• 제목/요약/키워드: X-ray Absorption Spectroscopy

검색결과 337건 처리시간 0.034초

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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    • 제9권4호
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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.

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

  • 임수용;주성후;양재웅
    • 한국표면공학회지
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    • 제45권1호
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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.

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

  • 강건욱;김철성
    • 한국자기학회지
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    • 제14권6호
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    • pp.219-223
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    • 2004
  • L $i_{0.5}$F $e_{2.5-{\chi}}$Rhx $O_4$($\chi$= 0.25, 0.50, 0.75, 1.00)을 직접합성법으로 제조하고, 시료의 조성비에 따른 자기적 성질과 결정학적 구조를 연구하였다. x선 회절실험분석 결과 시료 모두 공간군 Fd3m에 해당하는 입방 스피넬구조를 가졌고, Rh을 치환함에 따라 Li이온이 팔면체 자리에서 사면체 자리로의 이동이 나타났다. 시료의 격자상수는 Rh을 치환함에 따라 8.3365 $\AA$에서 8.3932 $\AA$으로 증가하였다. Neel 온도 이하에서 외부자기장을 가하지 않은 상태에서의 뫼스바우어 스펙트림과 외부자기장 (6 T)을 인가한 뫼스바우머 스펙트럼을 여러 온도에 대하여 취하여 미시적 자성구조를 측정하였다. 외부자기장하의 뫼스바우어 스펙트럼 분석으로 각 시료의 정확한 면적비를 계산하여 수행한 Debye온도 분석결과 전체 시료에서 사면체와 팔면체 자리가 비슷한 정도의 결합 세기를 가졌음을 알았다. $\chi$=0.75의 경우는 외부자기장하에서 사면체와 팔면체 자리의 초미세 자기장의 부호가 바뀌는 것을 알았고, 이는 Li ion의 자리이동과 일치하는 결과를 보인다 4.2K에서 극저온 하에서 6 T를 인가한 외부자기장의 스펙트럼분석으로 전체 시료의 자기적 스핀구조가 collinear spin 모형을 따름을 알 수 있었다.

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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    • 제9권3호
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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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    • 제31권2호
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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.

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

  • 김상규;;이광승;이동근
    • 한국입자에어로졸학회지
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    • 제6권2호
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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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    • 제10권2호
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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.

M ssbauer 효과에 의한 제주도 찰흙의 함철 광물의 열적 거동과 상변환에 관한 연구 (A Study on the Thermal Behavior and Phase Transformation of Iron-bearing Minerals in Clay of Cheju Island by M ssbauer Effect)

  • 강동우;김두철;류재연;고정대;홍성락;송관철
    • 한국광물학회지
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    • 제10권2호
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    • pp.148-161
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    • 1997
  • Based on the X-ray powder diffraction (XRD) and M ssbauer spectroscopy, the thermal behavior and phase transformations of two clays are investigated for raw and fired conditions, which are collected from Kwangryeongli and Ildo district in Cheju Island. M ssbauer spectra at room temperature and 20for two clays show that paramagnetic Fe3- is the structural iron of the layer silicate and ferrihydrite, and superparamagnetic goethite has about 50% of total iron contents. The XRD peaks of hematite for the fired clays appear from 80$0^{\circ}C$ in Kwangryeongli clay and from $600^{\circ}C$ in Ildo district clay, respectively. The structural Fe2+ was completely oxidized into Fe3- at 40$0^{\circ}C$ for Kwangryeongli clay and 50$0^{\circ}C$~$600^{\circ}C$ for Ildo district clay, respectively. The structural Fe2+ was completely oxidized into Fe3- at 40$0^{\circ}C$. For the temperature ranging from 40$0^{\circ}C$ to $700^{\circ}C$~80$0^{\circ}C$, two fired clays exhibit the dehydroxylation of the clay mineral. A disintegration of the clay mineral structure is observed from $700^{\circ}C$~80$0^{\circ}C$ to 110$0^{\circ}C$, followed by the onset and spread of vitrification process. It is also shown that well-crystallized hematite phase is formed at the temperature higher than 110$0^{\circ}C$ and the relative absorption area decreases, which might be related to the recrystallization of alluminosilicate matrix.

