum As(V) and Pb(II) adsorption capacity of Fe_0.25NPs@HC were found to be 11.81 and 116.28 mg/g respectively. The results of this study suggest that FeNPs@HC can be potentially used as an adsorbent or soil amendment for remediation of groundwater or soil contaminated with arsenic and cation heavy metals.

• Journal of the Korean Vacuum Society
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• v.10 no.1
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• pp.87-92
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• 2001

Magnetic Fe-Co(C) nanocapsules and Fe-Co nanoparticles were prepared by arc-discharge in two kinds of atmospheres, i.e. methane and a mixture of ($H_2$+Ar), respectively. Characterization and magnetic properties of this two kinds of ultrafine particles were investigated systematically by means of X-ray diffraction, Mssbauer spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy, energy disperse spectroscopy analysis, chemical analysis, oxygen determination and magnetization measurement. Effects of carbon element, decomposed from a methane atmosphere in carbon arc process, on phase structures, magnetic states and surface characterization were studied in comparison to that of Ar element. Two ultrafine particles showed a little difference in the weight ratio of (Fe/co) and the size for Fe-Co nanoparticles was about two times bigger than Fe-Co(C) nanocapsules. The saturation magnetization of Fe-Co (C) nanocapsules was about 8% higher than that of Fe-Co nanoparticles while their phase constitutions were similar. Although no carbon could be detected by XRD measurement because of extremely thin shells on the surfaces of the cores, it is still believed that they are carbon and oxygen layers.

• Journal of the Mineralogical Society of Korea
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• v.15 no.1
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• pp.78-84
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• 2002

New pyrochlore-type phases($A_2$$B_2$$O_{7}$) were synthesized in the systems: CaO-C$eO_2$-T$iO_2$, CaO-$UO_2$(T$hO_2$)-Z$rO_2$, CaO-$UO_2$(T$hO_2$)-$Gd_2$$O_3$-T$iO_2$-Z$rO_2$, 및 CaO-T$hO_2$-S$nO_2$. The starting materials were pressed with the pressure of 200~400 MPa and sintered at 1500~ 155$0^{\circ}C$ for 4~8 hours in air and at 1300~ 135$0^{\circ}C$ for 5 ~50 hours under oxygen atmosphere. The products were characterized using XRD, SEM/EDS and TEM. In the bulk compositions of CaCe$Ti_2$$O_{7}$, CaTh$Zr_2$$O_{7}$,($Ca_{0.5}$ Gd$Th_{0.5}$)(ZrTi)$O_{7}$) ($Ca_{0.5}$Gd$Th_{0.5}$)(ZrTi)$O_{7}$, ($Ca_{0.5}$G$dU_{0.5}$)(ZrTi)$O_{7}$ and CaTh$Sn_2$$O_{7}$ , pyrochlore was the major phase, together with other oxide phase $of_2$$O_{7}$ fluorite structure. In the samples with target compositions CaU$Zr_2$$O_2$및 $Ca_{0.5}$ G$dU_{0.5}$)$Zr_2$T$iO_{7}$ pyrochlore was not identified, but a fluorite-structured phase was detected. The formation factor as the stable phase depended on crystal chemical characteristics of the actinide and lanthanide elements of the system concerned.