• Title/Summary/Keyword: Microanalysis

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Integrated Microdisk Gold Electrode Modified with Metal-porphyrin and Metal-phthalocyanines for Nitric Oxide Determination in Biological Media

  • Kim, Il-Kwang;Bae, Hyun-Ok;Oh, Gi-Soo;Chung, Hun-Taeg;Kim, Young-Jin;Chun, Hyun-Ja
    • Bulletin of the Korean Chemical Society
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    • v.24 no.11
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    • pp.1579-1584
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    • 2003
  • An integrated gold microdisk electrode was constructed and modified with metal-porphyrin or metal-phthalocyanines for NO determination in biological media. Microanalysis of NO using square wave anodic stripping voltammetry in $1\;{\times}\;10^{-2}$ M $HClO_4$ was optimal when the accumulation potential was 0.1 V, frequency 100 Hz, and the scan rate was 200 mV/s. When the electrode was modified with metal-porphyrin or metal-phthalocyanines, the anodic peak currents of NO increased due to the catalytic oxidation of NO. In case of Fe(II)-phthalocyanine modified electrode, the peak currents remarkably increased and the sensitivity was high. The calibration curve had good linearity in the range from $3.6\;{\times}\;10^{-5}$ M to $7.2\;{\times}\;10^{-7}$ M, and the detection limit was $5.7\;{\times}\;10^{-7}$ M. For the structural stability and increased sensitivity, Fe(II)-phthalocyanine modified gold microdisk electrode coated with Nafion was applied to determination of NO released from cultured macrophase.

COMPARATIVE ANALYSIS OF STRUCTURAL CHANGES IN U-MO DISPERSED FUEL OF FULL-SIZE FUEL ELEMENTS AND MINI-RODS IRRADIATED IN THE MIR REACTOR

  • Izhutov, Aleksey.L.;Iakovlev, Valeriy.V.;Novoselov, Andrey.E.;Starkov, Vladimir.A.;Sheldyakov, Aleksey.A.;Shishin, Valeriy.Yu.;Kosenkov, Vladimir.M.;Vatulin, Aleksandr.V.;Dobrikova, Irina.V.;Suprun, Vladimir.B.;Kulakov, Gennadiy.V.
    • Nuclear Engineering and Technology
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    • v.45 no.7
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    • pp.859-870
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    • 2013
  • The paper summarizes the irradiation test and post-irradiation examination (PIE) data for the U-Mo low-enriched fuel that was irradiated in the MIR reactor under the RERTR Program. The PIE data were analyzed for both full-size fuel rods and mini-rods with atomized powder dispersed in Al matrix as well as with additions of 2%, 5% and 13% of silicon in the matrix and ZrN protective coating on the fuel particles. The full-size fuel rods were irradiated up to an average burnup of ${\sim}60%^{235}U$; the mini-rods were irradiated to an average burnup of ${\sim}85%^{235}U$. The presented data show a significant increase of the void fraction in the U-Mo alloy as the U-235 burnup rises from ~ 40% up to ~ 85%. The effect of irradiation test conditions and U-235 burnup were analyzed with regard to the formation of an interaction layer between the matrix and fuel particles as well as generation of porosity in the U-Mo alloy. Shown here are changes in distribution of U fission products as the U-235 burnup increases from ~ 40% up to ~ 85%.

