• Title/Summary/Keyword: X-ray absorption spectroscopy

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Effect of BSO addition on Cu-O bond of GdBa2Cu3O7-x films with varying thickness probed by extended x-ray absorption fine structure

  • Jeon, H.K.;Lee, J.K.;Yang, D.S.;Kang, W.N.;Kang, B.
    • Progress in Superconductivity and Cryogenics
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    • v.18 no.4
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    • pp.1-4
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    • 2016
  • We investigated the relation between the Cu-O bond length and the superconducting properties of $BaSnO_3$ (BSO)-added $GdBa_2Cu_3O_{7-x}$ (GdBCO) thin films by using extended x-ray absorption fine structure (EXAFS) spectroscopy. 4 wt.% $BaSnO_3$ (BSO) added $GdBa_2Cu_3O_{7-x}$ (GdBCO) thin films with varying thickness from $0.2{\mu}m$ to $1.0{\mu}m$ were fabricated by using pulsed laser deposition (PLD) method. The transition temperature ($T_c$) and the residual resistance ratio (RRR) of the GdBCO films increased with increasing thickness up to $0.8{\mu}m$, where the crystalline BSO has the highest peak intensity, and then decreased. This uncommon behaviors of $T_c$ and RRR are likely to be created by the addition of BSO, which may change the ordering of GdBCO atomic bonds. Analysis from the Cu K-edge EXAFS spectroscopy showed an interesting thickness dependence of ordering behavior of BSO-added GdBCO films. It is noticeable that the ordering of Cu-O bond and the transition temperature are found to show opposite behaviors in the thickness dependence. Based on these results, the growth of BSO seemingly have evident effect on the alteration of the local structure of GdBCO film.

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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Preparation and Characterization of CdSe nanoparticle for Solar Cell application (태양전지용 CdSe 나노입자의 합성)

  • Kim, Shin-Ho;Park, Myoung-Guk;Lee, Bo-Ram;Lee, Hyun-Ju;Kim, Yang-Do
    • 한국신재생에너지학회:학술대회논문집
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    • 2007.11a
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    • pp.318-321
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    • 2007
  • CdSe nanoparticles were prepared by chemical solution methods using $CdCl_2{\cdot}4H_2O$ (or $Cd(NO_3)_ 2{\cdot}4H_2O$) and $Na_2SeSO_3$. The characteristics of CdSe nanoparticles were controlled by the react ion time, reaction temperature and reaction method as well as the surfactants. Cetyltrimethyl ammonium bromide(CTAB) was used as a capping agent to control the chemical reactions in aqueous solution. Polyvinylalcohol(PVA) was used as a templet in sono-chemical method. CdSe nanoparticles synthesized in aqueous solution showed homogeneous size distribution with relatively stable surface. CdSe nanoparticles synthesized in non-aqueous solution containing diethanolamine(DEA) showed the structure transformation from cubic to hexagonal as the reduction temperature increased from 80 to $160^{\circ}C$. Core shell CdSe was synthesized by sono-chemical method. Characteristics of CdSe nanoparticles were analyzed using transmission electron microscopy(TEM), x-ray photoelectron spectroscopy(XPS), x-ray diffraction(XRD), UV-Vis absorption spectra, fourier transform infrared spectroscopy(FT-IR) and photoluminescence spectra spectroscopy(PL). This paper presents simple routes to prepare CdSe nanoparticles for solar cell applications.

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Synthesis of Cd1-xZnxS/K4Nb6O17 Composite and its Photocatalytic Activity for Hydrogen Production

