• 제목/요약/키워드: X-ray microanalysis

검색결과 74건 처리시간 0.027초

반응성 마그네트론 스퍼터링법으로 제조한 Ti-Al-V-N 박막의 미세조직 및 부착특성에 관한 연구 (The microstructure and adhesive characteristics of Ti-Al-V-N films prepared by reactive magnetron sputtering)

  • 손용운;이영기
    • 열처리공학회지
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    • 제12권3호
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    • pp.199-205
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    • 1999
  • The quaternary Ti-Al-V-N films have been grown on glass substrates by reactive dc and rf magnetron sputter deposition from a Ti-6Al-4V target in mixed Ar-$N_2$ discharges. The Ti-Al-V-N films were investigated by means of X-ray diffraction(XRD), electron probe microanalysis(EPMA) and scratch tester. Both XRD and EPMA results indicated that the Ti-Al-V-N films were of single B1 NaCl phase having columnar structure with the (111) preferred orientation. Scratch tester results showed that the adhesion strength of Ti-Al-V-N films which treated with substrate heating and vacuum annealing was superior to that of as-deposited film. The good adhesion strength was also achieved in the double-layer structure of Ti-Al-V-N/Ti-Al-V/Glass.

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오스테나이트 스테인리스 주강의 미세 조직 및 고온 산화 특성에 미치는 합금원소의 영향 (Effects of Alloying Elements on the Characteristics of Microstructure and High Temperature Oxidation of Cast Austenitic Stainless Steel)

  • 이인성;전순혁;김순태;이정석;고영상;김종명
    • 한국주조공학회지
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    • 제30권5호
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    • pp.179-186
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    • 2010
  • To elucidate the effects of alloying elements on the characteristics of microstructure and high temperature oxidation of cast austenitic stainless steel, a thermodynamic calculation, a cyclic oxidation test, a X-ray diffraction, a scanning electron microscopy-back scattered electron, a electron probe microanalysis were conducted. The thermodynamic calculation for the effect of vanadium (V) addition on the formation of various precipitates leads to a decrease of chromium (Cr)-rich $M_{23}C_6$ carbides due to the formation of M (C, N) carbo-nitrides containing V and / or niobium (Nb). The V added alloy increased the resistance to high temperature oxidation due to a decrease of Cr-depleted zone deteriorating the oxidation resistance and due to the V-enriched oxide layer formed in inner oxide layer blocking the outward transport of cations.

Electrochemical Characteristics of Carbon-coated Si/Cu/graphite Composite Anode

  • Kim, Hyung-Sun;Chung, Kyung-Yoon;Cho, Won-Il;Cho, Byung-Won
    • Bulletin of the Korean Chemical Society
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    • 제30권7호
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    • pp.1607-1610
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    • 2009
  • The carbon-coated Si/Cu powder has been prepared by mechanical ball milling and hydrocarbon gas decomposition methods. The phase of Si/Cu powder was analyzed using X-ray diffraction (XRD), dispersive Raman spectroscopy, electron probe microanalysis (EPMA) and transmission electron microscope (TEM). The carbon-coated Si/Cu powders were used as anode active material for lithium-ion batteries. Their electrochemical properties were investigated by charge/discharge test using commercial LiCo$O_2$ cathode and lithium foil electrode, respectively. The surface phase of Si/Cu powders consisted of carbon phase like the carbon nanotubes (CNTs) with a spacing layer of 0.35 nm. The carbon-coated Si/Cu/graphite composite anode exhibited a higher capacity than commercial graphite anode. However, the cyclic efficiency and the capacity retention of the composite anode were lower compared with graphite anode as cycling proceeds. This effect may be attributed to some mass limitations in LiCo$O_2$ cathode materials during the cycling.

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

  • Park T.J.;Kang M.J.;Choi S.Y.
    • 정보저장시스템학회논문집
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    • 제1권1호
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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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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.

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.

