• Title/Summary/Keyword: X-ray Absorption Spectroscopy

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Crystallographic and Magnetic Properties of Brownmillerite Ca1-xSrxFeO2.5(x=0, 0.3, 0.5, 0.7, 1.0) (Brownmillerite Ca1-xSrxFeO2.5(x=0, 0.3, 0.5, 0.7, 1.0)의 결정학적 및 자기적 성질에 관한 연구)

  • Yoon, Sung-Hyun;Yang, Ju-Il;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.14 no.2
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    • pp.76-82
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    • 2004
  • Crystallographic and magnetic properties for Brownmillerite-type oxides $Ca_{1-x}$Sr$_{x}$FeO$_{2.5}$ (x = 0, 0.3, 0.5, 0.7, 1.0) were investigated using x-ray diffraction (XRD) and Mossbauer spectroscopy. Polycrystalline samples were prepared by conventional solid-state reaction method. Information on exact crystalline structures, lattice parameters, bond lengths and bond angles were obtained by refining their XRD profiles using a Rietveld method. The crystal structures were found to be all orthorhombic with space group Icmm (x = 0, 0.3) and Icmm (x = 0.5, 0.7, 1.0) The lattice parameters increased monotonically with increasing Sr concentration. Both the tetrahedral and the octahedral sites were considerably distorted and elongated along b-axis. While bond lengths and bond angles O-Fe-O tend to increase minutely with the increase of Sr content, bond angles Fe-O-Fe decreased accordingly. The Mossbauer spectra showed two sets of sharp sextets originating from ferric ions occupying the tetrahedral and the octahedral sites under the magnetic transition temperature T$_{N}$. Regardless of the compositions x, the electric quadrupole splittings were -0.3 mm/s and 0.4 mm/s for the octahedral and the tetrahedral site, respectively. Above T$_{N}$, the Mossbauer spectra showed the paramagnetic doublets whose electric quadrupole splittings were about 1.6 mm/s, irrespective of compositions x. T$_{N}$ was found to decrease monotonically with the increase of Sr concentration. Ratios of absorption area for the two sites were almost 1:1 up to as high as 0.95 T$_{N}$ for all x. The result of the Debye temperature indicated that the inter-atomic binding force for the Fe atoms in the tetrahedral site was stronger than that for the octahedral site.hedral site.

Effects of Anodic Voltages of Photcatalytic TiO2 and Doping in H2SO4 Solutions on the Photocatalytic Activity (광촉매 TiO2의 황산용액에서의 양극산화전압과 도핑이 광촉매 활성에 미치는 영향)

  • Lee, Seung-Hyun;Oh, Han-Jun;Chi, Choong-Soo
    • Korean Journal of Materials Research
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    • v.22 no.8
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    • pp.439-444
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    • 2012
  • To compare the photocatalytic performances of titania for purification of waste water according to applied voltages and doping, $TiO_2$ films were prepared in a 1.0 M $H_2SO_4$ solution containing $NH_4F$ at different anodic voltages. Chemical bonding states of F-N-codoped $TiO_2$ were analyzed using surface X-ray photoelectron spectroscopy (XPS). The photocatalytic activity of the co-doped $TiO_2$ films was analyzed by the degradation of aniline blue solution. Nanotubes were formed with thicknesses of 200-300 nm for the films anodized at 30 V, but porous morphology was generated with pores of 1-2 ${\mu}m$ for the $TiO_2$ anodized at 180 V. The phenomenon of spark discharge was initiated at about 98 V due to the breakdown of the oxide films in both solutions. XPS analysis revealed the spectra of F1s at 684.3 eV and N1s at 399.8 eV for the $TiO_2$ anodized in the $H_2SO_4-NH_4F$ solution at 180 V, suggesting the incorporation of F and N species during anodization. Dye removal rates for the pure $TiO_2$ anodized at 30 V and 180 V were found to be 14.0% and 38.9%, respectively, in the photocatalytic degradation test of the aniline blue solution for 200 min irradiation; the rates for the F-N-codoped $TiO_2$ anodized at 30 V and 180 V were found to be 21.2% and 65.6%, respectively. From the results of diffuse reflectance absorption spectroscopy (DRS), it was found that the absorption edge of the F-N-codoped $TiO_2$ films shifted toward the visible light region up to 412 nm, indicating that the photocatalytic activity of $TiO_2$ is improved by appropriate doping of F and N by the addition of $NH_4F$.

