• 제목/요약/키워드: XAFS

검색결과 26건 처리시간 0.021초

Graphene Based Cu Oxide Nanocomposites for C-N Cross Coupling Reaction

  • Choi, Jong Hoon;Park, Joon B.
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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    • pp.138.2-138.2
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    • 2013
  • Copper oxide is a multi-functional material being used in various research areas including catalysis, electrochemical materials, oxidizing agents etc. Among these areas, we have synthesized and utilized graphene based copper oxide nanocomposites (CuOx/Graphene) for the catalytic applications (C-N cross coupling reaction). Briefly, Cu precursors were anchored on the graphite oxide(GO) sheets being exfoliated and oxidized from graphite powder. Two different crystalline structures of Cu2O and CuO on graphene and GO were prepared by annealing them in Ar and O2 environments, respectively. The morphological and electronic structures were systemically investigated using FT-IR, XRD, XPS, XAFS, and TEM. Here, we demonstrate that the catalytic performance was found to depend on oxidative states and morphological structures of CuOx graphene nanocomposites. The relationship between the structure of copper oxides and catalytic efficiency toward C-N cross coupling reaction will be discussed.

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The New X-ray Induced Electron Emission Spectrometer

  • Yu.N.Yuryev;Park, Hyun-Min;Lee, Hwack-Ju;Kim, Ju-Hwnag;Cho, Yang-Ku;K.Yu.Pogrebitsky
    • 한국결정학회:학술대회논문집
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    • 한국결정학회 2002년도 정기총회 및 추계학술연구발표회
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    • pp.5-6
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    • 2002
  • The new spectrometer for X-ray Induced Electron Emission Spectroscopy (XIEES) .has been recently developed in KRISS in collaboration with PTI (Russia). The spectrometer allows to perform research using the XAFS, SXAFS, XANES techniques (D.C.Koningsberger and R.Prins, 1988) as well as the number of techniques from XIEES field(L.A.Bakaleinikov et all, 1992). The experiments may be carried out with registration of transmitted through the sample x-rays (to investigate bulk samples) or/and total electron yield (TEY) from the sample surface that gives the high (down to several atomic mono-layers in soft x-ray region) near surface sensitivity. The combination of these methods together give the possibility to obtain a quantitative information on elemental composition, chemical state, atomic structure for powder samples and solids, including non-crystalline materials (the long range order is not required). The optical design of spectrometer is made according to Johannesson true focusing schematics and presented on the Fig.1. Five stepping motors are used to maintain the focusing condition during the photon energy scan (crystal angle, crystal position along rail, sample goniometer rail angle, sample goniometer position along rail and sample goniometer angle relatively of rail). All movements can be done independently and simultaneously that speeds up the setting of photon energy and allows the using of crystals with different Rowland radil. At present six curved crystals with different d-values and one flat synthetic multilayer are installed on revolver-type monochromator. This arrangement allows the wide range of x-rays from 100 eV up to 25 keV to be obtained. Another 4 stepping motors set exit slit width, sample angle, channeltron position and x-ray detector position. The differential pumping allows to unite vacuum chambers of spectrometer and x-ray generator avoiding the absorption of soft x-rays on Be foil of a window and in atmosphere. Another feature of vacuum system is separation of walls of vacuum chamber (which are deformed by the atmospheric pressure) from optical elements of spectrometer. This warrantees that the optical elements are precisely positioned. The detecting system of the spectrometer consists of two proportional counters, one scintillating detector and one channeltron detector. First proportional counter can be used as I/sub 0/-detector in transmission mode or by measuring the fluorescence from exit slit edge. The last installation can be used to measure the reference data (that is necessary in XANES measurements), in this case the reference sample is installed on slit knife edge. The second proportional counter measures the intensity of x-rays transmitted through the sample. The scintillating detector is used in the same way but on the air for the hard x-rays and for alignment purposes. Total electron yield from the sample is measured by channeltron. The spectrometer is fully controlled by special software that gives the high flexibility and reliability in carrying out of the experiments. Fig.2 and fig.3 present the typical XAFS spectra measured with spectrometer.

