• 제목/요약/키워드: X-ray spectrometry

검색결과 326건 처리시간 0.033초

Si-N 코팅막의 기계적 물성 및 구조 분석 (Characterization of Silicon Nitride Coating Films)

  • 고철호;김봉섭;윤존도;김광호
    • 한국세라믹학회지
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    • 제42권5호
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    • pp.359-365
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    • 2005
  • Silicon nitride coating films with various ratios of nitrogen to silicon contents were prepared and characterized. The film was coated on silicon substrate by sputtering method with changing nitrogen gas flow rate in a chamber. The nitrogen to silicon ratio was found to have values in a range from 0 to 1.4. Coated film was characterized with scanning electron microscopy, transmission electron microscopy, electron probe microanalysis, nanoindentation scanning probe microscopy, x-ray photon spectrometry, and Raman spectrometry. Silicon nitride phase in all samples showed amorphous nature regardless of N/Si ratio. When N/Si ratio was 1.25, hardness and elastic modulus of silicon nitride film showed maximum with 22 GPa and 210 GPa, respectively. Those values decreased, when N/Si ratio was higher than 1.25. Raman spectrum showed that no silicon phase exist in the film. XPS result showed that the silicon-nitrogen bond was dominant way for atomic bonding in the film. The structure and property was explained with Random Bonding Model(RBM) which was consistent with the microstructure and chemistry analysis for the coating films.

Chemical Compositions and Pyrolysis Characteristics of Oil Shales Distributed in Korea

  • Yang, Moon Yul;Yang, Myoung Kee;Lee, Sang Hak;Wakita, Hisanobu
    • 분석과학
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    • 제8권4호
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    • pp.487-492
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    • 1995
  • The chemical compositions and pyrolysis characteristics of oil shales and source rocks distributed in the southwestern and southeastern parts of the Korean peninsular have been investigated. In order to compare the results of Korean samples with those of shales giving high oil yields, two Colorado oil shale samples and one Paris source rock samples were also investigated. Chemical compositions of the samples were analysed by means of gravimetry, CHN analysis, X-ray diffraction method, inductively coupled plasma atomic emission spectrometry and atomic absorption spectrometry. A custom made pyrolyser and a Rock-Eval system were used for the pyrolysis studies. Pyrolyses of the samples were carried out by means of a temperature controlling device to $600^{\circ}C$ at a heating rate of $5^{\circ}C/min$ with a helium flow rate of $1200m{\ell}/min$. The results of pyrolysis study indicated that Colorado shale samples belong to type I and all the other samples belong to type II.

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Preparation and Characterization of Quercetin-Loaded Solid Dispersion by Solvent Evaporation and Freeze-Drying Method

  • Park, Sang Hyun;Song, Im-Sook;Choi, Min-Koo
    • Mass Spectrometry Letters
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    • 제7권3호
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    • pp.79-83
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    • 2016
  • We prepared solid dispersion formulations of quercetin to enhance its solubility and dissolution rate. Various quercetin-loaded solid dispersion were tested with quercetin, poloxamer 407, and carrier such as hydroxypropyl methyl cellulose (HPMC), polyethylene glycol 8000 (PEG 8000), and polyvinylpyrrolidone K40 (PVP K40) using solvent evaporation and freeze drying methods in terms of both the aqueous solubility and the dissolution rates of quercetin. The solubility of quercetin as its solid dispersion formulations was markedly improved compared with that of quercetin powder. Especially, highest solubility of quercetin was observed when HPMC was used as a carrier. The cumulative dissolution of quercetin within 360 min from solid dispersion composed of quercetin, poloxamer 407, and HPMC was 8.8-fold higher than the dissolution of pure quercetin. The results of powder X-ray diffraction (XRD) and scanning electron microscope (SEM) indicated that quercetin transformed from a crystalline to an amorphous form through the solid dispersion formulation process. These results suggest that the solid dispersion formulation of quercetin with poloxamer 407 and HPMC could be a promising option for enhancing the solubility and dissolution rate of quercetin.

Protein Structural Characterization by Hydrogen/Deuterium Exchange Mass Spectrometry with Top-down Electron Capture Dissociation

  • Yu, Hai Dong;Ahn, Seonghee;Kim, Byungjoo
    • Bulletin of the Korean Chemical Society
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    • 제34권5호
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    • pp.1401-1406
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    • 2013
  • This study tested the feasibility of observing H/D exchange of intact protein by top-down electron capture dissociation (ECD) mass spectrometry for the investigation of protein structure. Ubiquitin is selected as a model system. Local structural information was obtained from the deuteration levels of c and $z^{\cdot}$ ions generated from ECD. Our results showed that ${\alpha}$-helix region has the lowest deuteration level and the C-terminal fraction containing a highly mobile tail has the highest deuteration level, which correlates well with previous X-Ray and HDX/NMR analyses. We studied site-specific H/D exchange kinetics by monitoring H/D exchange rate of several structural motives of ubiquitin. Two hydrogen bonded ${\beta}$-strands showed similar HDX rates. However, the outer ${\beta}$-strand always has higher deuteration level than the inner ${\beta}$-strand. The HDX rate of the turn structure (residues 8-11) is lower than that of ${\beta}$-strands (residues 1-7 and residues 12-17) it connects. Although isotopic distribution gets broader after H/D exchange which results in a limited number of backbone cleavage sites detected, our results demonstrate that this method can provide valuable detailed structural information of proteins. This approach should also be suitable for the structural investigation of other unknown proteins, protein conformational changes, as well as protein-protein interactions and dynamics.

