• Title/Summary/Keyword: FE-TEM

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Electron Energy Loss Spectroscopy (EELS) Application to Mineral Formation (전자에너지 손실분광 분석법을 이용한 광물에서의 정량적 철 산화수 측정과 분석)

  • Yang, Kiho;Kim, Jinwook
    • Journal of the Mineralogical Society of Korea
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    • v.29 no.2
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    • pp.73-78
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    • 2016
  • The oxidation states of structural Fe in clay minerals often reflect the paleo-redox conditions of the depositional environments. It is inevitable to utilize the high resolution of transmission electron microscopy (TEM) to investigate the mechanism of mineral transformation at nano-scale. The applications of TEM- electron energy loss spectroscopy (EELS) for quantification of $Fe(III)/{\Sigma}Fe$ from the K-nontronite formation associated with structural Fe(III) reduction in nontronite under deep subseafloor environment were demonstrated. In particular, quantification of the changes in Fe-oxidation state at nanoscale is essential to understand the mechanisms of minerals formation. The procedure of EELS acquisition, quantitative determination of Fe-oxidation states, and advantages of EELS techniques were discussed.

A Study of Methane Partial Oxidation Characteristics on CuFe2O4 (CuFe2O4을 이용한 메탄부분산화 특성 연구)

  • Woo, Sung Woung;Kang, Yong;Kang, Kyoung Soo;Kim, Chang Hee;Kim, Chul Sung;Park, Chu Sik
    • Korean Chemical Engineering Research
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    • v.46 no.6
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    • pp.1113-1118
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    • 2008
  • Characteristics of reduction properties and carbon deposition of $CuFe_2O_4$ and $Fe_3O_4$ were investigated by using TGA, XRD, SEM, TEM and gas analysis at $900^{\circ}C$. XRD analyses indicated that the reduced $Fe_3O_4$ was composed of Fe, graphite and $Fe_3C$ phases. In contrast, the reduced $CuFe_2O_4$ did not show the graphite or $Fe_3C$ phases. It was observed by SEM analysis that the surface of the $Fe_3O_4$ was completely covered with carbon, after methane partial oxidation. From gas analysis, $CuFe_2O_4$ showed much higher methane conversion and reduction kinetics as compared to the $Fe_3O_4$ under the same reaction conditions and the estimated carbon deposition amounts on the reduced $CuFe_2O_4$ was much lower than those on the reduced $Fe_3O_4$ during the syngas production process. It was found by TEM that carbon on the reduced $Fe_3O_4$ particles has a platelet shape.

Structural Characterization of CoCrFeMnNi High Entropy Alloy Oxynitride Thin Film Grown by Sputtering (스퍼터링 방법으로 성장한 코발트크롬철망간니켈 고엔트로피 질산화물 박막의 구조특성)

  • Lee, Jeongkuk;Hong, Soon-Ku
    • Korean Journal of Materials Research
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    • v.28 no.10
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    • pp.595-600
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    • 2018
  • This study investigates the microstructural properties of CoCrFeMnNi high entropy alloy (HEA) oxynitride thin film. The HEA oxynitride thin film is grown by the magnetron sputtering method using nitrogen and oxygen gases. The grown CoCrFeMnNi HEA film shows a microstructure with nanocrystalline regions of 5~20 nm in the amorphous region, which is confirmed by high-resolution transmission electron microscopy (HR-TEM). From the TEM electron diffraction pattern analysis crystal structure is determined to be a face centered cubic (FCC) structure with a lattice constant of 0.491 nm, which is larger than that of CoCrFeMnNi HEA. The HEA oxynitride film shows a single phase in which constituting elements are distributed homogeneously as confirmed by element mapping using a Cs-corrected scanning TEM (STEM). Mechanical properties of the CoCrFeMnNi HEA oxynitride thin film are addressed by a nano indentation method, and a hardness of 8.13 GPa and a Young's modulus of 157.3 GPa are obtained. The observed high hardness value is thought to be the result of hardening due to the nanocrystalline microstructure.