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Combustion Generated Fine Particles, Trace Metal Speciation, and Health Effects

  • Linak, William P.
    • 한국대기환경학회:학술대회논문집
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    • 한국대기환경학회 2003년도 추계학술대회 논문집
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    • pp.195-195
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    • 2003
  • Combustion generated fine particles, defined as those with aerodynamic diameters less than 2.5 m, have come under increased regulatory scrutiny because of suspected links to adverse human health effects. Transition metals are of particular interest due to the results of a number of studies that have shown cardiopulmonary damage associated with exposure to these elements and their presence in coal, residual fuel oils, sewage sludge, and other combusted fuels and wastes. This lecture will review results from multi-di sciplinary studies being conducted at EPA and elsewhere examining the physical, chemical, and toxicological characteristics of combustion generated particles. The research describes how collaborative work between combustion engineers and health scientists can provide insight on how combustion processes affect particle properties and subsequent health effects as measured by a combination of in-vitro and in-vivo studies using a variety of animal models. The focus of this lecture is on the interdisciplinary approach required to address the problem. Difficulties are discussed. Engineering aspects involved in this approach are described in detail. Physical and chemical characterizations are performed using a variety of analytical approaches including new techniques of x-ray absorption fine structure (XAFS) spectroscopy and x-ray absorption near-edge structure (XANES) deconvolution of these spectra to gather metal speciation information.

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Amorphous Vanadium Titanates as a Negative Electrode for Lithium-ion Batteries

  • Lee, Jeong Beom;Chae, Oh. B.;Chae, Seulki;Ryu, Ji Heon;Oh, Seung M.
    • Journal of Electrochemical Science and Technology
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    • 제7권4호
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    • pp.306-315
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    • 2016
  • Amorphous vanadium titanates (aVTOs) are examined for use as a negative electrode in lithium-ion batteries. These amorphous mixed oxides are synthesized in nanosized particles (<100 nm) and flocculated to form secondary particles. The $V^{5+}$ ions in aVTO are found to occupy tetrahedral sites, whereas the $Ti^{4+}$ ions show fivefold coordination. Both are uniformly dispersed at the atomic scale in the amorphous oxide matrix, which has abundant structural defects. The first reversible capacity of an aVTO electrode ($295mAhg^{-1}$) is larger than that observed for a physically mixed electrode (1:2 $aV_2O_5$ | $aTiO_2$, $245mAhg^{-1}$). The discrepancy seems to be due to the unique four-coordinated $V^{5+}$ ions in aVTO, which either are more electron-accepting or generate more structural defects that serve as $Li^+$ storage sites. Coin-type Li/aVTO cells show a large irreversible capacity in the first cycle. When they are prepared under nitrogen (aVTO-N), the population of surface hydroxyl groups is greatly reduced. These groups irreversibly produce highly resistive inorganic compounds (LiOH and $Li_2O$), leading to increased irreversible capacity and electrode resistance. As a result, the material prepared under nitrogen shows higher Coulombic efficiency and rate capability.

In situ Structural Investigation of Iron Phthalocyanine Monolayer Adsorbed on Electrode Surface by X-ray Absorption Fine Structure