재산화 질화산화막의 기억트랩 분석과 프로그래밍 특성 (A Study on the Memory Trap Analysis and Programming Characteristics of Reoxidized Nitrided Oxide)

  • 남동우;안호명;한태현;서광열;이상은
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2001년도 추계학술대회 논문집
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    • pp.17-20
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    • 2001
  • Nonvolatile semiconductor memory devices with reoxidized nitrided oxide(RONO) gate dielectric were fabricated, and nitrogen distribution and bonding species which contributing memory characteristics were analyzed. Also, memory characteristics of devices according to anneal temperatures were investigated. The devices were fabricated by 0.35$\mu\textrm{m}$ retrograde twin well CMOS processes. The processes could be simple by in-situ process of nitridation anneal and reoxidation. The nitrogen distribution and bonding state of gate dielectric were investigated by Dynamic Secondary Ion Mass Spectrometry(D-SIMS), Time-of-Flight Secondary ton Mass Spectrometry(ToF-SIMS), and X-ray Photoelectron Spectroscopy(XPS). Nitrogen concentrations are proportional to nitridation anneal temperatures and the more time was required to form the same reoxidized layer thickness. ToF-SIMS results show that SiON species are detected at the initial oxide interface and Si$_2$NO species near the new Si-SiO$_2$ interface that formed after reoxidation. As the anneal temperatures increased, the device showed worse retention and degradation properties. These could be said that nitrogen concentration near initial interface is limited to a certain quantity, so excess nitrogen are redistributed near the Si-SiO$_2$ interface and contributed to electron trap generation.

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PECVD로 증착된 금속층을 포함하는 DLC 박막의 기계적 특성 분석 (An analysis of tribological properties of the metal interlayered DLC films prepared by PECVD method)

  • 전영숙;최원석;박용섭;홍병유
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2004년도 하계학술대회 논문집 Vol.5 No.2
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    • pp.951-954
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    • 2004
  • 본 논문에서는 DLC(Diamond-like Carbon) 박막과 기판 사이에 금속층을 포함하는 DLC 박막의 기계적 특성을 분석하였다. 금속층은 sputtering법을 사용하고, DLC 박막은 PECVD법을 사용하여 각각 중착하였다. 티타늄(Ti), 니켄(Ni), 크롬(Cr)을 각 중간 금속층으로 사용한 후 DLC 박막과 실리콘(Si) 기판 간의 기계적 특성을 분석하였다. 각 막의 두께는 FE-SEM으로 확인하였고, DLC 박막의 구조 평가는 Raman spectrometer를 사용하여 분석하였으며, 각 금속층과 DLC 박막의 표면 상태는 AFM을 이용하여 확인하였다. XRD 분석을 통하여 박막의 격자분석을 하였고, SIMS(secondary ion mass spectrometry) 분석을 통하여 DLC 박막의 depth Profile을 확인하였다.

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고밀도 $CF_{4}/Ar$ 플라즈마에서 $YMnO_3$ 박막의 식각 매카니즘 (Etching Mechanism of $YMnO_3$ Thin Films in High Density $CF_{4}/Ar$ Plasma)

  • 이철인;김동표;김창일
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2001년도 춘계학술대회 논문집 반도체재료
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    • pp.12-16
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    • 2001
  • We investigated the etching characteristics of $YMnO_3$ thin films in high-density plasma etching system. In this study. $YMnO_3$ thin films were etched with $CF_{4}/Ar$ gas chemistries in inductively coupled plasma (ICP). Etch rates of $YMnO_3$ were measured according to gas mixing ratios. The maximum etch rate of $YMnO_3$ is 18 nm/min at $CF_{4}/(CF_{4}+Ar)$ of 20%. In optical emission spectroscopy (OES) analysis, F radical and Ar* ions in plasma at various gas chemistries decreased with increasing $CF_4$ content. Chemical states of $YMnO_3$ films exposed in plasma were investigated with x-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS). There is a chemical reaction between metal (Y, Mn) and F and metal-fluorides were removed effectively by Ar ion sputtering. $YF_x$, $MnF_x$ such as YF, $YF_2$, $YF_3$ and $MnF_3$ Were detected using SIMS analysis. The etch slope is about $65^{\circ}C$ and free of residues.