A STUDY OF ION BEAM ASSISTED DEPOSITION(IBAD) OF TiN ON Ni-Cr Be ALLOY FOR SURFACE CHARACTERISTIC (이온빔 보조 증착법에 의한 TiN 박막도포가 니켈-크롬-베릴륨 합금의 표면 성상에 미치는 영향에 관한 연구)

  • Choi, Soo-Young;Lee, Sun-Hyung;Chang, Ik-Tae;Yang, Jae-Ho;Chung, Hun-Young
    • The Journal of Korean Academy of Prosthodontics
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    • v.37 no.2
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    • pp.212-234
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    • 1999
  • Dental restorative materials must have the physical properties to withstand wear and corrosion. Base metal alloys possess better mechanical properties and lower price than the gold alloys. For these reasons such alloys have largely replaced the precious metal alloys. One aspect to con-sider is the release of metal substances to oral environment. The release of elements from dental alloys is a continuing concern because the elements may have the potentially harmful biological effects on local tissues. The purpose of this study was to minimize metal release on the nonprecious metal surfaces by ion beam assisted deposition(IBAD) of titanium nitride (TiN) Ni-Cr-Be alloys with and without TiN coatings were secured in an wear test machine opposing ruby ball to determine their relative resistance to wear with loom, 200m, 300m and 400m sliding distance. And the corrosion behavior of the Ni-Cr-Be alloys with and without TiN coatings and 3 dental noble alloys have been studied. Potentiodynamic curves were used to analyse the corrosion characteristics of the alloys. The measurement of the released Ni and Cr ions was conducted by analysis of the electrolyte solution with atomic absorption spectroscopy. The results were as follows : 1. The critical sliding distance that wore down TiN coatings of $2.5{\mu}m$ thickness in this study condition was 300m. 2. Ion beam assisted deposition of TiN showed a good surface modification with respect to the properties of wear and corrosion resistance. 3. X-ray diffraction showed that the strongest peak of TiN is TiN(111) in the coatings. 4. The release of Ni and Cr ions from alloys measured by means of atomic absorption spectroscopy was reduced by ion beam assisted deposition of TiN.

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Nanolayered CuWO4 Decoration on Fluorine-Doped SnO2 Inverse Opals for Solar Water Oxidation

  • Cho, Ha Eun;Yun, Gun;Arunachalam, Maheswari;Ahn, Kwang-Soon;Kim, Chung Soo;Lim, Dong-Ha;Kang, Soon Hyung
    • Journal of Electrochemical Science and Technology
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    • v.9 no.4
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    • pp.282-291
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    • 2018
  • The pristine fluorine-doped $SnO_2$ (abbreviated as FTO) inverse opal (IO) was developed using a 410 nm polystyrene bead template. The nanolayered copper tungsten oxide ($CuWO_4$) was decorated on the FTO IO film using a facile electrochemical deposition, subsequently followed by annealing at $500^{\circ}C$ for 90 min. The morphologies, crystalline structure, optical properties and photoelectrochemical characteristics of the FTO and $CuWO_4$-decorated FTO (briefly denoted as $FTO/CuWO_4$) IO film were investigated by field emission scanning electron microscopy, X-ray diffraction, UV-vis spectroscopy and electrochemical impedance spectroscopy, showing FTO IO in the hexagonally closed-pack arrangement with a pore diameter and wall thickness of about 300 nm and 20 nm, respectively. Above this film, the $CuWO_4$ was electrodeposited by controlling the cycling number in cyclic voltammetry, suggesting that the $CuWO_4$ formed during 4 cycles (abbreviated as $CuWO_4$(4 cycles)) on FTO IO film exhibited partial distribution of $CuWO_4$ nanoparticles. Additional distribution of $CuWO_4$ nanoparticles was observed in the case of $FTO/CuWO_4$(8 cycles) IO film. The $CuWO_4$ layer exhibits triclinic structure with an indirect band gap of approximately 2.5 eV and shows the enhanced visible light absorption. The photoelectrochemical (PEC) behavior was evaluated in the 0.5 M $Na_2SO_4$ solution under solar illumination, suggesting that the $FTO/CuWO_4$(4 cycles) IO films exhibit a photocurrent density ($J_{sc}$) of $0.42mA/cm^2$ at 1.23 V vs. reversible hydrogen electrode (RHE, denoted as $V_{RHE}$), while the FTO IO and $FTO/CuWO_4$(8 cycles) IO films exhibited a $J_{sc}$ of 0.14 and $0.24mA/cm^2$ at $1.23V_{RHE}$, respectively. This difference can be explained by the increased visible light absorption by the $CuWO_4$ layer and the favorable charge separation/transfer event in the cascading band alignment between FTO and $CuWO_4$ layer, enhancing the overall PEC performance.

