• 한국재료학회:학술대회논문집
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• 한국재료학회 2012년도 춘계학술발표대회
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• pp.70.1-70.1
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• 2012

In-situ X-ray photoelectron spectroscopy (XPS) and infrared (IR) spectroscopy studies of SOFC cathode materials will be discussed in this presentation. The mixed conducting perovskites (ABO3) containing rare and alkaline earth metals on the A-site and a transition metal on the B-site are commonly used as cathodes for solid oxide fuel cells (SOFC). However, the details of the oxygen reduction reaction are still not clearly understood. The information about the type of adsorbed oxygen species and their concentration is important for a mechanistic understanding of the oxygen incorporation into these cathode materials. XPS has been widely used for the analysis of adsorbed species and surface structure. However, the conventional XPS experiments have the severe drawback to operate at room temperature and with the sample under ultrahigh vacuum (UHV) conditions, which is far from the relevant conditions of SOFC operation. The disadvantages of conventional XPS can be overcome to a large extent with a "high pressure" XPS setup installed at the BESSY II synchrotron. It allows sample depth profiling over 2 nm without sputtering by variation of the excitation energy, and most importantly measurements under a residual gas pressure in the mbar range. It is also well known that the catalytic activity for the oxygen reduction is very sensitive to their electrical conductivity and oxygen nonstoichiometry. Although the electrical conductivity of perovskite oxides has been intensively studied as a function of temperature or oxygen partial pressure (Po2), in-situ measurements of the conductivity of these materials in contact with the electrolyte as a SOFC configuration have little been reported. In order to measure the in-plane conductivity of an electrode film on the electrolyte, a substrate with high resistance is required for excluding the leakage current of the substrate. It is also hardly possible to measure the conductivity of cracked thin film by electrical methods. In this study, we report the electrical conductivity of perovskite $La_{0.6}Sr_{0.4}CoO_{3-{\delta}}$ (LSC) thin films on yttria-stabilized zirconia (YSZ) electrolyte quantitatively obtained by in-situ IR spectroscopy. This method enables a reliable measurement of the electronic conductivity of the electrodes as part of the SOFC configuration regardless of leakage current to the substrate and cracks in the film.

• Bulletin of the Korean Chemical Society
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• 제34권4호
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• pp.1195-1198
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• 2013

Nickel hexacyanoferrate supported palladium nanoparticles (Pd-NiHCF NPs) were synthesized and studied for oxygen reduction reactions in direct methanol fuel cell. The NiHCF support was readily synthesized by a comixing of $Ni(OCOCH_3)_2$ and equimolar $K_3[Fe(CN)_6]$ solution into DI water under rigorous stirring. After the preparation of NiHCF support, Pd NPs were loaded on NiHCF via L-ascorbic acid reduction method at $80^{\circ}C$. Pd-NiHCF NPs were electrochemically active for oxygen reduction reaction in 0.1 M $HClO_4$ solution. X-ray absorption near edge structure analysis was conducted to measure the white line intensity of Pd-NiHCF to verify the OH adsorption. As a comparison, carbon supported Pd NPs exhibited same white line intensity. This study provides a general synthetic approach to easily load Pd NPs on porous coordination polymers such as NiHCF and can provide further light to load Pd based alloy NPs on NiHCF framework.

• 한국재료학회지
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• 제14권4호
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• pp.270-275
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• 2004

Due to the luminescence by$ Er ^{ 3+}$ activator, Er-doped $LaPO_4$ powders can be applied for optical amplification materials. In this study, $LaPO_4$:Er nanoparticles were synthesized in solution system using a high-boiling coordinating solvent and their properties were investigated through various spectroscopic techniques. The nanoparticles were to take a single phase of monazite structure by a X-ray diffraction analysis and to have the 5-6 nm of particles size with narrow size distribution by a TEM. And it was confirmed by the EA and FT-IR analyses that the surfaces of nanoparticles are coordinated with the solvent molecules, which will possibly keep from agglomerating between LaPO$_4$:Er nanoparticles. In the emission spectrum of $LaPO_4$:Er nanoparticle at NIR region, on the other hand, it was measured that the emission intensity is very weak, which is due to the transition from $^4$$I_{(13/2)}$ to $^4$$I_{(15/2)}$ of $Er^{3+ }$ion. It was interpreted that the weak luminescence of $LaPO_4$:Er is originated from the hydroxyl groups adsorbed on the surfaces of the nanoparticles, because OH group acts as an efficient quencher for the $^4$$I_{(13/2)}$ \longrightarrow $^4$$I_{(15/2)}$ emission of $Er^{3+}$ activator. But the co-doping of Yb$^{3+}$ as a sensitizer in this nanoparticle results in the increase of the emission intensity at 1539 nm due to the effective energy transfer from $Yb^{3+}$ to $Er^{3+}$ . In addition, the synthesized nanoparticles exhibited good dispersibility with some polymers and effective luminescence at NIR region.n.

