• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.193.1-193.1
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• 2014

This study was to investigate the electronic structure and optical properties of Na doped into NiO thin film using XPS and REELS. The films were grown by electron beam evaporation with varying the annealing temperature. The relationship between the electrical characteristics with the local structure of NiO thin films was also discussed. The x-ray photoelectron results showed that the Ni 2p spectra for all films consist of Ni 2p3/2 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 reflection electron energy loss spectroscopy spectra showed that the band gaps of the NiO thin films were slightly decreased with Na-doped into films. The Na-doped NiO showed relatively low resistivity compared to the undoped NiO thin films. In addition, the Na-doped NiO thin films deposited at room temperature showed the best properties, such as a p-type semiconducting with low electrical resistivity of $11.57{\Omega}.cm$ and high optical transmittance of ~80% in the visible light region. These results indicate that the Na doping followed by annealing process plays a crucial in enhancing the electrical and optical properties of NiO thin films. We believe that our results can be a good guide for those growing NiO thin films with the purpose of device applications, which require deposited at room temperature.

• 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.

• Korean Journal of Mineralogy and Petrology
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• v.36 no.4
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• pp.303-312
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• 2023

The determination of the oxidation states of metal elements in manganese nodules sheds light on the understanding of the formation mechanism of nodules, providing insights into the paleo-environmental conditions such as the redox potential of the aqueous system. This study aims to reveal the oxidation states and chemical bonding of manganese in the natural polymetallic nodules, utilizing conventional X-ray photoelectron spectroscopy (XPS). Specifically, shallow manganese nodules from the Siberian Arctic Sea, effectively recording mineralogical variations, were used in this study. Detailed analysis of XPS Mn 2p spectra showed changes in the manganese oxidation state from the center to the outer parts of the nodules. The central part of the nodules showed a higher Mn⁴⁺ content, approximately 67.9%, while the outermost part showed about 63% of Mn⁴⁺ due to an increase in the Mn³⁺+Mn²⁺. The decrease in the Mn oxidation state with the growth is consistent with the previously reported mineralogical variations from todorokite to birnessite with growth. Additionally, the O 1s spectra presented a predominance of Mn-O-H bonds in the outer layers compared to the center, suggesting hydration by water in the layered manganates of outer layers. The results of this study demonstrate that XPS can be directly applied to understand changes in paleo-environmental conditions such as the redox states during the growth of manganese nodules. Finally, future studies using high-resolution synchrotron-based XPS experiments could achieve details in oxidation states of manganese and trace metal elements.

• Journal of the Korean Ceramic Society
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• v.48 no.6
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• pp.559-564
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• 2011

In order to investigate the behavior of $SiO_2$ in the molybdenum silicide powders, crystal structure of these powders was measured by XRD, in addition, surface composition and surface phase (or chemical states) and microstructure were analysed by XPS and TEM, respectively. Mo-silicide powders containing $SiO_2$ were synthesized by SHS (Self-Propagating High-Temperature Synthesis) technique. In XRD result, according to increase of $SiO_2$ contents, the crystal structure for synthesized $MoSi_2$ powders was still typical $MoSi_2$ bct without any other phases. By XPS analysis, the surface of Mo and Si source powders was covered with $MoO_3$ and $SiO_2$, respectively, and the surface of synthesized $MoSi_2$ powder was also covered with $MoO_3$ and $SiO_2$, which were stable oxides at room temperature. However, according to increase of $SiO_2$ addition, $MoSi_2$ phase in XPS spectra decreased and $SiO_2$ phase increased relatively in synthesized $MoSi_2$ powders. From the results by XPS and XRD, we found that the existent $SiO_2$ has amorphous structure. In the microstructure, the small particulates of the synthesized products added $SiO_2$ agglomerated together to form larger clusters (from ~10 nm to ~1 ${\mu}m$). From TEM, XPS, and XRD results, we found that the out layer of agglomeration of synthesized $MoSi_2$ powder is surrounded by amorphous $SiO_2$.

• Economic and Environmental Geology
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• v.42 no.5
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• pp.479-486
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• 2009

In natural environments, manganese (Mn) exists in the valence of +2, +3, and +4 and plays a pivotal role as a strong oxidant or reductant in the geochemical cycles of elements. Especially, Mn forms varying (oxyhydr)oxides. The oxidation state of structural Mn is characteristic to each oxide and is one of the most important factors controlling its geochemical behaviors such as solubility, sorption capacity, and redox potential. Therefore, it is important to elucidate processes governing Mn oxidation state in predicting the fate and transport of many redox sensitive elements in the environment. X-ray photoelectron spectroscopy (XPS) is a very useful method to determine the oxidation state of various elements in solid phases. In this study, the oxidation states of structural Mn in MnO, $Mn_2O_3$, $MnO_2$ were assessed based on the binding energy spectra of $Mn2p_{3/2}$ and Mn3s using XPS and were compared with those reported elsewhere. $Mn2p_{3/2}$ binding energies were determined as 640.9, 641.5, 641.8 eV for MnO, $Mn_2O_3$, $MnO_2$, respectively, which indicates that the binding energy increased with increasing Mn oxidation state. It was also noted that Ar etching may cause changes in electronic structure configuration on surface of the original sample.