전자현미분석에서 발생하는 규산염 유리 시료의 Na 이동 효과 보정 (Correction for Na Migration Effects in Silicate Glasses During Electron Microprobe Analysis)

  • 김화영;박창근
    • 광물과 암석
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    • 제35권4호
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    • pp.457-467
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    • 2022
  • 전자현미분석기를 이용한 규산염 유리의 정량화학조성 분석 시 알칼리 원소, 특히 Na이 전자빔에 의해 분석 영역 밖으로 이동(migration)하면서 X선 측정 세기가 시간에 따라 감소하는 현상은 오래 전부터 알려져 왔다. EPMA로 규산염 유리의 Na 함량을 정확하게 측정하기 위해서는 전자빔에 의한 Na 이동을 최소화하는 분석방법을 적용하거나 Na 이동에 따른 X선 측정 세기의 감소 효과를 보정해 주어야 한다. 본 연구에서는 X선 세기의 시계열 변화 곡선을 이용해 Na 이동에 의한 X선 감소를 보정할 수 있는 Probe for EPMA 소프트웨어의 Time Dependent Intensity(TDI) 보정 기능을 이용해 규산염 유리 표준시료 8종의 Na을 분석하였다. 일반적인 지질시료 분석 조건인 15 kV 가속전압, 20 nA 전류 세기 하에서 TDI 보정의 정확도를 검증하였다. 연구 결과 20 ㎛ 크기의 큰 전자빔을 사용했을 때는 Na 감소가 거의 일어나지 않아 보정 없이도 Na의 함량을 정확하게 측정할 수 있었다. 빔의 크기가 10 ㎛ 이하일 때는 Na 감소가 일어나 최대 -55%에 달하는 큰 오차가 발생하는데 TDI 보정을 적용해 이 오차를 ±10% 이내로 줄일 수 있다. Na X선 시계열 변화의 초기 측정값에 가중치를 주고 변화 추세를 선형적으로 가정하는 방법을 사용하면 상대오차를 ±6% 이내로 더 줄여 정확한 Na2O 함량을 얻을 수 있었다. 따라서 알칼리 원소가 많이 포함된 유리질 시료에서 분석 영역이 충분히 크지 못해 작은 전자빔을 사용해야만 한다면 적절한 TDI 보정을 반드시 해주어야 정확한 조성을 얻을 수 있다.

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

  • 최승현;문향란;이영부;이정후
    • 한국광물학회지
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    • 제24권4호
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    • pp.313-320
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    • 2011
  • 강원도 태백지역에 분포하는 만항층 셰일의 운모류 층상규산염광물입자에 대한 EPMA 및 TEM 연구를 수행하였다. EPMA 분석에 의한 만항층 셰일 내 운모류 층상규산염광물의 평균 화학식은 $K_{1.35}(Fe_{0.18}Mg_{0.03}Al_{3.86})(Si_{6.55}Al_{1.45})O_{20}(OH)_4$이며, 이는 백운모의 이상화학식과 비교하면 층간 양이온인 K의 함량이 낮아서 일라이트에 가까운 조성을 갖는다. X-선 회절 분석에 의하면 만항층 셰일에서 파이로필라이트가 흔히 백운모와 함께 산출된다. TEM 격자상 관찰에 의하여 $10{\AA}$의 백운모와 $9.3{\AA}$의 파이로필라이트 층들이 단일 층 수준에서의 층간 혼합 및 층 내 혼합 현상이 동시에 관찰되었다. EPMA 분석에서 K 함량이 백운모에 비해 낮게 분석된 원인은 이처럼 입자 내에서 백운모와 파이로필 라이트가 밀접하게 공존하기 때문으로 판단된다.