On-Site Corrosion Behavior of Water-Treated Boiler Tube Steel

  • Seo, Junghwa;Choi, Mihwa;He, Yinsheng;Yang, Seok-Ran;Lee, Je-Hyun;Shin, Keesam
    • Applied Microscopy
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    • v.45 no.3
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    • pp.177-182
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    • 2015
  • The boiler tubes of X20CrMoV12.1 used in fossil-fired power plants were obtained and analyzed for the effect of water treatment on the steam corrosion-induced oxide scale in an effort to better understand the oxide formation mechanism, as well as pertinent method of maintenance and lifetime extension. The specimens were analyzed using various microscopy and microanalysis techniques, with focuses on the effect of water treatment on the characters of scale. X-ray diffraction analysis showed that the scales of specimens were composed of hematite ($Fe_2O_3$), magnetite ($Fe_3O_4$), and chromite ($FeCr_2O_4$). Electron backscatter diffraction analysis showed that the oxides were present in the following order on the matrix: outer $Fe_2O_3$, intermediate $Fe_3O_4$, and inner $FeCr_2O_4$. After all volatile treatment or oxygenated treatment, a dense protective $Fe_2O_3$ layer was formed on the $Fe_3O_4$ layer of the specimen, retarding further progression of corrosion.

Growth and Characterization of Vertically well Aligned Crbon Nanotubes on Glass Substrate by Plasma Enhanced Hot Filament Chemical Vapor deposition

  • Park, Chong-Yun;Yoo, Ji-Beom
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.210-210
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    • 2000
  • Vertically well aligned multi-wall carbon nanotubes (CNT) were grown on nickel coated glass substrates by plasma enhanced hot filament chemical vapor deposition at low temperatures below 600$^{\circ}C$. Acetylene and ammonia gas were used as the carbon source and a catalyst. Effects of growth parameters such as pre-treatment of substrate, plasma intensity, filament current, imput gas flow rate, gas composition, substrate temperature and different substrates on the growth characteristics of CNT were systematically investigated. Figure 1 shows SEM image of CNT grown on Ni coated glass substrate. Diameter of nanotube was 30 to 100nm depending on the growth condition. The diameter of CNT decreased and density of CNT increased as NH3 etching time etching time increased. Plasma intensity was found to be the most critical parameter to determine the growth of CNT. CNT was not grown at the plasma intensity lower than 500V. Growth of CNT without filament current was observed. Raman spectroscopy showed the C-C tangential stretching mode at 1592 cm1 as well as D line at 1366 cm-1. From the microanalysis using HRTEM, nickel cap was observed on the top of the grown CNT and very thin carbon amorphous layer of 5nm was found on the nickel cap. Current-voltage characteristics using STM showed about 34nA of current at the applied voltage of 1 volt. Electron emission from the vertically well aligned CNT was obtained using phosphor anode with onset electric field of 1.5C/um.

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A way Analyzing Oxide Layer on an Irradiated CANDU-PHWR Pressure Tube Using an EPMA and X-ray Image Mapping

  • Jung, Yang Hong;Kim, Hee Moon
    • Corrosion Science and Technology
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    • v.20 no.3
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    • pp.118-128
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    • 2021
  • The oxide layer in samples taken from an irradiated Zr-2.5Nb pressure tube from a CANDU-PHWR reactor was analyzed using electron probe microanalysis (EPMA). The examined tube had been exposed to temperatures ranging from 264 to 306 ℃ and a neutron fluence of 8.9 × 1021 n/cm2 (E > 1 MeV) for the maximum 10 effective full-power years in a nuclear power plant. Measuring oxide layer thickness generally employs optical microscopy. However, in this study, analysis of the oxide layer from the irradiated pressure tube components was undertaken through X-ray image mapping obtained using EPMA. The oxide layer characteristics were analyzed by X-ray image mapping with 256 × 256 pixels using EPMA. In addition, the slope of the oxide layer was measured for each location. A particular advantage of this study was that backscattered electrons and X-ray image mapping were obtained at a magnification of 9,000 when 20 kV volts and 30 uA of current were applied to radiation-shielded EPMA. The results of this study should usefully contribute to the study of the oxide layer properties of various types of metallic materials irradiated by high radiation in nuclear power plants.

