• Title/Summary/Keyword: X-ray spectroscopy

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A Study on the Properties of Substituted Ferrite (Fe-Al-Ga-Si) (치환형 Ferrite (Fe-Al-Ga-Si)의 특성 연구)

  • Choi, Seung-Han
    • Korean Journal of Materials Research
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    • v.21 no.8
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    • pp.439-443
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    • 2011
  • The crystal structure and magnetic properties of a new solid solution type ferrite $(Fe_2O_3)_5-(Al_2O_3)_{3.4}-(Ga_2O_3)_{0.6}-SiO$ were investigated using X-ray diffraction and M$\"{o}$ssbauer spectroscopy. The results of the X-ray diffraction pattern indicated that the crystal structure of the sample appears to be a cubic spinel type structure. The lattice constant (a = 8.317 ${\AA}$) decreases slightly with the substitution of $Ga_2O_3$ even though the ionic radii of the Ga ions are larger than that of the Al ions. The results can be attributed to a higher degree of covalency in the Ga-O bonds than in the Al-O and Fe-O bonds, which can also be explained using the observed M$\"{o}$ssbauer parameters, which are the magnetic hyperfine field, isomer shift, and quadrupole splitting. The drastic change in the magnetic structure according to the Ga ion substitution in the $ (Fe_2O_3)_5(Al_2O_3)_{4-x}(Ga_2O_3)_xSiO$ system and the low temperature variation have been studied through a M$\"{o}$ssbauer spectroscopy. The M$\"{o}$ssbauer spectrum at room temperature shows the superpositions of two Zeeman patterns and a strong doublet. It shows significant departures from the prototypical ferrite and is comparable with the diluted ferrite. The doublet of spectrum at room temperature appears to originate from superparamagnetic clusters and also the asymmetry of the doublet appears to be caused by the preferred orientation of the crystallites. The M$\"{o}$ssbauer spectra below room temperature show various complicated patterns, which can be explained by the freezing of the superparamagnetic clusters. On cooling, the magnetic states of the sample were various and multi critical.

Analysis of Wide-gap Semiconductors with Superconducting XAFS Apparatus

  • Shiki, S.;Zen, N.;Matsubayashi, N.;Koike, M.;Ukibe, M.;Kitajima, Y.;Nagamachi, S.;Ohkubo, M.
    • Progress in Superconductivity
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    • v.14 no.2
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    • pp.99-101
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    • 2012
  • Fluorescent yield X-ray absorption fine structure (XAFS) spectroscopy is useful for analyzing local structure of specific elements in matrices. We developed an XAFS apparatus with a 100-pixel superconducting tunnel junction (STJ) detector array with a high sensitivity and a high resolution for light-element dopants in wide-gap semiconductors. An STJ detector has a pixel size of $100{\mu}m$ square, and an asymmetric layer structure of Nb(300 nm)-Al(70 nm)/AlOx/Al(70 nm)-Nb(50 nm). The 100-pixel STJ array has an effective area of $1mm^2$. The XAFS apparatus with the STJ array detector was installed in BL-11A of High Energy Accelerator Research Organization, Photon Factory (KEK PF). Fluorescent X-ray spectrum for boron nitride showed that the average energy resolution of the 100-pixels is 12 eV in full width half maximum for the N-K line, and The C-K and N-K lines are separated without peak tail overlap. We analyzed the N dopant atoms implanted into 4H-SiC substrates at a dose of 300 ppm in a 200 nm-thick surface layer. From a comparison between measured X-ray Absorption Near Edge Structure (XANES) spectra and ab initio FEFF calculations, it has been revealed that the N atoms substitute for the C site of the SiC lattice.

Fine Structure Effect of PdCo electrocatalyst for Oxygen Reduction Reaction Activity: Based on X-ray Absorption Spectroscopy Studies with Synchrotron Beam

  • Kim, Dae-Suk;Kim, Tae-Jun;Kim, Jun-Hyuk;Zeid, E. F. Abo;Kim, Yong-Tae
    • Journal of Electrochemical Science and Technology
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    • v.1 no.1
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    • pp.31-38
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    • 2010
  • In this study, we have demonstrated the fine structure effect of PdCo electrocatalyst on oxygen reduction reaction activity with different alloy composition and heat-treatment time. In order to identify the intrinsic factors for the electrocatalytic activity, various X-ray analyses were used, including inductively coupled plasma-atomic emission spectrometer, transmission electron microscopy, X-ray diffractometer, and X-ray Absorption Spectroscopy technique. In particular, extended X-ray absorption fine structure was employed to extract the structural parameters required for understanding the atomic distribution and alloying extent, and to identify the corresponding simulated structures by using FEFF8 code and IFEFFIT software. The electrocatalytic activity of PdCo alloy nanoparticles for the oxygen reduction reaction was evaluated by using rotating disk electrode technique and correlated to the change in structural parameters. We have found that Pd-rich surface was formed on the Co core with increasing heating time over 5 hours. Such core shell structure of PdCo/C showed that a superior oxygen reduction reaction activity than pure Pd/C or alloy phase of PdCo/C electrocatalysts, because the adsorption energy of adsorbates was apparently reduced by lowering the dband center of the Pd skin due to a combination of the compressive strain effect and ligand effect.

