• 제목/요약/키워드: Electron Probe Microanalysis (EPMA)

검색결과 53건 처리시간 0.02초

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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    • 제30권2호
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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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Bismuth를 이용한 다층구조의 개미산 연료전지 연료전극 개발 (Development of a Formic Acid Fuel Cell Anode by Multi-layered Bismuth Modification)

  • 권영국;엄성현;이재영
    • Korean Chemical Engineering Research
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    • 제46권4호
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    • pp.697-700
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    • 2008
  • 본 연구에서는 개미산 연료전지의 연료극에서 Pt 촉매의 안정성과 활성을 높이기 위해 Bi를 UPD법을 이용하여 Pt 촉매 위에 증착시켰다. 증착된 Bi의 활용도를 높이기 위해 다층 전극구조를 적용하였으며, 전자탐침미세분석(EPMA) 결과에서 Bi가 장기성능 실험동안 촉매층에 안정적으로 존재하는 것을 확인할 수 있었다. 연료전지 성능실험에서는 Pt black 촉매 위에 Bi를 UPD한 다층 구조의 전극이 PtRu black 촉매보다 전류밀도 $150mA/cm^2$에서 약 200 mV정도 높은 성능을 나타냈다. Pt black을 40% Pt/C로 대체했을 경우 역시 높은 성능과 장기 안정성을 보였다.

사용 후 핵연료 용해 중 휘발 및 잔류 요오드 분석 (Determination of volatile and residual iodine during the dissolution of spent nuclear fuel)

  • 김정석;박순달;전영신;하영경;송규석
    • 분석과학
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    • 제22권5호
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    • pp.395-406
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    • 2009
  • 사용 후 핵연료시료 중의 요오드를 정량하고 용해과정 중 요오드의 휘발거동을 조사하기 위하여 중성자 방사화 분석(NAA) 및 전자미세탐침분석(EPMA)을 이용하였다. 모의 사용 후 핵연료시료(SIMFUELs)를 준비하여 $HNO_3$(1+1) 용액으로 $90^{\circ}C$에서 8시간 용해하고 용해 후 용해용액 중에 잔류된 요오드, 용해장치에 응축된 요오드 및 휘발하여 흡착체에 포집된 요오드 각각을 정량하였다. 응축된 요오드는 장치내 용해용액을 옮긴 후 $HNO_3$(1+1) 용액으로 재증류하여 회수하였다. 용해 및 재증류 용액중의 요오드는 용매추출과 이온교환 및 침전법으로 분리한 후 방사화학적 중성자 방사화 분석(RNAA)으로 정량하였다. 요오드 분리에 사용한 이온교환분리관 및 여과키트는 폴리에틸렌 관으로 제작하여 중성자 조사를 위한 이송관 내부의 삽입체(Insert)로 이용하였다. 핵연료용해 중 휘발된 요오드는 제조한 흡착체(Ag-Silica gel)를 담은 흡착관에 포집하였다. 흡착체를 구간별로 나누어 균질시료로 만든 다음 비파괴 중성자 방사화 분석(INAA)으로 정량하였다. 흡착된 요오드의 분포를 EPMA 분석으로 조사하였다. 모의 사용 후 핵연료 및 원자력발전소로부터의 실제 사용 후 핵연료 시료로부터 휘발된 요오드의 흡착특성을 비교하였다.

Effect of Cu-Additions on the Hand-Over Layer of an Aluminum Alloy - Hardening for the Top Ring Groove of Automotive Piston by the Plasma Transferred Arc Welding Process -

  • Moon, J.H.;Seo, C.J.;Hwang, S.H.
    • International Journal of Korean Welding Society
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    • 제1권1호
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    • pp.58-62
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    • 2001
  • The surface of AC8A Ah alloy was modified by adding the Cu powder using a Plasma Transferred Arc (PTA) welding process. Under the optimum fabricating conditions, the modified surface of AC8A Ah alloy was observed to possess the sound microstructure with a minimum porosity. Hardness and wear resistance properties of the as-fabricated alloy were compared with those of the 76 heat-treated one. In case of the as-fabricated alloy, the hardness of the modified layer was twice that of the matrix region. Although significant increase in the hardness of the matrix region was observed after T6 heat treatment, the hardness of the modified layer was not observed to change. The wear resistance of the modified layer was significantly increased compared to that of the matrix region. The microstructure of a weld zone and the matrix region were investigated using the optical microscope, scanning electron microscope (SEM), electron probe microanalysis (EPMA), and transmission electron microscope (TEM). The primary and eutectic silicon in the weld zone were finer and more curved than in the matrix region, while some precipitates has had been found therein. According to the TEM observation, the predominant precipitate present in the weld zone was the $\theta$'phase, which is precipitated during cooling by rapid solidification in PTA welding process. Improvement of hardness and wear properties in the weld zone in the as-fabricated condition can be explained based on the presence of $\theta$’precipitates and fine primary and eutectic silicon distribution.

