• Title/Summary/Keyword: Electron Probe

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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.

High Temperature Oxidation Behavior of Cr-Mo Low Alloy Steel According to Atmospheric Pressures in Humid Air (Humid air 분위기로부터 대기 압력에 따른 Cr-Mo 저합금강의 고온 산화 거동)

  • Kwon, Gi-hoon;Park, Hyunjun;Lee, Young-Kook;Moon, Kyoungil
    • Journal of the Korean Society for Heat Treatment
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    • v.35 no.5
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    • pp.246-254
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    • 2022
  • The high-temperature oxidation behavior of Cr-Mo steel AISI 4115 in air at different temperatures (600, 850, 950℃) for 120 min was studied by mass gain analysis, phase analysis (optical microscopy, electron probe micro-analysis, x-ray diffraction) and hardness measurement of each iron oxide-phase. The oxidation scales that formed on oxidation process consisted outer layer (Hematite), middle layer (Magnetite) and the inner layer (Chromite). In the case of 850 and 950℃, the oxidation mass gain per unit area of AISI 4115 steel increased according to the logarithmic rate as atmospheric pressure increased. Especially, It has been observed that with an increase in the atmospheric pressure at 600℃, the oxidation mass gain per unit area changed from a linear to logarithmic relationship.

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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High Functional $GdB_2C_3O_{7-x}$ Thin Films Fabricated by Pulsed Laser Deposition

  • Song, S.H.;Ko, K.P.;Song, K.J.;Moon, S.H.;Yoo, S.I.
    • Progress in Superconductivity and Cryogenics
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    • v.8 no.4
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    • pp.15-18
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    • 2006
  • REBCO coated conductors (RE: rare earth elements) have recently drawn great attention since they are known to possess stronger flux pinning centers in high magnetic fields compared with YBCO coated conductors. In this study, $GdBa_2Cu_3O_{7-d}(GdBCO)$ was selected to investigate the influence of the distance between target and substrate and substrate temperature on the superconducting properties of GdBCO films on the $SrTiO_3(100)$ substrate. Samples were fabricated by pulsed laser deposition (PLD) with a Nd:YAG laser (355nm). Under a given oxygen pressure of 800mTorr, we changed the distance between target and substrate from 5.5cm to 7.0cm and the substrate temperature from $750^{\circ}C\;to\;850^{\circ}C$. The crystallinity and texture of GdBCO films were analyzed by X-ray diffraction (XRD), and the surface morphology was observed by the scanning electron microscopy (SEM). Tc and Jc values were measured by the four point probe method. High quality GdBCO films with Tc of 89.7K and Jc over $1MA/cm^2$ at 77 K in self field were successfully fabricated by optimizing processing parameters. The detailed processing conditions, microstructure and superconducting properties will be presented for a discussion.

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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EPMA quantification on the chemical composition of retained austenite in a Fe-Mn-Si-C-based multi-phase steel

  • Yoon‑Uk Heo;Chang‑Gon Jeong;Soo‑Hyun Kim;Gun‑Young Yoon;T. T. T. Trang;Youngyun Woo;Eun Yoo Yoon;Young‑Seon Lee
    • Applied Microscopy
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    • v.52
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    • pp.14.1-14.10
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    • 2022
  • An electron probe X-ray microanalyzer (EPMA) is an essential tool for studying chemical composition distribution in the microstructure. Quantifying chemical composition using standard specimens is commonly used to determine the composition of individual phases. However, the local difference in chemical composition in the standard specimens brings the deviation of the quantified composition from the actual one. This study introduces how to overcome the error of quantification in EPMA in the practical aspect. The obtained results are applied to evaluate the chemical com position of retained austenite in multi-phase steel. Film-type austenite shows higher carbon content than blocky-type one. The measured carbon contents of the retained austenite show good coherency with the calculated value from the X-ray diffraction.

Alteration Textures and Mineral Chemistry of Margarite from Miwon Area, Chungcheongbukdo (충북미원지역에서 산출하는 마카라이트의 변질양상 및 광물화학)

  • 이승준;안중호;김현철;조문섭
    • Journal of the Mineralogical Society of Korea
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    • v.15 no.1
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    • pp.69-77
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    • 2002
  • Margarite, which occurs in the Unkyori Formation of Miwon area, Chungcheongbukdo, South Korea, was investigated using the petrographic microscope, back-scattered electron images (BSEI), and electron probe microanalyzer (EPMA) to characterize the alteration textures and mineral chemistries. Most margarite crystals are inhomogeneous, and chlorite was commonly observed to occur at the boundaries parallel to the rim of margarite. Cracks occur across the basal plane of the margarite, and margarite is partly replaced by chlorite along the cracks. In additon, muscovite and biotite are intergrown in margarite and chlorite crystals, suggesting that margarite was partially altered to chlorite as well as to muscovite and biotite. Chemical analysis data show that paragonite solid solution in the margarite is approximately 19.6 mol%, but clintonite solid solution is negligible. Margarite crystals in the Unkyori Formation cut or penetrate other metamorphic minerals In the same thin sections and are oriented randomly without any relationship with the foliation of host rocks, indicating that formed as a secondary mineral after peak metamorphism. Furthermore, it seems that hydrothermal fluids associated with the Mesozoic intrusions developed near the sample are closely related to the margarite formation.