A Study on the Electron Transfer at the Alq3/Ba and Alq3/Au Interfaces by NEXAFS Spectroscopy (NEXAFS 분광법에 의한 Alq3/Ba과 Alq3/Au의 계면에서의 전자 천이에 관한 연구)

  • Lim, Su-Yong;Ju, Sung-Hoo;Yang, Jae-Woong
    • Journal of Surface Science and Engineering
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    • v.45 no.1
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    • pp.15-19
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    • 2012
  • Tris(8-quinolinolato)aluminum(III); $Alq_3$ has been frequently used as an electron transporting layer in organic light-emitting diodes. Either Ba with a low work function or Au with a high work function was deposited on $Alq_3$ layer in vacuum. And then, the behaviors of electron transition at the $Alq_3$/Ba and $Alq_3$/Au interfaces were investigated by using the near edge x-ray absorption fine structure (NEXAFS) spectroscopy. In the each interface, the energy levels of unoccupied obitals were assigned as ${\pi}^*$(LUMO, LUMO+1, LUMO+2 and LUMO+3) and ${\sigma}^*$. And the relative intensities of these peaks were investigated. In an oxygen atom composing $Alq_3$ molecule, the relative intensities for a transition from K-edge to LUMO+2 were largely increased as Ba coverage (${\Theta}_{Ba}$, 2.7 eV) with a low work function was in-situ sequentially increased on $Alq_3$ layer. In contrast, the relative intensities for the LUMO+2 peak were reduced as Au coverage (${\Theta}_{Au}$, 5.1 eV) with a high work function were increased on $Alq_3$ layer. This means that the electron transition by photon in oxygen atom which consists in the unoccupied orbitals in $Alq_3$ molecule, largely depends on work function of a metal. Meanwhile, in the case of electron transition in a carbon atom, as ${\Theta}_{Ba}$ was increased on $Alq_3$, the relative intensity from K-edge to ${\pi}_1{^*}$ (LUMO and LUMO+1) was slightly decreased, and from K-edge to ${\pi}_2{^*}$ (LUMO+2 and LUMO+3) was somewhat increased. This rising of the energy state from ${\pi}_1{^*}$ to ${\pi}_2{^*}$ exhibits that electrons provided by Ba would contribute to the process of electron transition in the $Alq_3$/Ba interfaces. As shown in above observation, the analyses of NEXAFS spectra in each interface could be important as a basic data to understand the process of electron transition by photon in pure organic materials.