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직류 마그네트론 스퍼터법에 의한 AlNO 복층박막의 제조와 특성 (Properties and Preparation of AlNO Multi-layer Thin Films Using DC Magnetron Sputter Method)

  • 김현후;오동현;백찬수;장건익;최동호
    • 한국전기전자재료학회논문지
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    • 제27권9호
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    • pp.589-593
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    • 2014
  • AlNO multi-layer thin films on aluminum substrates were prepared by DC reactive magnetron sputtering method. $Al_2O_3$/AlNO(LMVF)/AlNO(HMVF)/Al/substrate of 4 multi-layer has been prepared in an Ar and ($N_2+O_2$) gas mixture, and $Al_2O_3$ of top layer is anti-reflection layer on double AlNO(LMVF)/AlNO(HMVF) layers and Al metal of infrared reflection layer. In this study, the roughness and surface properties of AlNO thin films were estimated by field emission scanning electron microscopy(FE-SEM). The grain size of AlNO thin films increased with increasing sputtering power. The composition of thin films has been systematically investigated using electron probe microanalysis(EPMA). The optical properties with wavelength spectrum were recorded by UV-Vis-NIR spectrophotometry at a range of 200~1,500 nm. The absorptance of AlNO films shows the increasing trend with swelling ($N_2+O_2$) gas mixture in HMVF and LMVF deposition. The excellent optical performance showed above 98% of absorptance in visible wavelength region.

엔진 마운트 브라켓용 다이캐스팅 Al-Si-Cu 합금의 미세조직과 기계적 특성 (Microstructural and Mechanical Characteristics of Al-Si-Cu Die Casting Alloy for Engine Mount Bracket)

  • 천인범;홍승표;김정석
    • 열처리공학회지
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    • 제27권6호
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    • pp.281-287
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    • 2014
  • Microstructural and mechanical characteristics of Al-6Si-2Cu alloy for engine mount bracket prepared by gravity casting (as-cast) and die-casting (as-diecast) process have been investigated. For the microstructural characterization, the inductively coupled plasma mass spectrometry (ICP-MS), optical microscope (OM), scanning electron microscope (SEM) and electron probe microanalysis (EPMA) analyses are conducted. For the intermetallic phases, the X-ray diffraction (XRD) and energy dispersive spectroscopy (EDS) are also conducted with quantitative and qualitative analysis. Micro Vickers hardness and static tensile test are achieved in order to measure mechanical properties of alloys. Secondary dendrite arm spacing (SDAS) of as-cast and as-diecast show 37um and 18um, respectively. A large amount of coarsen eutectic Si, $Al_2Cu$ intermetallic phase and Fe-rich phases are identified in the Al-6Si-2Cu alloy. Mechanical properties of gravity casting alloy are much higher than those of die-casting alloy. Especially, yield strength and elongation of gravity casting alloy show 2 times higher than die-casting alloy. After shot peening, shot peening refined the surface grains and Si particles of the alloys by plastic deformation. The surface hardness value shows that shot peening alloy has higher value than unpeening alloy.

태양열 흡수판용 복층 TiNOx 박막의 제조와 특성 분석 (Characteristic Analysis and Preparation of Multi-layer TiNOx Thin Films for Solar-thermal Absorber)

  • 오동현;한상욱;김현후;장건익;이용준
    • 한국전기전자재료학회논문지
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    • 제27권12호
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    • pp.820-824
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    • 2014
  • TiNOx multi-layer thin films on aluminum substrates were prepared by DC reactive magnetron sputtering method. 4 multi-layers of $TiO_2$/TiNOx(LMVF)/TiNOx(HMVF)/Ti/substrate have been prepared with ratio of Ar and ($N_2+O_2$) gas mixture. $TiO_2$ of top layer is anti-reflection layer on double TiNOx(LMVF)/TiNOx(HMVF) layers and Ti metal of infrared reflection layer. In this study, the crystallinity and surface properties of TiNOx thin films were estimated by X-ray diffraction(XRD) and field emission scanning electron microscopy(FE-SEM), respectively. The grain size of TiNOx thin films shows to increase with increasing sputtering power. The composition of thin films has been investigated using electron probe microanalysis(EPMA). The optical properties with wavelength spectrum were recorded by UV-Vis-NIR spectrophotometry at a range of 200~1,500 nm. The TiNOx multi-layer films show the excellent optical performance beyond 9% of reflectance in those ranges wavelength.