  • Liang, Yinghua;Shao, Meiyi;Liu, Li;Hu, Jinshan;Cui, Wenquan
    • Bulletin of the Korean Chemical Society
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    • v.35 no.4
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    • pp.1182-1190
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    • 2014
  • $Cd_{1-x}Zn_xS$-sensitized $K_4Nb_6O_{17}$ composite photocatalysts (designated $Cd_{1-x}Zn_xS/K_4Nb_6O_{17}$) were prepared via a simple deposition-precipitation method. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectrometry (EDS), $N_2$ sorption, ultraviolet-visible light diffuse reflectance spectroscopy (UV-Vis DRS), photoluminescence measurements (PL), and X-ray photoelectron spectroscopy (XPS). The $Cd_{0.8}Zn_{0.2}S$ particles were scattered on the surface of $K_4Nb_6O_{17}$, and had a relatively uniform size distribution around 50 nm. The absorption edge of $K_4Nb_6O_{17}$ was shifted to the visible light region and the recombination of photo-generated electrons and holes suppressed after $Cd_{0.8}Zn_{0.2}S$ loading. The $Cd_{0.8}Zn_{0.2}S$(25 wt %)/$K_4Nb_6O_{17}$ composite possessed the highest photocatalytic activity for hydrogen production under visible light irradiation, evolving 8.278 mmol/g in 3 h. Recyclability tests were performed, and the composite photocatalysts were found to be fairly stable. The mechanism of charge separation between the photogenerated electrons and holes at the $Cd_{0.8}Zn_{0.2}S/K_4Nb_6O_{17}$ composite was discussed.

Ag-modified BiOX (X=Cl, Br and I) Plates for Photocatalytic Dye Removal

  • Lee, Seung-Won;Choe, Yeong-In;Lee, Ju-Heon;Park, Yo-Han;Son, Yeong-Gu
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.424.2-424.2
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    • 2014
  • Ag-modified BiOX (X=Cl, Br and I) nanoplates were synthesized by an ion-exchange reaction. We examined the fundamental properties by scanning electron microscopy (SEM), electron transmission microscopy (TEM), X-ray diffraction, UV-visible absorption, Fourier-transform infrared and photoluminescence spectroscopy. The adsorption and photocatalytic performances of the catalysts were tested with dyes under UV and visible light. A chemical scavenger method was employed to test the roles of active species (${\cdot}OH$, ${\cdot}O2-$ and h+) and understand photodegradation mechanism. Photoluminescence spectroscopy was used to examine ${\cdot}OH$ radical formation using terephthalic acid during photoirradiation.

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Enhanced Photocatalytic Properties of Visible Light Responsive La/TiO2-Graphene Composites for the Removal of Rhodamin B in Water

  • Areerob, Yonrapach;Oh, Won-Chun
    • Journal of the Korean Chemical Society
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    • v.61 no.4
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    • pp.168-178
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    • 2017
  • $La/TiO_2$ - graphene composites were synthesized in this study, and applied to the photocatalytic degradation of Rhodamine B (RhB) under UV-visible light irradiation. X-ray diffraction (XRD), surface analysis, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) analysis demonstrated that $La/TiO_2$ nanoparticles were well distributed on the surface of graphene, and formed the heterostructure of $La/TiO_2$-graphene. Compared to the pure $TiO_2$, $La/TiO_2$-graphene composites displayed much higher photocatalytic activities in RhB degradation under UV-visible light irradiation. The photocatalytic data of $La/TiO_2$-graphene composites exhibit extended light absorption in the visible light region, and possess better charge separation capability than that of pure $TiO_2$. The high photocatalytic activity was attributed to the composite's high adsorptivity, extended light absorption, and increased charge separation efficiency, due to the excellent electrical properties of graphene, and the large surface contact between graphene and $La/TiO_2$ nanoparticles.

Correlation study on microstructure and mechanical properties of rice husk ash-Sodium aluminate geopolymer pastes

  • Singh, N. Shyamananda;Thokchom, Suresh;Debbarma, Rama
    • Advances in concrete construction
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    • v.11 no.1
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    • pp.73-80
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    • 2021
  • Rice Husk Ash (RHA) geopolymer paste activated by sodium aluminate were characterized by X-ray diffractogram (XRD), scanning electron microscope (SEM), energy dispersion X-Ray analysis (EDAX)and fourier transform infrared spectroscopy (FTIR). Five series of RHA geopolymer specimens were prepared by varying the Si/Al ratio as 1.5, 2.0, 2.5, 3.0 and 3.5. The paper focuses on the correlation of microstructure with hardened state parameters like bulk density, apparent porosity, sorptivity, water absorption and compressive strength. XRD analysis peaks indicates quartz, cristobalite and gibbsite for raw RHA and new peaks corresponding to Zeolite A in geopolymer specimens. In general, SEM micrographs show interconnected pores and loosely packed geopolymer matrix except for specimens made with Si/Al of 2.0 which exhibited comparatively better matrix. Incorporation of Al from sodium aluminate were confirmed with the stretching and bending vibration of Si-O-Si and O-Si-O observations from the FTIR analysis of geopolymer specimen. The dense microstructure of SA2.0 correlate into better performance in terms of 28 days maximum compressive strength of 16.96 MPa and minimum for porosity, absorption and sorptivity among the specimens. However, due to the higher water demand to make the paste workable, the value of porosity, absorption and sorptivity were reportedly higher as compared with other geopolymer systems. Correlation regression equations were proposed to validate the interrelation between physical parameters and mechanical strength. RHA geopolymer shows comparatively lower compressive strength as compared to Fly ash geopolymer.