Preparation and Characterization of Suvarna Bhasma Parada Marit - Characterization of Suvarna Bhasma Parada Marit -

  • Thakur, Kapil;Gudi, Ramacharya;Vahalia, Mahesh;Shitut, Shekhar;Nadkarni, Shailesh
    • Journal of Pharmacopuncture
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    • v.20 no.1
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    • pp.36-44
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    • 2017
  • Objectives: The goal of this study was to characterize Suvarna Bhasma Parada Marit by using the Ayurvedic test parameters, physico-chemical tests, and various instrumentation techniques. Methods: Suvarna Bhasma, an Ayurvedic formulation manufactured as per Bharat Bhaishajya Ratnakar 5/8357 (BBR), has been studied using various instrumentation techniques: X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), laser particle size distribution (PSD) analysis, fourier transform infrared spectroscopy (FT-IR), and atomic absorption spectroscopy (AAS), and physico-chemical parameters, such as the loss on drying (LOD), loss on ignition (LOI), and acid insoluble Ash (AIA) were determined. In addition, Ayurvedic tests, such as Rekhapurnatva (enterable in the furrows of the fingers), Varitaratwa (floatable over water), Nirdhoomta (smokeless), Dantagre Kach-Kach (gritty particle feeling between the teeth), were performed. Results: The XRD study showed Suvarna Bhasma to be crystalline in nature and to contain more than 98% gold. The mean size of the gold crystallites was less than 10 microns, and the morphology was globular and irregular. Suvarna Bhasma contains gold as its single and major element, with EDAX and FT-IR spectra showing that it is more than 98% pure gold. The moisture content (LOD) is less than 0.5%, the LOI is less than 2%, and the AIA is not less than 95%. The Ayurvedic tests, as specified above, helped to confirm the quality of Suvarna bhasma prepared as per the text reference (BBR). Conclusion: This chemical characterization of Suvarna Bhasma performed in this study by using modern instrumentation techniques will be helpful in understanding its pharmacological actions and will help in establishing quality protocols and specifications to substantiate the safety, efficacy & quality of Suvarna Bhasma.

Comparative Study of Undoped and Nickel-Doped Molybdenum Oxide Photoanodes for PEC Water Splitting

  • Garcia-Garcia, Matias
    • Journal of Electrochemical Science and Technology
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    • v.13 no.3
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    • pp.377-389
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    • 2022
  • The current global energy supply depends heavily on fossil fuels. This makes technology such as direct water splitting from harvesting solar energy in photoelectrochemical (PEC) systems potentially attractive due to its a promising route for environmentally benign hydrogen production. In this study, undoped and nickel-doped molybdenum oxide photoanodes (called photoanodes S1 and S2 respectively) were synthesized through electrodeposition by applying -1.377 V vs Ag/AgCl (3 M KCl) for 3 hours on an FTO-coated glass substrate immersed in molibdatecitrate aqueous solutions at pH 9. Scanning electron microscopy (SEM), atomic force microscopy (AFM), energy-dispersive X-ray spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS) were used for microstructural and compositional characterizations of the photoanodes. In addition, the optical and photoelectrochemical characterizations of these photoanodes were performed by UV-Visible spectroscopy, and linear scanning voltammetry (LSV) respectively. The results showed that all the photoanodes produced exhibit conductivity and catalytic properties that make them attractive for water splitting application in a photoelectrochemical cell. In this context, the photoanode S2 exhibited better photocatalytic activity than the photoanode S1. In addition, photoanode S2 had the lowest optical band-gap energy value (2.58 eV), which would allow better utilization of the solar spectrum.

Studies on the etching characteristics of PZT thin films using inductively coupled plasma (고밀도 플라즈마에 의한 PZT 박막의 식각특성 연구)

  • 안태현;김창일;장의구;서용진
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.13 no.3
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    • pp.188-192
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    • 2000
  • In this study PZT etching was performed using planar inductively coupled Ar/Cl$_2$/BCI$_3$ plasma. The etch rate of PZT film was 2450 $\AA$/min at Ar(20)/BCl$_3$(80) gas mixing ratio and substrate temperature of 8$0^{\circ}C$. X-ray photoelectron spectroscopy(XPS) analysis for films composition of etched PZT surface was utilized. The chemical bond of PbO is broken by ion bombardment and Cl radical, and the peak of metal Pb in a Pb 4f narrow scan begins to appear upon etching. As increasing additive BCl$_3$content the relative content of oxygen decreases rapidly in contrast with etch rate of PZT thin film. So we though that the etch rate of PZT thin film increased because abundant B and BCl radicals made volatile oxy-compound such as B$_{x}$/O$_{y}$ and/or BClO$_{x}$ bond. We achieved etch profile of about 80$^{\circ}$ at Ar(20)/BCl$_3$(80) gas mixing condition and substrate temperature of 8$0^{\circ}C$TEX>X>.