Small scale magNetospheric and Ionospheric Plasma Experiments; SNIPE mission

  • Hwang, Junga;Lee, Jaejin;Shon, Jongdae;Park, Jaeheung;Kwak, Young-Sil;Nam, Uk-Won;Park, Won-Kee
    • The Bulletin of The Korean Astronomical Society
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    • v.42 no.1
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    • pp.40.3-41
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    • 2017
  • Korea Astronomy and Space Science Institute The observation of particles and waves using a single satellite inherently suffers from space-time ambiguity. Recently, such ambiguity has often been resolved by multi-satellite observations; however, the inter-satellite distances were generally larger than 100 km. Hence, the ambiguity could be resolved only for large-scale (> 100 km) structures while numerous microscale phenomena have been observed at low altitude satellite orbits. In order to resolve those spatial and temporal variations of the microscale plasma structures on the topside ionosphere, SNIPE mission consisted of four (TBD) nanosatellites (~10 kg) will be launched into a polar orbit at an altitude of 700 km (TBD). Two pairs of satellites will be deployed on orbit and the distances between each satellite will be from 10 to 100 km controlled by a formation flying algorithm. The SNIPE mission is equipped with scientific payloads which can measure the following geophysical parameters: density/temperature of cold ionospheric electrons, energetic (~100 keV) electron flux, and magnetic field vectors. All the payloads will have high temporal resolution (~ 16 Hz (TBD)). This mission is planned to launch in 2020. The SNIPE mission aims to elucidate microscale (100 m-10 km) structures in the topside ionosphere (below altitude of 1,000 km), especially the fine-scale morphology of high-energy electron precipitation, cold plasma density/temperature, field-aligned currents, and electromagnetic waves. Hence, the mission will observe microscale structures of the following phenomena in geospace: high-latitude irregularities, such as polar-cap patches; field-aligned currents in the auroral oval; electro-magnetic ion cyclotron (EMIC) waves; hundreds keV electrons' precipitations, such as electron microbursts; subauroral plasma density troughs; and low-latitude plasma irregularities, such as ionospheric blobs and bubbles. We have developed a 6U nanosatellite bus system as the basic platform for the SNIPE mission. Three basic plasma instruments shall be installed on all of each spacecraft, Particle Detector (PD), Langmuir Probe (LP), and Scientific MAGnetometer (SMAG). In addition we now discuss with NASA and JAXA to collaborate with the other payload opportunities into SNIPE mission.

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Microstructural Study of Mortar Bar on Akali-Silica Reaction by Means of SEM and EPMA Analysis (알칼리-실리카 반응에 의한 모르타르 봉의 SEM과 EPMA 분석을 통한 미세구조 연구)

  • Jun, Ssang-Sun;Lee, Hyo-Min;Jin, Chi-Sub
    • Journal of the Korea Concrete Institute
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    • v.21 no.4
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    • pp.531-537
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    • 2009
  • In this study alkali reactivity of crushed stone was conducted according to the ASTM C 227 that is traditional mortar bar test, and C 1260 that is accelerated mortar bar test method. The morphology and chemical composition of products formed in mortar bar, 3 years after the mortar bar tests had been performed, were examined using scanning electron microscopy (SEM) with secondary electron imaging (SEI) and electron probe microanalysis (EPMA) with backscattered electron imaging (BSEI). The crushed stone used in this study was not identified as being reactive by ASTM C 227. However, mortar bars exceeded the limit for deleterious expansion in accelerated mortar bar test used KOH solution. The result of SEM (SEI) analysis, after the ASTM C 227 mortar bar test, confirmed that there were no reactive products and evidence of reaction between aggregate particles and cement paste. However, mortar bars exposed to alkali solution (KOH) indicated that crystallized products having rosette morphology were observed in the interior wall of pores. EPMA results of mortar bar by ASTM C 227 indicated that white dots were observed on the surface of particles and these products were identified as Al-ASR gels. It can be considered that the mortar bar by ASTM C 227 started to appear sign of alkali-silica reaction in normal condition. EPMA results of the mortar bar by ASTM C 1260 showed the gel accumulated in the pores and diffused in to the cement matrix through cracks, and gel in the pores were found to be richer in calcium compared to gel in cracks within aggregate particles. In this experimental study, damages to mortar bars due to alkali-silica reaction (ASR) were observed. Due to the increasing needs of crushed stones, it is considered that specifications and guidelines to prevent ASR in new concrete should be developed.