  • 김성현;;강광훈
    • Bulletin of the Korean Chemical Society
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    • 제21권6호
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    • pp.588-594
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    • 2000
  • Structural changes of an iron phthalocyanine (FePC) monolayer induced by adsorption and externally applied potential on high area carbon surface have been investigated in situ by iron K-edge X-ray absorption fine structure (XAFS) in 0.5 M $H_2S0_4.$ Fine structures shown in the X-ray absorption near edge structure (XANES) for microcrystalline FePC decreased upon adsorption and further diminished under electrochemical conditions. Fe(II)PC(-2) showed a 1s ${\rightarrow}$ 4p transition as poorly resolved shoulder to the main absorption edge rather than a distinct peak and a weak 1s ${\rightarrow}$ 3d transition. The absorption edge position measured at half maximum was shifted from 7121.8 eV for Fe(lI)PC(-2) to 7124.8 eV for $[Fe(III)PC(-2)]^+$ as well as the 1s ${\rightarrow}$ 3d pre-edge peak being slightly enhanced. However, essentially no absorption edge shift was observed by the 1-electron reduction of Fe(Il)PC(-2), indicating that the species formed is $[Fe(II)PC(-3)]^-$. Structural parameters were obtained by analyzing extended X-ray absorption fine structure (EXAFS) oscillations with theoretical phases and amplitudes calculated from FEFF 6.01 using multiple-scattering theory. When applied to the powder FePC, the average iron-to-phthalocyanine nitrogen distance, d(Fe-$N_p$) and the coordination number were found to be 1.933 $\AA$ and 3.2, respectively, and these values are the same, within experimental error, as those reported ( $1.927\AA$ and 4). Virtually no structural changes were found upon adsorption except for the increased Debye-Wailer factor of $0.005\AA^2$ from $0.003\AA^2.$ Oxidation of Fe(II)PC(-2) to $[Fe(III)PC(-2)]^+$ yielded an increased d(Fe-Np) (1 $.98\AA)$ and Debye-Wailer factor $(0.005\AA^2).$ The formation of $[Fe(II)PC(-3)]^-$, however, produced a shorter d(Fe-$N_p$) of $1.91\AA$ the same as that of crystalline FePC within experimental error, and about the same DebyeWaller $factor(0.006\AA^2)$.

Eco-Friendly Light Emitting Diodes Based on Graphene Quantum Dots and III-V Colloidal Quantum Dots

  • Lee, Chang-Lyoul
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2015년도 제49회 하계 정기학술대회 초록집
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    • pp.65-65
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    • 2015
  • In this talk, I will introduce two topics. The first topic is the polymer light emitting diodes (PLEDs) using graphene oxide quantum dots as emissive center. More specifically, the energy transfer mechanism as well as the origin of white electroluminescence in the PLED were investigated. The second topic is the facile synthesis of eco-friendly III-V colloidal quantum dots and their application to light emitting diodes. Polymer (organic) light emitting diodes (PLEDs) using quantum dots (QDs) as emissive materials have received much attention as promising components for next-generation displays. Despite their outstanding properties, toxic and hazardous nature of QDs is a serious impediment to their use in future eco-friendly opto-electronic device applications. Owing to the desires to develop new types of nanomaterial without health and environmental effects but with strong opto-electrical properties similar to QDs, graphene quantum dots (GQDs) have attracted great interest as promising luminophores. However, the origin of electroluminescence (EL) from GQDs incorporated PLEDs is unclear. Herein, we synthesized graphene oxide quantum dots (GOQDs) using a modified hydrothermal deoxidization method and characterized the PLED performance using GOQDs blended poly(N-vinyl carbazole) (PVK) as emissive layer. Simple device structure was used to reveal the origin of EL by excluding the contribution of and contamination from other layers. The energy transfer and interaction between the PVK host and GOQDs guest were investigated using steady-state PL, time-correlated single photon counting (TCSPC) and density functional theory (DFT) calculations. Experiments revealed that white EL emission from the PLED originated from the hybridized GOQD-PVK complex emission with the contributions from the individual GOQDs and PVK emissions. (Sci Rep., 5, 11032, 2015). New III-V colloidal quantum dots (CQDs) were synthesized using the hot-injection method and the QD-light emitting diodes (QLEDs) using these CQDs as emissive layer were demonstrated for the first time. The band gaps of the III-V CQDs were varied by varying the metal fraction and by particle size control. The X-ray absorption fine structure (XAFS) results show that the crystal states of the III-V CQDs consist of multi-phase states; multi-peak photoluminescence (PL) resulted from these multi-phase states. Inverted structured QLED shows green EL emission and a maximum luminance of ~45 cd/m2. This result shows that III-V CQDs can be a good substitute for conventional cadmium-containing CQDs in various opto-electronic applications, e.g., eco-friendly displays. (Un-published results).

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