Synthesis and spectroscopic characterization of zinc ferrite nanoparticles

  • Arora, Shefali;Nandy, Subhajit;Latwal, Mamta;Pandey, Ganesh;Singh, Jitendra P.;Chae, Keun H.
    • Advances in nano research
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    • v.13 no.5
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    • pp.437-451
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    • 2022
  • Synthesis approaches usually affect the physical and chemical properties of ferrites. This helps ferrite materials to design them for desired applications. Some of these methods are mechanical milling, ultrasonic method, micro-emulsion, co-precipitation, thermal decomposition, hydrothermal, microwave-assisted, sol-gel, etc. These methods are extensively reviewed by taking example of ZnFe2O4. These methods also affect the microstructure and local structure of ferrite which ultimately affect the physical and chemical properties of ferrites. Various spectroscopic techniques such as Raman spectroscopy, Fourier Transform Infrared spectroscopy, Ultra Violet-Visible spectroscopy, Mossbauer spectroscopy, extended x-ray absorption fine structure, and electron paramagnetic resonance are found helpful to reveal this information. Hence, the basic principle and the usefulness of these techniques to find out appropriate information in ZnFe2O4 nanoparticles is elaborated in this review.

Analyses on Fine Structure and Electronic Structure of Cr-doped Li4Ti5O12 by Using X-ray Absorption Spectroscopy and First Principle Calculation (X-선 흡수실험 및 제일원리계산을 통한 Cr-doped Li4Ti5O12의 미세구조 및 전자구조 해석)

  • Song, Han-Nah;Kim, Hyung-Sun;Cho, Byung-Won;Kim, Yong-Tae
    • Journal of the Korean Electrochemical Society
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    • v.14 no.1
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    • pp.33-37
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    • 2011
  • $Li_4Ti_5O_{12}$ has been considered a potential material for high power lithium batteries. Since $Li_4Ti_5O_{12}$ is however an insulator having a broad band gap, various methods have been employed to improve the conductivity. In this study, we have investigated the change of fine structure and electronic structure by Cr doping using X-ray absorption spectroscopy and First Principle Calculation. Doping with Cr, we could obtain an enhanced electronic conductivity by locating the Fermi level at the center position of Cr d-band and identify the change of XANES pre-edge and white line peak due to the increase of electron density of Ti d-band.

Iron(II) Tris(3-bromo-1,10-phenanthroline) Complex: Synthesis, Crystal Structure and Electropolymerization

  • Lee, Kyeong-Jong;Yoon, Il;Lee, Shim-Sung;Lee, Bu-Yong
    • Bulletin of the Korean Chemical Society
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    • v.23 no.3
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    • pp.399-403
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    • 2002
  • The complex of iron(II) tris(3-Br-phen) (3-Br-phen; 3-bromo-1,10-phenanthroline) was prepared as a precursor of electropolymerization and the crystal structure of [Fe(3-Br-phen)3]($PF_6$)2${\cdot}$CH3CN with a distorted octahedral geometry has been investigated. The reductive electropolymerization of $>[Fe(3-Br-phen)3]^{2+}$ complex onto the surface of a glassy carbon electrode and indium tin oxide (ITO) optically transparent electrode were performed in acetonitrile at room temperature. Thin film of poly-$>[Fe(3-Br-phen)3]^{2+}$ formed was adherent, electroactive and stably deposited on a glassy carbon disk electrode. The thin metallopolymeric film formed was also confirmed by absorption spectroscopy.