Annealing of Co-Cr dental alloy: effects on nanostructure and Rockwell hardness

  • Ayyildiz, Simel;Soylu, Elif Hilal;ide, Semra;Kilic, Selim;Sipahi, Cumhur;Piskin, Bulent;Gokce, Hasan Suat
    • The Journal of Advanced Prosthodontics
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    • 제5권4호
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    • pp.471-478
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    • 2013
  • PURPOSE. The aim of the study was to evaluate the effect of annealing on the nanostructure and hardness of Co-Cr metal ceramic samples that were fabricated with a direct metal laser sintering (DMLS) technique. MATERIALS AND METHODS. Five groups of Co-Cr dental alloy samples were manufactured in a rectangular form measuring $4{\times}2{\times}2$ mm. Samples fabricated by a conventional casting technique (Group I) and prefabricated milling blanks (Group II) were examined as conventional technique groups. The DMLS samples were randomly divided into three groups as not annealed (Group III), annealed in argon atmosphere (Group IV), or annealed in oxygen atmosphere (Group V). The nanostructure was examined with the small-angle X-ray scattering method. The Rockwell hardness test was used to measure the hardness changes in each group, and the means and standard deviations were statistically analyzed by one-way ANOVA for comparison of continuous variables and Tukey's HSD test was used for post hoc analysis. P values of <.05 were accepted as statistically significant. RESULTS. The general nanostructures of the samples were composed of small spherical entities stacked atop one another in dendritic form. All groups also displayed different hardness values depending on the manufacturing technique. The annealing procedure and environment directly affected both the nanostructure and hardness of the Co-Cr alloy. Group III exhibited a non-homogeneous structure and increased hardness ($48.16{\pm}3.02$ HRC) because the annealing process was incomplete and the inner stress was not relieved. Annealing in argon atmosphere of Group IV not only relieved the inner stresses but also decreased the hardness ($27.40{\pm}3.98$ HRC). The results of fitting function presented that Group IV was the most homogeneous product as the minimum bilayer thickness was measured (7.11 ${\AA}$). CONCLUSION. After the manufacturing with DMLS technique, annealing in argon atmosphere is an essential process for Co-Cr metal ceramic substructures. The dentists should be familiar with the materials that are used in clinic for prosthodontics treatments.

항온항습 조건하에서 Ni/Cr 층의 두께에 따른 FCCL의 접합 신뢰성 평가 (Adhesion reliability of flexible copper clad laminate under constant temperature and humidity condition by thickness of Ni/Cr seed layer)

  • 최정현;노보인;윤정원;윤재현;최돈현;김용일;정승부
    • 대한용접접합학회:학술대회논문집
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    • 대한용접접합학회 2009년 추계학술발표대회
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    • pp.75-75
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    • 2009
  • 연성회로기판은 일반적으로 절연체를 이루는 폴리이미드와 전도체를 이루는 구리로 구성되어 있다. 폴리이미드는 뛰어난 열적 화학적 안정성, 기계적 특성, 공정성 등의 장점으로 인해 연성회로기판의 절연체로서 제안되었지만 전도체를 이루는 구리와의 접합 특성이 우수하지 않기 때문에 많은 연구가 현재까지 진행되고 있고, 그 결과 연성회로기판의 접합 특성에 많은 개선이 이루어짐과 동시에 다양한 공정 방법이 제안되고 있다. 하지만 고온다습한 환경에서 사용될 경우 폴리이미드의 높은 흡습성과, 구리와 seed layer의 산화 문제로 인해 접합 특성이 저하된다는 단점 또한 가지고 있다. 따라서 본 연구를 통해 고온다습한 조건하에서 seed layer가 80Ni/20Cr 합금으로 구성된 연성회로기판의 seed layer의 두께와 시효시간으로 인해 발생하는 접합 신뢰성의 차이를 관찰하였다. 본 연구에서는 두께 $25{\mu}m$의 폴리이미드 위에 각각 100, 200, $300{\AA}$ 두께의 80Ni/20Cr의 합금 조성을 가지는 seed layer를 스퍼터링 공정을 통해 형성한 후 전해도금법을 이용하여 $8{\mu}m$ 두께의 구리 전도층을 형성하였다. 접합 특성 평가를 위해 ICP 규격에 따라 전도층 패턴을 폭 3.2mm, 길이 230mm로 시편을 제작하여 50.8mm/min의 이송 속도로 각 시편당 8회의 $90^{\circ}$ peel test를 실시하였다. 또한 $85^{\circ}C$/85% 항온항습 조건하에서 각각 24, 72, 120, 168시간 동안 시효 처리 후 같은 방법으로 연성회로기판의 접합 특성을 평가하였다. 파면의 형상과 조성을 분석하기 위해 SEM (Scanning electron microscope)과 EDS (Energy-dispersive X-ray spectroscopy)를 사용하였으며, 파면의 조도 측정을 위해 AFM (Atomic force microscope)을 사용하였다. 또한 파면의 잔여물 분석을 위해 EPMA (Energy probe microanalysis)를 사용하였고 계면의 화학적 결합상태를 분석하기 위해 XPS (X-ray photoelectron spectroscopy)를 통해 파면을 분석하였다.

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