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A Study on Iron Compounds of Scoria in The Northern Area of Jeju (제주 북부지역 스코리아의 철 화합물에 관한 연구)

  • Choi, Won-Jun;Ko, Jeong-Dae
    • Journal of the Korean Magnetics Society
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    • v.18 no.5
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    • pp.168-173
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    • 2008
  • Fe compounds of scoria distributed in northern area of Jeju island are investigated using X-ray fluorescence spectroscopy, X-ray diffractometry, and $^{57}Fe$ Mossbauer spectroscopy. The samples were prepared from four parasite volcanos. These samples consist of the typical basalt comprised of $SiO_2,\;Al_2O_3$, Fe compounds, and silicate minerals. The $M{\ddot{o}}ssbauer$ spectra showed doublets for olivine, pyroxene, and ilmenite as well as sextets for hematite and magnetite. The valence state of Fe is chiefly a 3+ charge state with a little 2+ charge state. It is expected that this results will add to the body of information related to the information mechanism of Jeju island. The geochemistry for these samples is the same results to mid-mountain's samples in Jeju Island.

X-ray Induced Electron emission Spectroscopy

  • 송세안;이재철;최진학;김준홍;이재학;임창빈
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.191-191
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    • 1999
  • Extended X-ray Absorption Fine Structure (EXAFS)는 일반적으로 널리 사용하는 X선 회절분광기로 분석하기 힘든 chemical 또는 biological system의 structural analyses에 매우 유용한 분석방법이다. 특히 세라믹이나 유전체 비정질 재료의 미세 원자 구조에 관한 정보를 얻는데는 가장 강력한 분석방법중의 하나로 알려져 있다. 현재까지 대부분의 EXAFS 실험은 방사광 가속기를 이용하여 수행하였다. 그런데 신제품 개발의 순환주기가 급속하게 단축되는 현실적인 문제에 부응하기 위하여 실험실에서 EXAFS 실험을 수행할 수 있는 system을 개발하게 되었다. 개발한 XIEES 장비는 rotating anode 형의 18kW X-ray source, Optical system, Detection system, Stepping motor control system, vacuum system, Utility 등으로 구성하였다. Optical system에서의 6개의 Johanson type monochromator를 사용하여 분석가능한 x-ray energy range를 480eV에서 41keV까지 구현하였다. 이는 산소에서 우라늄까지 분석이 가능함을 의미하는 것으로, 산화물 연구에 많이 활용할 것으로 기대한다. XIEES는 투과 및 형광 X-ray를 검출할 수 있는 기능과 X-ray에 의해 여기 되는 모든(광전자, Aiger 전자, 이차전자)들을 검출할 수 있는 기능을 갖추고 있는데 이를 Total Electron Yield 측정이라고 한다. Total Electron Yield 측정은 박막 시료와 같이 투과가 되지 않는 시료를 분석할 뿐만 아니라, 경원소 분석, 낮은 에너지에서 흡수 edge가 나타나는 L-edge 측정을 통한 전자 구조 분석 등에 유용한다. 실험실용 XIEES 장비는 방사광가속기에 비해 x-ray flux가 크게 뒤지는 문제와 Total Electron Yield를 측정하는 데 있어서 source에서 나오는 x-ray beam이 진공용기 안에서 산란되어 이차전자를 여기하고 이 이차전자들이 전자검출기에 유입되어 측정에 영향을 미치는 background 문제 등이 있다. 이 두 가지 문제를 해결하기 위하여 Capillary tube를 사용하였다. 본 연구에서는 실험실용 XIEES 장비를 소개하고 이를 이용하여 Cu standard 시료에서 측정한 EXAFS 결과와 Capillary tube를 사용하여 얻은 x-ray flux 증진 및 background 제거 효과에 대해서 발표한다.

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Tribological Properties of Sputtered Boron Carbide Coating and the Effect of ${CH}_4$ Reactive Component of Processing Gas

  • Cuong, Pham-Duc;Ahn, Hyo-Sok;Kim, Jong-Hee;Shin, Kyung-Ho
    • KSTLE International Journal
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    • v.4 no.2
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    • pp.56-59
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    • 2003
  • Boron carbide thin coatings were deposited on silicon wafers by DC magnetron sputtering using a ${B}_4$C target with Ar as processing gas. Various amounts of methane gas (${CH}_4$) were added in the deposition process to better understand their influence on tribological properties of the coatings. Reciprocating wear tests employing an oscillating friction wear tester were performed to investigate the tribological behaviors of the coatings in ambient environment. The chemical characteristics of the coatings and worn surfaces were studied using X-ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES). It revealed that ${CH}_4$addition to Ar processing gas strongly affected the tribologcal properties of sputtered boron carbide coating. The coefficient of friction was reduced approximately from 0.4 to 0.1, and wear resistance was improved considerably by increasing the ratio of ${CH}_4$gas component from 0 to 1.2 vol %. By adding a sufficient amount of ${CH}_4$(1.2 %) in the deposition process, the boron carbide coating exhibited lowest friction and highest wear resistance.