Crystallographic and Magnetic Properties of Li0.5Fe2.5-χRhχO4 by Using Applied Field Mossbauer Spectrometer (외부자기장 뫼스바우어 분광기를 이용한 Li0.5Fe2.5-χRhχO4의 자기적 성질과 결정학적 구조에 관한 연구)

  • Kang, Kun-Uk;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.14 no.6
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    • pp.219-223
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    • 2004
  • L $i_{0.5}$F $e_{2.5-{\chi}}$R $h_{\chi}$ $O_4$ ($\chi$ = 0.25, 0.50, 0.75, 1.00) has been prepared by solid state reaction. Crystallographic and magnetic properties were investigated by Mossbauer spectroscopy, SQUID magnetometry, and x-ray diffraction. The crystal structure is found to be a cubic spinel structure with space group Fd3m for all the samples. The lattice constant $a_{0}$ increases from 8.3365 $\AA$ to 8.3932 $\AA$ with increasing Rh concentration $\chi$. The migration of Li ion has been confirmed by x-ray patterns and the results of applied field Mossbauer analysis. The temperature dependence of the absorption area of each site was analyzed with the Debye model for the recoil-free fraction. The Debye temperature for the octahedral sites is almost as large as for the tetrahedral sites, thereby suggesting similar inter-atomic binding forces for the octahedral and the tetrahedral sites. The saturated magnetic moment and the Mossbauer spectra taken at 4.2 K under the applied field (6 T) show that the spin structure of L $i_{0.5}$F $e_{2.5-{\chi}}$R $h_{\chi}$ $O_4$ is compatible with the collinear Neel Model.

The impact of municipal waste disposal of heavy metals on environmental pollution: A case study for Tonekabon, Iran

  • Azizpour, Aziz;Azarafza, Mohammad;Akgun, Haluk
    • Advances in environmental research
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    • v.9 no.3
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    • pp.175-189
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    • 2020
  • Municipal solid waste disposal is considered as one of the most important risks for environmental contamination which necessitates the development of strategies to reduce destructive consequences on the ecosystem as related especially to heavy metal accumulation. This study investigates heavy metal (i.e., As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Zn) accumulation in the Tonekabon region, NW of Iran that is related to city waste disposal and evaluates the environmental impact in the Caspian Sea coastal region. For this purpose, after performing field studies and collecting 50 soil specimens from 5 sites of the study area, geochemical tests (i.e., inductively coupled plasma mass spectrometry, atomic absorption spectroscopy and x-ray fluorescence) were conducted on the soil specimens collected from the 5 sites (named as Sites A1, A2, A3, A4 and A5) and the results were used to estimate the pollution indices (i.e., geo-accumulation index, normalized enrichment factor, contamination factor, and pollution load index). The obtained indices were utilized to assess the eco-toxicological risk level in the landfill site which indicated that the city has been severely contaminated by Cu, Mn, Ni, Pb and Zn. These levels have been developed along the stream towards the nearshore areas indicating uptake of soil degradation. The heavy metal contamination was classified to range from unpolluted to highly polluted, which indicated serious heavy metal pollution in the study area as related to municipal solid waste disposal in Tonekabon.

TiO2/Carbon Composites Prepared from Rice Husk and the Removal of Bisphenol A in Photocatalytic Liquid System

  • Kim, Ji-Yeon;Kwak, Byeong-Sub;Kang, Mi-Sook
    • Bulletin of the Korean Chemical Society
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    • v.31 no.2
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    • pp.344-350
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    • 2010
  • The improved photocatalytic performance of a carbon/$TiO_2$ composite was studied for the Bisphenol A (BPA) decomposition. Titanium tetraisopropoxide (TTIP) and a rice husk from Korea were heterogeneously mixed as the titanium and carbon sources, respectively, for 3 h at room temperature, and then thermally treated at $600^{\circ}C$ for 1 h in $H_2$ gas. The transmission electron microscopy (TEM) images revealed that the bulk carbon partially covered the $TiO_2$ particles, and the amount that was covered increased with the addition of the rice husk. The acquired carbon/$TiO_2$ composite exhibited an anatase structure and a novel peak at $2{\theta}=32^{\circ}$, which was assigned to bulk carbon. The specific surface area was significantly enhanced to 123~164 $m^2/g$ in the carbon/$TiO_2$ composite, compared to $32.43m^2/g$ for the pure $TiO_2$. The X-ray photoelectron spectroscopy (XPS) results showed that the Ti-O bond was weaker in the carbon/$TiO_2$ composite than in the pure $TiO_2$, resulting in an easier electron transition from the Ti valence band to the conduction band. The carbon/$TiO_2$ composite absorbed over the whole UV-visible range, whereas the absorption band in the pure$TiO_2$ was only observed in the UV range. These results agreed well with an electrostatic force microscopy (EFM) study that showed that the electrons were rapidly transferred to the surface of the carbon/$TiO_2$ composite compared to the pure $TiO_2$. The photocatalytic performance of the BPA removal was optimized at a Ti:C ratio of 9.5:0.5, and this photocatalytic composite completely decomposed 10.0 ppm BPA after 210 min, whereas the pure $TiO_2$ achieved no more than 50% decomposition under any conditions.