Effect of Preparation Method for Pd/C Catalysts on Pd Characterization and their Catalytic Activity (Pd/C 촉매 제조 방법에 따른 Pd 금속의 특성 및 촉매 활성)

  • Kim, Ji Sun;Hong, Seong-Soo;Kim, Jong-Hwa;Lee, Man Sig
    • Applied Chemistry for Engineering
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    • v.26 no.5
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    • pp.575-580
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    • 2015
  • Pd/C catalysts were prepared by various preparation methods such as ion exchange, impregnation and polyol method and also characterized by nitrogen adsorption-desorption isothermal, XRD, FE-TEM and CO-chemisorption. The activities of these catalysts were tested in the hydrogenation of cyclohexene to cyclohexane. Catalytic activities of Pd/C catalysts were found to be effected by the chosen preparation methods. Pd dispersions of each Pd/C catalysts prepared by ion exchange, impregnation and polyol method were 17.55, 13.82% and 1.35%, respectively, confirmed by CO-chemisorption analysis. These were also in good agreement with the FE-TEM results. The Pd/C catalyst prepared by ion exchange method exhibits good performance with the cyclohexene conversion rate of 71% for 15 min. These results indicate that Pd/C catalyst having higher dispersion and lower particle size is in favor of hydrogenation cyclohexene and also Pd dispersion increases with the increment of catalytic activity.

Effect of Ag on microstructural behaviour of Nanocrystalline $Fe_{87-x}Zr_7B_6Ag_x$($0{\leq}x_{Ag}{\leq}4$) Magnetic Thin Films Materials

  • Lee, W.J.;Min, B.K.;Song, J.S.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.04a
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    • pp.3-6
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    • 2002
  • Effect of Ag additive element on microstructure of $Fe_{87-x}Zr_7B_6Ag_x$, magnetic thin films on Si(001) substrates has been investigated using Transmission Electron Microscopy(TEM) and X-ray Diffraction(XRD). All samples with additive Ag element were made by DC-sputtering and subjected to annealing treatments of $300^{\circ}C{\siim}600^{\circ}C$ for 1 hr. TEM and XRD showed that perfectly amorphous state in Ag-free Fe-based films was observed in as-deposited condition. The as-deposited Fe-based films with the presence of Ag constituent have a mixture of Fe-based amorphous and nano-sized Ag crystalline phases. In this case, additive element, Ag was soluted into Fe-based matrix. With the increase in additive element, Ag, insoluble nano-crystalline Ag particles were dispersed in the Fe-based amorphous matrix. Crystallization of Fe-based amorphous phase in the matrix of $Fe_{82}Zr_7B_6Ag_5$ thin films occurred at an annealing temperature of $400^{\circ}C$. Upon annealing, the amorphous-Ag crystalline state of Fe-Zr-B-Ag films was transformed into the mixture of Ag crystalline phase + Fe-based amorphous phase + ${\alpha}$-Fe cluster followed by the crystallization process of ${\alpha}$-Fe nanocrystalline + Ag crystalline phases.

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Studying Carbon Coating on the Surface of Nano-sized Fe Particle by Mössbauer Analysis (뫼스바우어 분광법에 의한 Fe-나노입자의 탄화물 코팅에 관한 연구)

  • Oh, Sei-Jin;Choi, Chul-Jin;Kim, Jin-Chun;Kwon, Soon-Ju;Jin, Sang-Ho
    • Journal of the Korean Magnetics Society
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    • v.15 no.3
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    • pp.172-176
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    • 2005
  • Four nano-sized Fe-nano particle samples synthesized by Chemical Vapor Condensation (CVC) were analyzed using $M\ddot{o}ssbauer$ spectroscopy, XRD, BET and TEM. The samples were consisted as functions of carrier gas and decomposition temperature. The synthesized nanoparticles consisted of two- or three-layers with the circular shape. The average particle size was increased with increasing the decomposition temperature. At $500^{\circ}C$ for the decomposition temperature, $Fe_3C$ was formed more under the environment of CO carrier gas than that of $CH_4$. However, at $1,100^{\circ}C$, almost of Fe-nano particles were transformed into $Fe_3C$ with using both carrier gas.