기상성장법(CVT)에 의한 Iron disilicide단결정의 합성 (Synthesis of iron disilicide single crystal by chemical vapour transport)

  • 이충효;홍대석;이상진;최종건;김판채
    • 한국결정성장학회지
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    • 제12권2호
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    • pp.68-72
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    • 2002
  • Iodine ($I_2$)을 이용한 기상성장법(chemical vapour transport CVT)으로 상용 FeSi$_2$분말로부터 $\beta$-$FeSi_2$$\alpha$-$FeSi_2$단결정을 제조하였다 $FeSi_2$ 분말은 iodine과 함게 석영 ampoule에 넣은 후 진공배기하여 two-zone 전기로 내에서 기상성장 시켰다. CVT법에 의한 기상성장시 고온부분의 source측 온도는 $1050^{\circ}C$이었으며 $\beta$-$FeSi_2$$\alpha$-$FeSi_2$ 단결정이 얻어지는 성장측 온도는 각각 $750^{\circ}C$$950^{\circ}C$이었다. 이때 얻어진$\alpha$-$FeSi_2$ 단격정은 $l0\times10 \textrm{mm}^2$크기의 판상결정이었고 orthorhombic 구조의 $\beta$-$FeSi_2$, 단결정은 길이 10mm의 needle형 결정임을 알 수 있었다. $\alpha$-$FeSi_2$ 단결정의 조성을 EPMA로 조사한 결과 Si이 화학양론비보다 많은 $FeSi_{2.58}$ 이었다. CVT법으로 합성된 $\beta$-$FeSi_2$ 격정의 승온에 따른 상의 안정성을 조사한 결과 $930^{\circ}C$ 이상에서 $\alpha$-$FeSi_2$로 상변태함을 알 수 있었다.

용융온도와 유지시간이 용융법으로 제작한 고온초전도체의 임계특성에 미치는 영향 (The Effects of Melting Temperature and Holding Time on Critical Characteristics of HTSC Fabricated by Melting Method)

  • 임성훈;한태희;박경국;임성우;조동언;한병성
    • 한국전기전자재료학회논문지
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    • 제11권2호
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    • pp.154-161
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    • 1998
  • The effects of melting temperature and holding time on the critical current density($J_c$) of $YBa_2Cu_3O_x$ based superconducting bulk fabricated by MPMG process were investigated. The amount of the formed $Y_2BaCuO_5$ phases increased with the melting temperature. However, the value of critical current density was highest at 1120 $^{\circ}C$. With this proper melting temperature, the effect of holding time on the critical characteristics was also investigated. In the case of Ag addition, the volume of the formed $Y_2BaCuO_5$ phase when the amount of Ag addition was 10 wt% and 20 wt% was observed to be highest at 20 minute and 40 minute respectively. But in the specimen without Ag, volume of $Y_2BaCuO_5$ phase increased as the holding time increased. The proper melting temperature and the holding time obtained were 1120 $^{\circ}C$ and 20 minute. The long holding time was not effective for the $J_c$ improvement as well as the formation of $Y_2BaCuO_5$.

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단일입자분석법을 이용한 지하상가에서 채취한 실내입자의 특성분석 (Single-particle Characterization of Aerosol Samples Collected at an Underground Shopping Area)

  • 강선이;황희진;박유명;강수진;김혜경;노철언
    • 한국대기환경학회지
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    • 제24권5호
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    • pp.594-603
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    • 2008
  • A single particle analytical technique, named low-Z particle electron probe X-ray microanalysis, was applied to characterize four samples collected at an underground shopping area connected to Dongdeamun subway station, in January and May 2006. Based on the analysis of their chemical compositions of the samples, many distinctive particle types are identified and the major chemical species are observed to be soil-derived particles, iron-containing particles. sulfates. nitrates, and carbonaceous particles. which are encountered both in coarse and fine fractions. Carbonaceous particles exist in carbon-rich and organic. Soil derived particles such as aluminosilicates, AlSi/C, $CaCO_3\;and\;SiO_2$ are more frequently encountered in spring samples than winter samples. Nitrate- and sulfate-con taming particles are more frequently encountered in winter samples, and those nitrate- and sulfate-containing particles mostly exist in the chemical forms of $Ca(CO_3,\;NO_3),\;Ca(NO_3,\;SO_4),\;(Na,\;Mg)NO_3\;and\;(Mg,\;Na)(NO_3,\;SO_4)$. Fe-containing particles which came from nearby subway platform are in the range of about 10% relative abundances for all the samples. It is observed that nitrate- and sulfate-containing particles and carbonaceous particles are much more frequently encountered in indoor aerosol samples than in outdoor aerosols, implying that $NO_x,\;SO_x$, and VOCs at the underground shopping area were more partitioned into aerosol phase.