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알루미나가 11Å Tobermorite의 수열합성에 미치는 영향 (Influence of Alumina on Hydrothermal Synthesis of 11Å Tobermorite)

  • 임굉;임재석
    • 한국재료학회지
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    • 제15권2호
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    • pp.97-105
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    • 2005
  • [ $11\AA$ ] tobermorite$(5CaO{\cdot}6SiO_2{\cdot}5H_2O)$ is synthesized from the mixtures of calcium hydroride and quartz using alumina in a molar ratio $Ca(OH)_2/SiO_2$ of 0.8 at $180^{\circ}C$ for 8 and 24 hrs under saturated steam pressure. The influence of alumina on the formation of $11\AA$ tobermorite was investigated by X-ray diffraction, differential thermal analysis and infrared spectroscopy. $11\AA$ tobermorite containing increasingly larger amounts of aluminum showed a shift of the basal spacing from 11.3 to $11.6\AA$. In general, there was a direct linear relation between the basal spacing and added content of alumina. The differential thermal analysis curves showed that $11\AA$ tobermorite with increasing alumina contents exhibited the exothermic peak at high temperature, namely $11\AA$ tobermorite containing aluminum gave a sharp exothermic peak at temperature around $850\~860^{\circ}C$ in the case of $S_3\~S_5$. The absorption band at $1607\~1620cm^{-1}$ is attributed to the bending vibration of water, and the position of the main O-H stretching and Si-O lattice vibration of $11\AA$ tobermorite at 3500 and $965cm^{-1}$ respectively is not altered. Consequently the existence of alumina accelerates the crystallization of $11\AA$ tobermorite, and that the aluminum ion appears to substitute for the silicon ion in $11\AA$ tobermorite structure. Al-containing tobermorite is distinguished from Al-free tobermorite.

Cr(III)-Tetraaza Macrocyclic Complexes Containing Auxiliary Ligands (Part IV); Synthesis and Characterization of Cr(III)-Acetylacetonato, -Malonato and -Oxalato Macrocyclic Complexes

  • Byun, Jong-Chul;Han, Chung-Hun
    • Bulletin of the Korean Chemical Society
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    • 제26권9호
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    • pp.1395-1402
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    • 2005
  • The reaction of cis-[Cr([14]-decane)$(OH)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = acetylacetonate (acac), oxalate (ox) or malonate (mal)} leads to a new cis-[Cr([14]-decane)(acac)]$(ClO_4)_2{\cdot}(1/2)H_2O\;(1),\;cis-[Cr([14]-decane)(ox)]ClO_4{\cdot}(1/2)H_2O\;(2)\;or\;cis-[Cr([14]-decane)(mal)]ClO_4{\cdot}(1/4)H_2O\;(3)$. These complexes have been characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[Cr([14]-decane)(acac)]$(ClO_4)_2{\cdot}(1/2)H_2O$ reveals that central chromium(III) has a distorted octahedral coordination environment and two acetylacetonate-oxygen atoms are bonded to the chromium(III) ion in the cis positions. The angle $N_{axial}-Cr-N_{axial}$ deviates by $11^{\circ}$ from the ideal value of $180^{\circ}$ for a perfect octahedron. The bond angle O-Cr-O between the chromium(III) ion and the two acetylacetonate-oxygen atoms is close to $90^{\circ}$. The bond lengths of Cr-O between the chromium and the acetylacetonate-oxygen atoms are 1.950(3) and 1.954(2) $\AA$. They are shorter than those between chromium and nitrogen atoms of the macrocycle. The IR spectra of 1, 2 and 3 display bands at 1560 {ν (C=O)}, 1710 {${\nu}_{as}$(OCO)} and 1660 $cm^{-1}$ {${\nu}_{as}$(OCO)} attributed to the acac, ox and mal auxiliary ligands stretching vibrations, respectively.