Aerosol-gel synthesis of ZnO quantum dots dispersed in SiO2 matrix and their characteristics (에어로솔-젤 법을 이용한 SiO2에 분산된 ZnO 양자점의 합성과 그 특성)

  • Kim, Sang-Gyu;Firmansyah, Dudi Adi;Lee, Kwang-Sung;Lee, Donggeun
    • Particle and aerosol research
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    • v.6 no.2
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    • pp.51-59
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    • 2010
  • ZnO quantum dots embedded in a silica matrix without agglomeration were synthesized from $TEOS:Zn(NO_3)_2$ solutions in one-step process by aerosol-gel method. It was successfully demonstrated that the size of ZnO Q-dots could be controlled from 2 to 7 mm verified by a high resolution transmission electron microscope observation. The line scanning energy dispersive X-ray spectroscopy(EDS) revealed that the Q-dots existed preferentially inside SiO2 sphere when Zn/Si < 0.5. However, the Q-dots distributed homogeneously all over the sphere when Zn/Si > 1.0. Blue-shifted UV/Vis absorption peak observation confirmed the quantum size effect on the optical properties. The photoluminescence(PL) emission peaks of the powders at room temperature were consistent with previous reports in the following aspects: 1) PL characteristics are dominated by two peaks of deep-level defect-related emissions at 2.4 - 2.8 eV, 2) the first defect-related peak at 2.4 eV was blue shifted due to the quantum size effect with decreasing the concentration of $Zn(NO_3)_2$(decreasing the size of ZnO q dots). More interestingly, the existence of surface-exposed ZnO q dots affects greatly the second defect PL peak at 2.8 eV.

Surface Impregnation of Glycine to Activated Carbon Adsorbents for Dry Capture of Carbon Dioxide

  • Lim, Yun Hui;Adelodun, Adedeji A.;Kim, Dong Woo;Jo, Young Min
    • Asian Journal of Atmospheric Environment
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    • v.10 no.2
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    • pp.99-113
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    • 2016
  • In order to improve the portability of basic absorbents monoethanolamine (MEA) and glycine (Gly), both were supported on microporous activated carbon (AC). Chemical modification by alkali-metal ion exchange (of Li, Na, K) was carried out on Gly-based absorbents. All supported absorbents were subjected to $CO_2$ absorption capacity (pure $CO_2$) and selectivity (indoor level) tests. Textural and chemical characterizations were carried out on test sorbents. All impregnation brought about significant reduction of specific surface area and microporosity of the adsorbent Depreciation in the textural properties was found to result to reduction in pure $CO_2$ sorption. Contrarily, low-level $CO_2$ removal capacity was enhanced as the absorbent dosage increases, resulting in supported 5 molar MEA in methanol solution. Adsorption capacities were improved from 0.016 and 0.8 in raw ACs to 1.065 mmol/g for MEA's. Surface chemistry via X-ray photoelectron spectroscopy (XPS) of the supported sorbents showed the presence of amine, pyrrole and quaternary-N. In reducing sequence of potency, pyridine, amine and pyrrolic-N were noticed to contribute significantly to $CO_2$ selective adsorption. Furthermore, the adsorption isotherm study confirms the presence of various SNGs heterogeneously distributed on AC. The adsorption mechanism of the present AC adsorbents favored Freundlich and Langmuir isotherm at lower and higher $CO_2$ concentrations respectively.