Formation Fe2O3 Nanowalls through Solvent-Assisted Hydrothermal Process and Their Application for Titan Yellow GR Dye Degradation

  • Ahmed, Khalid Abdelazez Mohamed
    • Journal of the Korean Chemical Society
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    • v.58 no.2
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    • pp.205-209
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    • 2014
  • Hematite iron oxide (${\alpha}$-$Fe_2O_3$) nanowalls were fabricated on aluminum substrate by a facile solvent-assisted hydrothermal oxidation process. The XRD and EDS patterns indicate that the sample has a rhombohedral phase of hematite $Fe_2O_3$. FE-SEM, TEM, HR-TEM, SA-ED were employed to characterize the resulting materials. $N_2$ adsorption-desorption isotherms was used to study a BET surface area. Their capability of catalytic degradation of titan yellow GR azo dye with air oxygen in aqueous solution over $Fe_2O_3$ catalysts was studied. The result indicates that the as-prepared product has a high catalytic activity, because it has a larger surface area. Langmuir and Freundlich isotherms of adsorption dye on the catalysts surface were investigated and the decomposition of titan yellow GR follows pseudo-first order kinetic.

Preparation and Characterization of Pt-Fe/Carbon Black Nanocatalyst for Anion Exchange Membrane in Alkaline Electrolysis (음이온 교환막 수전해용 Pt-Fe/카본블랙 나노 촉매 제조 및 특성)

  • SUNGKOOK CHO;JAEYOUNG LEE;HONGKI LEE
    • Journal of Hydrogen and New Energy
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    • v.33 no.6
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    • pp.715-722
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    • 2022
  • Pt-Fe/carbon black nanocatalysts were prepared by spontaneous reduction reaction of Platinum(II) acetylacetonate and Iron(II) acetylacetonate in a nucleophilic solvent and they were characterized by scanning electron microscopy (SEM), energy dispersive X-ray analyzer (EDS), thermogravimetric analyzer (TGA), transmission electron microscopy (TEM), Brunauer, Emmett and Teller (BET) surface area analysis and anion exchange membrane (AEM) water electrolysis test station. The distribution of the Pt and Fe nanoparticles on carbon black was observed by TEM, and the loading weight of Pt-Fe nanocatalysts on the carbon black was measured by TGA. Elemental ratio of Fe:Pt was estimated by EDS and it was found that elemental ratio of Pt and Fe was changed in the range of 1:0 to 0:1, and the loading weight of Pt-Fe nanoparticles on the carbon black was 5.95-6.78 wt%. Specific surface area was greatly reduced because Pt-Fe nanocatalysts blocked the pores. I-V characteristics were estimated.

Mechanical Properties of ODS Fe Alloys Produced by Mechano-Chemical Cryogenic Milling (극저온 기계화학적 밀링(Mechano-Chemical Milling)에 의해 제조된 ODS Fe 합금의 기계적 특성)

  • Hahn, Sung-In;Hong, Young-Hwan;Hwang, Seung-Joon
    • Journal of the Korean Society for Heat Treatment
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    • v.25 no.3
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    • pp.138-145
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    • 2012
  • An ${\alpha}$-Ferrite (Fe) powder dispersed with 4 vol.% of $Al_2O_3$ was successfully produced by a simple miling at 210 K with a mixture of $Fe_2O_3$, Fe and Al ingredient powders, followed by 2 step high temperature consolidation: Hot Pressing (HP) at 1323 K and then Hot Isostatic Pressing at 1423 K. The microstructure of the consolidated material was characterized by standard metallographic techniques such as XRD (X-ray Diffraction), TEM and STEM-EDS. The results of STEM-EDS analysis showed that the HIPed materials comprised a mixture of pure Fe matrix with a grain size of ~20 nm and $Al_2O_3$ with a bimodal size distribution of extremely fine (~5 nm) and medium size dispersoids (~20 nm). The mechanical properties of the consolidated materials were characterized by compressive test and micro Vickers hardness test at room temperature. The results showed that the yield strength of the ODS (Oxide Dispersion Strengthened) Fe alloy are as much as $674{\pm}39$ MPa and the improvement of the yield strength is attributed to the presence of the fine $Al_2O_3$ dispersoid.