Influence of Sn/Bi doping on the phase change characteristics of $Ge_2Sb_2Te_5$

  • Park T.J.;Kang M.J.;Choi S.Y.
    • Transactions of the Society of Information Storage Systems
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    • v.1 no.1
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    • pp.93-98
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    • 2005
  • Rewritable optical disk is one of the essential data storage media in these days, which takes advantage of the different optical properties in the amorphous and crystalline states of phase change materials. As well known, data transfer rate is one of the most important parameter of the phase change optical disks, which is mostly limited by the crystallization speed of recording media. Therefore, we doped Sn/Bi to $Ge_2Sb_2Te_5$ alloy in order to improve the crystallization speed and investigated the dependence of phase change characteristics on Sn/Bi doping concentration. The Sn/Bi doped $Ge_2Sb_2Te_5$ thin film was deposited by RF magnetron co-sputtering system and phase change characteristics were investigated by X-ray diffraction (XRD), static tester, UV-visible spectrophotometer, electron probe microanalysis (EPMA), inductively coupled plasma mass spectrometer (ICP-MS) and atomic force microscopy (AFM). Optimum doping concentration of Bi and Sn were 5${\~}$6 at.$\%$ and the minimum time for crystallization was below than 20 ns. This improvement is correlated with the simple crystalline structure of Sn/Bi doped $Ge_2Sb_2Te_5$ and the reduced activation barrier arising from Sn/Bi doping. The results indicate that Sn/Bi might play an important role in the transformation kinetics of phase change materials..

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Microstructural Properties of the Insoluble Residue in a Simulated Spent Fuel

  • Kim, J.S.;Song, B.C.;Jee, K.Y.;Kim, J.G.;Chun, K.S.
    • Nuclear Engineering and Technology
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    • v.30 no.2
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    • pp.99-111
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    • 1998
  • Chemical composition of the insoluble residue in a simulated spent PWR fuel(SIMRJEL) were studied. SIMFUELS were prepared by adding calculated amount of FP(fission product) elements with a burnup of 3.6% FIMA(fission per initial metal atom) to uranium in nitrate solution, evaporating the mixed solution to dryness, calcining at 90$0^{\circ}C$ in a stream of 4% H$_2$ + 96% He, and heating the pellet at 140$0^{\circ}C$ under high and low oxygen potentials. Insoluble residue was obtained from the dissolution of the SIMFUEL with HNO$_3$(1 : 1). The chemical composition of the SIMFUELs and the insoluble residues was determined by EPMA(electron probe microanalysis), XPS(X-ray photoelectron spectroscopy) and by XRD (X-ray diffraction) measurements. All of the insoluble residues suspended and precipitated were composed mainly of Mo, Ru with a small amount of Zr, Rh, Pd and Cd. The amount of insoluble residue(<1 wt.%) and a Mo/Ru ratio decreased with increasing oxygen potential. Formation of the zirconium molybdate precipitate, ZrMo$_2$O$_{7}$(OH)$_2$($H_2O$)$_2$, was observed in the residues. The possible role of Mo on the phase formation was discussed in regard to oxygen potential.l.

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Numerical investigation into particle crushing effects on the shear behavior of gravel

  • Xi Li;Yayan Liu;Guoping Qian;Xueqing Liu;Hao Wang;Guoqing Yin
    • Geomechanics and Engineering
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    • v.35 no.2
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    • pp.209-219
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    • 2023
  • This paper presents numerical investigations into the particle crushing effect on the shear properties of gravel under direct shear condition. A novel particle crushing model was developed based on the octahedral shear stress criterion and fragment replacement method. A series of direct shear tests were carried out on unbreakable particles and breakable particles with different strengths. The evolutions of the particle crushing, shear strength, volumetric strain behavior, and contact force fabric during shearing were analyzed. It was observed that the number of crushed particles increased with the increase of the shear displacement and axial pressure and decreased with the particle strength increasing. Moreover, the shear strength and volume dilatancy were obviously decreased with particle crushing. The shear displacement of particles starting to crush was close to that corresponding to the peak shear stress got. Besides, the shear-hardening behavior was obviously affected by the number of crushed particles. A microanalysis showed that due to particle crushing, the contact forces and anisotropy decreased. The mechanism of the particle crushing effect on the shear strength was further clarified in terms of the particle friction and interlock.