CCP에서의 마이크로 아킹 Fast-imging을 통한 마이크로 아킹 방전 메커니즘 조사

  • Kim, Yong-Hun;Jang, Hong-Yeong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.276-277
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    • 2012
  • 플라즈마 아킹은 PECVD, 플라즈마 식각 그리고 토카막과 같은 플라즈마를 이용하는 여러 공정과 연구 분야에서 문제가 되어왔다. 하지만, 문제의 중요성과 다르게 아킹에 대한 본질적인 연구는 아직 미비한 상태이다. 플라즈마 아킹은 집단전자방출(collective electron emission)에 의한 스파크 방전(spark discharge) 현상이다. 집단전자방출은 전계방출(field emission)이나 플라즈마와 쉬스를 두고 인접한 표면위에서의 유전분극(dielec emission)에 의해 발생한다. 우리는 CCP 플라즈마를 이용해 micro-arcing(MA)을 일으키고 랑뮈르 프로브를 이용해 MA 동안의 플로팅 포텐셜의 변화를 측정한다. MA시 PM-tube를 이용해 광량의 변화를 측정하고 플로팅 포텐셜을 fast-imaging과 동기화 시켜 MA 발생 메커니즘을 유추한다. 우리는 $30{\times}20$ cm 크기의 사각 전극을 위 아래로 가진 챔버에서 Ar 가스를 RF (13.56 MHz) 파워를 이용해 방전시켰다. 방전 전압과 전류는 파워 전극 앞단에서 High voltage probe (Tektronix P6015A)와 Current probe (TCPA300 + TCP312)를 이용해 측정했다. 플라즈마 아킹시 변하는 플라즈마 플로팅 포텐셜은 챔버 중앙에 위치한 랑뮈프 프로브에 의해 측정되고 챔버 옆의 뷰포트 앞에 위치한 PM-tube를 이용해 아킹시 변하는 광량을 측정하고 Intensified CCD를 이용해 fast-imaging을 한다. 또한 CCD 앞에 band pass filter를 부착하여 MA의 발생 메커니즘을 유추한다. RF 방전에서의 플라즈마 아킹은 아킹시 플로팅 포텐셜의 변화에 의해 크게 세부분으로 나눌 수 있다. 아킹 발생과 동시에 급격히 감소하는 감소부분(약 2 us) 그리고 감소한 포텐셜이 유지되는 유지부분(약 0~10 ms) 그리고 감소했던 포텐셜이 서서히 원래 상태로 회복되는 회복부분(약 100 us)이다. 아킹 초기시 방출된 집단 전자들은 쉬스를 단락시키게 되고 이로 인해 플로팅 포텐셜은 급격히 감소하게 된다. 이렇게 감소한 플로팅 포텐셜은 아킹 스트리머가 유지되는 한 계속 감소한 상태를 유지하게 된다. 그리고 플라즈마를 섭동했던 집단전자방출이 중단되면 플라즈마는 섭동전의 원래 상태로 회복된다. 플라즈마 아킹 발생시 생성되는 순간적으로 많은 전자들을 국소적으로 생성하게 되고 이 전자들에 의해 광량이 순간적으로 증가하게 된다. PM-tube (750.4 nm)에 의해 측정된 아킹시 광량은 정상방전 상태의 두배 가량이 된다. 그리고 이 순간적으로 증가된 광량은 시간이 지남에 따라 감소하게 되고 정상방전 일때의 광량이 된다. 광량이 증가한 후 정상방전상태의 광량에 이르는 부분은 플로팅 포텐셜이 감소한 상태에서 유지되는 부분과 일치하고 이는 플로팅 포텐셜의 유지부분동안 집단전자방출이 있다는 간접적인 증거가 된다. 그리고 정상 방전 상태 일때의 광량이 되면 집단전자방출이 중단되었다는 것이므로 그 시점부터 플로팅 포텐셜은 정산 방전상태 일때의 포텐셜로 복구되기 시작한다. 이처럼 PM-tube를 이용한 아킹 광량 측정은 아킹 스트리머를 간접적으로 측정하게 하고 집단전자방출을 이용해 아킹 시의 플로팅 포텐셜의 변화를 설명하게 해 준다.

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