• Corrosion Science and Technology
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• v.5 no.4
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• pp.141-148
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• 2006

The chemical composition and the semiconducting properties of the passive films formed on Alloy 690 in various film formation conditions were investigated by XPS, photocurrent measurement, and Mott-Schottky analysis. The XPS and photocurrent spectra showed that the passive films formed on Alloy 690 in pH 8.5 buffer solution at ambient temperature, in air at $400^{\circ}C$, and in PWR condition comprise $Cr_2O_3$, $Cr(OH)_3$, ${\gamma}-Fe_2O_3$, NiO, and $Ni(OH)_2$. The thermally grown oxide in air and the passive film formed at high potential (0.3 $V_{SCE}$) in pH 8.5 buffer solution were highly Cr-enriched, whereas the films formed in PWR condition and that formed at low potential (-0.3 $V_{SCE}$) in pH 8.5 buffer solution showed relatively high Ni content and low Cr content. The Mott-Schottky plots exhibited n-type semiconductivity, inferring that the semiconducting properties of the passive films formed on Alloy 690 in various film formation conditions are dominated by Cr-substituted ${\gamma}-Fe_2O_3$. The donor density, i.e., concentration of oxygen vacancy, was measured to be $1.2{\times}10^{21}{\sim}4.6{\times}10^{21}cm^{-3}$ and lowered with increase in the Cr content in the passive film.

• Environmental Engineering Research
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• v.23 no.1
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• pp.1-9
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• 2018

The degradation of methylene blue (MB) in an aqueous solution by nano-metallic particles (NMPs) was studied to evaluate the possibility of applying NMPs to remove MB from the wastewater. Scanning electron microscopy (SEM), Fourier-transform infrared (FTIR) spectroscopy and X-ray photoelectron spectroscopy (XPS) were used to characterize the synthesized NMPs before and after the reaction. The effects of the NMP dosage, the initial pH, the initial concentration of MB and the amount of $H_2O_2$ on the MB degradation outcomes were studied. The highest removal rate of MB was achieved to be 100% with an initial MB concentration of 5 mg/L, followed by 99.6% with an initial concentration of 10 mg/L under the following treatment conditions: dose of NMP of 0.15 g/L, concentration of $H_2O_2-100mM$ and a temperature of $25^{\circ}C$. The SEM analysis revealed that the nano particles were not spherical in shape. FTIR spectra shows occurrence of metal oxides on the surfaces of the NMPs. The XPS analyses results represent that Fe, Zn, N, Ca, C and O were occurred on the surfaces of the NMPs. The degradation of MB was suitable for the pseudo-first-order kinetics.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.06a
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• pp.49-49
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• 2009

Nanocomposites of gold nanoparticles and multi-walled carbon nanotubes (MWNTs) were prepared by electrostatic interaction. Gold nanopartic1es were stabilized by polyvinylpyrrolidone (PVP), sodium dodecyl sulfate (SDS) and poly(sodium-4-styrenesulfonate) (PSS) in aqueous medium, and MWNTs were modified by poly(diallyldimethylammonium)chloride (PDDA) in water. The as-perpared Au-MWNT nanocomposites were structurally and electrically characterized by transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), UV/Vis spectroscopy, X-ray photoelectron spectroscopy (XPS) and cyclo voltammetry (CV). UV/Vis spectra of Au-MWNT nanocomposites showed the characteristic surface plasmon bands in the range of ~515nm, depending on the stabilizers. There is only slight change on the band shape with variation of stabilizing agents for gold nanoparticles. Through FE-SEM and TEM images, the distribution of gold, nanoparticles on the sidewalls of MWNTs was deliberately investigated on Au-MWNT nanocomposites treated with different stabilizers. XPS and CV showed redistribution of electron densities and changes in the binding energy states of nanopartic1es in nanocomposite respectively.

• 한국전기화학회:학술대회논문집
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• 2002.07a
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• pp.211-218
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• 2002

In this study, Pt/Pd (1.1), PtPd (2:1) and PtPd (3:1) binary catalysts and Pt/Ru/Pd (5:4:1) ternary catalyst were designed. The catalysts were synthesized by impregnation method using $NaBH_4$ as a reducing agent. A good catalyst for methanol oxidation requires low on-set potential, stable durability and low activation energy. In order to investigate the catalytic activity for the methanol oxidation, electrochemical measurements such as cyclic voltammetry and chronoamperometry were peformed in sulfuric acid with/without methanol solution. In order to calculate the activation energy of the reaction, electrochemical measurements were also tested at different temperatures. For investigation of the structural analysis such as particle size and alloying, X-ray diffraction and transmission electron microscopy analysis were used. In order to identify the role of the Pd and to determine the composition of the surface of the Pt/Pd nanoparticles, X-ray photoelectron spectroscopy (XPS) analysis was investigated. The XPS spectra of Pd showed that Pd appears only as a metallic state in the binary catalysts. The chemical states of Pt in PtPd catalysts are both metallic and oxidative. Polarization curves and power density data were obtained by testing the DMFC unit cell performance of PtPd and PtRuPd catalysts. These data showed that Pt/Pd (2:1) and Pt/Ru/Pd (5:4:1) have better performance than Pt and Pt/Ru, respectively.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.07b
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• pp.735-738
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• 2002

Single crystal 3C-SiC(cubic silicon carbide) thin-films were deposited on Si(100) substrate up to a thickness of $4.3{\mu}m$ by APCVD method using HMDS(hexamethyildisilane) at $1350^{\circ}C$. The HMDS flow rate was 0.5 sccm and the carrier gas flow rate was 2.5 slm. The HMDS flow rate was important to get a mirror-like crystal surface. The growth rate of the 3C-SiC films was $4.3{\mu}m/hr$. The 3C-SiC epitaxical films grown on Si(100) were characterized by XRD, AFM, RHEED, XPS and raman scattering, respectively. The 3C-SiC distinct phonons of TO(transverse optical) near $796cm^{-1}$ and LO(longitudinal optical) near $974{\pm}1cm^{-1}$ were recorded by raman scattering measurement. The heteroepitaxially grown films were identified as the single crystal 3C-SiC phase by XRD spectra$(2{\theta}=41.5^{\circ})$.