• Proceedings of the Korean Vacuum Society Conference
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• 2009.08a
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• pp.177-177
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• 2009

• Proceedings of the Korean Vacuum Society Conference
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• 2009.08a
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• pp.176-176
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• 2009

• Bulletin of the Korean Chemical Society
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• v.31 no.12
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• pp.3675-3678
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• 2010

In-situ X-ray absorption spectroscopy (XAS) was used to elucidate the structural variation of $\alpha-MoO_3$ electrode upon discharge/charge reaction in a lithium ion battery. According to the XAS analysis, hexavalent Mo atoms in $\alpha-MoO_3$ framework are reduced as the amount of intercalated lithium ions increases. As lithium de-intercalation proceeds, most of pre-edge peaks are restored again. However, according to the Fourier transforms of the extended X-ray absorption fine structure (EXAFS) spectra, lithium de-intercalation reaction is partially irreversible upon the charge reaction, which is one of the main reasons why the capacity of $\alpha-MoO_3$ electrode decreases upon successive discharge/charge cycles.

• Bulletin of the Korean Chemical Society
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• v.19 no.1
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• pp.5-21
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• 1998

The purpose of this paper is to show that X-ray absorption spectroscopy (XANES and EXAFS) is a powerful technique for characterizing both crystalline and amorphous solids from structural (local order) and electronic point of view. The principle of this technique is briefly described by showing the main factors which must be considered for recording and fitting the experimental results. Some non-trivial examples have been selected for demonstrating that XAS spectroscopy is the only technique for bringing a definitive answer as for example: the determination of the local distortion of the $NiO_6$ octahedra in the $Li_{1-z}Ni_{1+z}O_2$ layered oxides and the evidence of the presence of copper pairs in the NASICON-type phosphate $CuZr_2 (PO_4)_3$. Are also reported some significant examples for which XAS spectroscopy is decisive with other characterization methods as (i) Raman spectroscopy for glasses (ii) Mossbauer spectroscopy for $LiNi_{1+z-t}Fe_To_2$ oxides (iii) magnetic measurements for Ce-based intermetallic compounds.

• Bulletin of the Korean Chemical Society
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• v.19 no.9
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• pp.947-951
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• 1998

$K_2NiF_4$-type layered compounds of the ($C_nH_{2n+1}NH_3)_2SnCl_4$ (n=2, 4, 6, 8, and 10) system have been synthesized from a stoichiometric mixture of $SnCl_2$ and alkyl ammonium salt using a low temperature solution technique under the inert atmosphere condition. Their crystal structures are assigned to the orthorhombic system by X-ray powder diffraction analysis. The a and b cell parameters show small changes. However, the c parameter is varied significantly according to the increment of alkyl chains of the organic layer which is located between inorganic layers in the compounds. The conformational phase transitions of the compounds are studied by the DSC in the temperature range of 300 to 500 K. FT-IR and Raman spectra are analyzed in the ranges of 1300 to 4000 cm-1 and of 50 to 360 $cm^{-1}$ with Ar-laser (λ=514.5 nm) excitation, respectively. Photoluminescence phenomena are observed for some compounds. The bond-length of Sn-Cl is determined by the EXAFS spectroscopic analysis.

• Bulletin of the Korean Chemical Society
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• v.21 no.10
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• pp.1049-1051
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• 2000

A chromia-pillared clay has been prepared by ion exchange type intercalation reaction between the sodium ion in montmorillonite and the trimeric chromium oxyformate (TCF) ion, and by subsequent heat-treatment. The structural and thermal properties have been systematically studied by thermal analysis, powder XRD, IR spec-troscopy, and XAS. The gallery height of~6.8 $\AA$ upon intercalation of the TCF ion suggests that the $Cr_3O$ plane is parallel to the aluminosilicate layers. Even though the basal spacing of TCF intercalated clay decreases slightly upon heating, the layer structure was retained up to $550^{\circ}C$ as confirmed by XRD and TG/DTA. Ac-cording to the EXAFS spectroscopic analysis, it is identified that the (Cr-Cr) distance of 3.28 $\AA$ between vertex-linked CrO6 octahedra in TCF splits into 2.64 $\AA$, 2.98 $\AA$, and 3.77 $\AA$ due to the face-, edge-, and corner-shared CrO6 octahedra after heating at $400^{\circ}C$, implying that a nano-sized chromium oxide phase was stabilized within the interlayer space of clay.