Genesis of the Lead-Zinc-Silver and Iron Deposits of the Janggun Mine, as Related to Their Structural Features Structural Control and Wall Rock Alteration of Ore-Formation (장군광산(將軍鑛山)의 연(鉛)·아연(亞鉛)·은(銀) 및 철(鐵) 광상(鑛床)의 성인(成因)과 지질구조(地質構造)와의 관계(關係) - 광상(鑛床) 생성(生成)의 지질구조(地質構造) 규제(規制)와 모암(母岩)의 변질(變質) -)

  • Lee, Hyun Koo;Ko, Suck Jin;Naoya, Imai
    • Economic and Environmental Geology
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    • v.23 no.2
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    • pp.161-181
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    • 1990
  • The lead-zinc-silver-iron deposits from the Janggun mine are of hydrothermal-metasomatic origin, characterized by the marked hydrothermal alteration of the wallrocks, such as hydrothermal manganese enrichment of carbonate rocks, silicification, chloritization, sericitization, montmorillonitization and argillic alteration. The ore deposits have been emplaced within the Janggun Limestone of Cambro-Ordovician age at the immediate contacts with apophyses injected from the Chunyang Granite plutons of Late Jurrasic age. They have been structurally controlled by fractures in the carbonate rocks and the irregular intrusive contacts of granitic rocks, and are closely associated with hypogene manganese carbonate deposits. In the mine nine seperate orebodies are being mined. On the basis of the petrological study, hydrothermal alteration zone of this mine may be divided into the following four zones from wallrock to orebody. (I) Primary calcite and dolomite zone${\rightarrow}$(II) dolomitic limestone zone${\rightarrow}$(III) dolomitic zone${\rightarrow}$(IV) rhodochrosite zone${\rightarrow}$ orebody. There was not recongnized Mn and Fe elements in the primary calcite and dolomite zone. But, in the dolomitic limestone and dolomite zone, calcite and dolomite were subjected to weak hydrothermal manganese enrichment and the grade of the manganese enrichment increase oreward. By means of electron probe microanalysis, it was found that manganoan dolomite occured between primary dolomite grains, cross the cleavage of the primary dolomite and around the dolomite grains. Above these result supports that the Janggun manganese carbonate deposits are of hydrothermal metasomatic origin.

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A Study on the Muscovite-Pyrophyllite Mixed Phase in the Shale from the Manhang Formation, Taebaek Area (태백지역 만항층 셰일에서 산출되는 백운모-파이로필라이트 혼합상에 대한 연구)

  • Choi, Seung-Hyun;Mun, Hyang-Ran;Lee, Young-Boo;Lee, Jung-Hoo
    • Journal of the Mineralogical Society of Korea
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    • v.24 no.4
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    • pp.313-320
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    • 2011
  • Mica-type phyllosilicate particles in the shales of the Manhang formation at the Taeback area in the Kangwon Province were studied using electron probe microanalysis (EPMA) and transmission electron microscopy (TEM). The average chemical formula of the mica-type phyllosilicate mineral analysed by EPMA is $K_{1.35}(Fe_{0.18}Mg_{0.03}Al_{3.86})(Si_{6.55}Al_{1.45})O_{20}(OH)_4$. Low K contents compared to the ideal chemistry of muscovite indicate the presence of illite in the mica-type phyllosilicate particle. X-ray diffraction study showed that pyrophyllite commonly coexists with muscovite in the shales from the Manhang Formation. TEM observations showed both the interlayer and intralayer mixing of $9.3-{\AA}$ pyrophyllite and $10-{\AA}$ muscovite layers. The low K content of the mica-type phyllosilicates apparently come from the close mixing of pyrophyllite and muscovite.