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Cobalt가 치환된 Barium Ferrite 분말 제조 시 자기적 특성변화 (Changes in Magnetic Properties When Manufacturing Cobalt-substituted Barium Ferrite Powder)

  • 엄명헌;연제욱;이차진;하범용
    • 한국산학기술학회논문지
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    • 제21권10호
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    • pp.30-39
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    • 2020
  • 본 연구에서는 Sol-Gel 방법을 이용하여 단일상의 Barium ferrite 분말을 제조하였으며, 이때 Ba에 대한 Fe(Fe/Ba)의 몰비와 열처리 온도를 달리하여 단일상의 Barium ferrite를 제조하기 위한 최적의 실험조건을 찾고자 하였다. 또한 고밀도 자기기록매체에 사용되기 위한 2.5 ~ 5.5 kOe 크기의 보자력을 가지는 ferrite 미립자 제조를 위해 보자력 제어에 뛰어난 효과를 지닌 cobalt를 첨가제로 하여 cobalt가 치환된 Barium ferrite 미립자를 제조하고 이들에 대한 자기적 특성 변화를 조사하였다. 제조된 Barium ferrite의 결정구조 및 단일상의 합성여부를 확인하기 위해 X-Ray Diffractometer(XRD), Thermogravimetric-Differential Thermal Analysis(TG-DTA), Field Emission Scanning Electron Microscope(FE-SEM)을 이용하여 분석하였으며, 화학적 구조와 조성의 분석을 위해 Fourier Transform Infrared Spectroscopy(FT-IR), Energy Dispersive X-Ray Spectrometer(EDS)를 사용하였다. 또한 Vibrating Sample Magnetometer(VSM)을 통해 cobalt가 치환된 Barium ferrite 분말의 보자력을 측정하였다. 그 결과 단일상의 Barium ferrite는 Fe/Ba의 몰비가 10, 900 ℃의 열처리 온도에서 가장 잘 합성되었다. Co의 첨가량이 증가할수록 보자력은 감소하였으며 Fe에 대한 Co(Co/Fe)의 몰비가 0.16 이내 일 때, 고밀도 자기기록매체에 사용할 수 있는 보자력 값인 2.5 ~ 5.5 kOe를 가지는 Barium ferrite가 합성되었다.

TOF-SIMS를 이용한 광물 표면의 단층조직 분석 연구 (Mono-layer Compositional Analysis of Surface of Mineral Grains by Time-of-Flight Secondary-Ion Mass Spectrometry (TOF-SIMS))

  • 공봉성;;김주영
    • 한국광물학회지
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    • 제18권2호
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    • pp.127-134
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    • 2005
  • 금속제련공학 및 환경과학 분야에 있어서 물질전체를 구성하고 있는 화학적 조성이 중요한 요소이나, 입자 표면의 화학조성과 미분화된 입자들의 표면 반응성을 제어함과 동시에, 입자 계면에서 일어나는 중금속과 유기물질등의 반응은 제련공정과 환경오염에 중요한 역할을 한다. 그러므로, 수용액상에 존재하는 여러 종류의 화학 물질과 광물입자 표면 사이에서 일어나는 계면반응 과정의 이해는 상당히 중요한 것이다. 일반적으로 입자 표면 분석에는 ex-situ 법을 사용하는 X-ray photo-electron spectroscopy (XPS) 분석 방법이 많이 적용되고 있으나, 이는 분석대상시료의 크기가 보통 100 마이크론에서 1 cm 정도의 범위 안에 혼재-혼합되어있는 고체 입자들을 분석하기 때문에 채취 분석된 X-ray의 원래 발산한 입자표면을 분석할 수는 없다. 그래서 본 연구에서는 Time-of-Flight Secondary-Ion Mass Spectroscopy (TOF-SIMS)를 응용하여 황화광물의 부유선광 공정 중 생성된 미세한 유화광물입자$(30\~75\;microns)$ 표면에 형성된 무기, 유기물의 반응 관찰을 통해 이들의 정성분석 및 상대적 정량분석법을 연구하고자 하였다.

Basic characterization of uranium by high-resolution gamma spectroscopy

  • Choi, Hee-Dong;Kim, Junhyuck
    • Nuclear Engineering and Technology
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    • 제50권6호
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    • pp.929-936
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    • 2018
  • A basic characterization of uranium samples was performed using gamma- and X-ray spectroscopy. The studied uranium samples were eight types of certified reference materials with $^{235}U$ enrichments in the range of 1-97%, and the measurements were performed over 24 h using a high-resolution and high-purity planar germanium detector. A general peak analysis of the spectrum and the $XK_{\alpha}$ region of the uranium spectra was carried out by using HyperGam and HyperGam-U, respectively. The standard reference sources were used to calibrate the spectroscopy system. To obtain the absolute detection efficiency, an effective solid angle code, EXVol, was run for each sample. Hence, the peak activities and isotopic activities were determined, and then, the total U content and $^{234}U$, $^{235}U$, and $^{238}U$ isotopic contents were determined and compared with those of the certified reference values. A new method to determine the model age based on the ratio of the activities of $^{223}Ra$ and $^{235}U$ in the sample was studied, and the model age was compared with the known true age. In summary, the present study developed a method for basic characterization of uranium samples by nondestructive gamma-ray spectrometry in 24 h and to obtain information on the sample age.