• Bulletin of the Korean Chemical Society
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• v.20 no.12
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• pp.1394-1398
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• 1999

The structures of modified Ti$(OPr^i)_4$ with chelating ligands (L) such as ethylacetoacetate (Etac), acetylacetone (Acac) and methylacetoacetate (Mtac) were identified by using IR, ¹H NMR and $^13C$ NMR spectroscopies, and the octahedral structure was confirmed after modification. The pre-edge peaks of XANES spectra of modified metal alkoxides also denoted the mixture of five-fold and six-fold structures. The EXAFS fitting results showed the local structure around Ti atom after alkoxide modification. The hydrolysis-condensation rates of modified Ti alkoxide with organic additives were investigated by ¹H NMR spectroscopy. The Ti$(OPr^i)_4$ modified by Acac was less reactive toward hydrolysis-condensation reaction than those modified by the other alkoxides, which can be attributed to the stable ligand structure between Ti$(OPr^i)_4$ and Acac. The small particle size of modified Ti$(OPr^i)_4$ sol was obtained when Acac was employed.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.397-397
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• 2013

The electrical, electronic, optical properties and the local structure of Nickel Oxide (NiO) thin film have been investigated by X-ray photoelectron spectroscopy (XPS), Reflection Electron Energy Loss Spectroscopy (REELS), UV-spectrometer,Hall Effect measurement and X-ray absorption spectroscopy (XAS). The XPS results show that the Ni 2p spectra for all films consist of $Ni2p_{3/2}$ at around 854.5 eV which indicate the presence of Ni-O bond from NiO phase and for the annealed film at temperature above $200^{\circ}C$ shows the coexist Ni oxide and Ni metal phase. The REELS spectra showed that the band gaps of the NiO thin films were abruptly decreased with increasing temperature. The values of the band gaps are consistent with the optical band gaps estimated by UV-Spectrometer. The optical transmittance spectra shows that the transparency of NiO thin films in the visible light region was deteriorated with higher temperature due to existence of $Ni^0$. Hall Effect measurement suggest that the NiO thin films prepared at relatively low temperatures (RT and $100^{\circ}C$) are suitable for fabricating p-type semiconductor which showed that the best properties was achieved at $100^{\circ}C$, such as a low resistivity of $7.49{\Omega}.cm$. It can be concluded that the annealing process plays a crucial role in converting from p type to n type semiconductor which leads to reducing electrical resistivity of NiO thin films. Furthermore, the extended X-ray absorption fine structure (EXAFS) spectrum at the Ni K-edge was used to address the local structure of NiO thin films. It was found that the thermal treatments increase the order in the vicinity of Ni atom and lead the NiO thin films to bunsenite crystal structure. Moreover, EXAFS spectra show in increasing of coordination number for the first Ni-O shell and the bond distance of Ni-O with the increase of substrate temperature.

• Journal of the Korean Chemical Society
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• v.43 no.6
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• pp.636-643
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• 1999

Green-emission intensity of a $Zn_{2-x}Mn_xSiO_4$ phosphor, which is a potential candidate as a green component in PDP device, significantly increases provided that the compound is additionally heat treated at 900$^{\circ}C$ after solid state reaction at 1300$^{\circ}C$. In order to verify origin of such an intensity enhancement after the additional heat treatment in association with the electronic and local structural change at around Mn ions, the Mn K-edge X-ray absorption spectra were recorded. From the analyses of the preedge peak corresponding to $1s{\rightarrow}3d$ bound state transition and XANES spectrum, it is known that most Mn ions are in +2 oxidation state and substitute Zn ion site regardless of the thermal treatment. In addition, EXAFS analyses revealed that Mn ions formed $MnO_4$ tetrahedra with the Mn-O bond length shortened by 0.01${\AA}$ and with reduced Debye-Waller factor in the thermally treated sample.

• Korean Chemical Engineering Research
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• v.49 no.1
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• pp.1-9
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• 2011

Platinum catalysts were prepared by impregnating platinum precursor on titania-, vanadia-, zirconia- and ceria-incorporated silicas followed by hydrogen peroxide treatment. The effects of the oxide incorporation and the hydrogen peroxide treatment in the preparation of the platinum catalysts on their platinum dispersion and catalytic activity in carbon monoxide oxidation were investigated. XRD, TEM, EXAFS, XPS and carbon monoxide chemisorption studies confirmed the high dispersion of platinum even on silica by the oxide incorporation and hydrogen peroxide treatment. However, the type of oxides incorporated on silica caused considerable variances in the adsorption and the catalytic activity in the oxidation of carbon monoxide on them. The incorporation of titania, zirconia and ceria on silica and further hydrogen peroxide treatment enhanced the platinum dispersion, resulting in the improved catalytic activities. Among the catalysts supported on the oxide-incorporated silicas, the platinum catalyst supported on zirconia-incorporated silica exhibited the highest activity because of the highest platinum dispersion due to the formation of Pt-O-Zr bonds.