• Macromolecular Research
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• 제16권8호
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• pp.725-733
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• 2008

Polyimide (PI) multilayer thin films were prepared by spin-coating from a poly(amic acid) (PAA) and poly(amic acid) ammonium salt (PAAS). PI was prepared from pyromellitic dianhydride (PMDA) and 4,4'-oxydianiline (ODA) PAA. Different compositions of PAAS were prepared by incorporating triethylamine (TEA) into PMDA-ODA PAA in dimethylacetamide. PI multilayer thin films were spin-coated from PMDA-ODA PAA and PAAS. The PAAS comprising cationic and anionic moieties were spherical with a particle size of $20{\sim}40\;nm$. Some particles showed layers with ammonium salts, despite poor ordering. Too much salt obstructed the interaction between the polymer chains and caused phase separation. A small amount of salt did not affect the interactions of the interlayer structure but did interrupt the stacking between chains. Thermogravimetric analysis (TGA) showed that the average decomposition temperature of the thin films was $611^{\circ}C$. All the films showed almost single-step, thermal decomposition behavior. The nanostructure of the multilayer thin films was confirmed by X -ray reflectivity (XRR). The LF 43 film, which was prepared with a 4:3 molar ratio of PMDA and ODA, was comprised of uniformly spherical PAAS particles that influenced the nanostructure of the interlayer by increasing the interaction forces. This result was supported by the atomic force microscopy (AFM) data. It was concluded that the relationship between the uniformity of the PAAS particle shapes and the interaction between the layers affected the optical and thermal properties of PI layered films.

• Bulletin of the Korean Chemical Society
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• 제32권1호
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• pp.49-52
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• 2011

A dinuclear copper(II) complex of [$Cu_2(aceace)_4$(dipyph)] [aceace = acetylacetone, dipyph = 1,4-di(4-pyridylethene-2-yl-)benzene] has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction. It crystallizes in the monoclinic system, space group P21/c, with lattice parameters a = 7.9584(16) $\AA$, b = 18.594(4) $\AA$, c = 15.063(4) $\AA$ $\beta=120.97(2)^o$ and $M_r$ = 807.85 ($C_{40}H_{44}Cu_2N_2O_8$), Z = 2. Each of the $Cu^{2+}$ ion adopts a square pyramid geometry and coordinates with four oxygen atoms from two aceace ligands and one nitrogen atom from dipyph bidentate ligand. Magnetic measurement shows that the Weiss constant and Curie constant for the title compound are -0.22 K and 0.1154 emu K/mol, respectively. Thermal stability data indicate that the title complex undergoes two steps decomposition and the residue is $Cu_2O_4$. In the potential range of -1.5 ~ 0.8 V, the title complex represents an irreversible electrochemical process.

• 한국세라믹학회지
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• 제53권6호
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• pp.659-664
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• 2016

Ash deposition of heat exchange boiler, caused mainly by accumulation of particulate matter, reduces heat transfer of the boiler system. Heat and mass transfer through porous media such as ash deposits mainly depend on the microstructure of deposited ash. Therefore, in this study, we investigated microstructural and thermal properties of the ash deposited on the boiler tube. Samples for this research were obtained from the fuel economizer tube in an industrial waste incinerator. To characterize microstructures of the ash deposit samples, scanning electron microscope (SEM), energy-dispersive spectroscopy (EDS), inductively coupled plasma optical emission spectroscopy (ICP-OES), X-ray diffraction (XRD) and BET analysis were employed. The results revealed that it had a porous structure with small particles mostly of less than a few micrometers; the contents of Ca and S were 19.3, 22.6% and 18.5, 18.7%, respectively. Also, the results showed that it consisted mainly of anhydrite ($CaSO_4$) crystals. - The thermal conductivities of the ash deposit sample obtained from the economizer tube in industrial waste incinerator were measured to be 0.63 and 0.54 W/mK at $200^{\circ}C$, which were about 100 times less than the thermal conductivity (61.32 W/mK) of the boiler tube itself, indicating that ash deposition on the boiler tube was closely related to a decrease in boiler heat transfer.

• 한국전기전자재료학회논문지
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• 제31권7호
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• pp.455-461
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• 2018

Boron nitride (BN) nanofibers were fabricated using BN nanoparticles (70 nm) by electrospinning. Morphologies such as the diameter and density of the BN nanofibers are strongly influenced by the viscosity and dispersion state of the precursor solution. In this study, the precursor solution was prepared by ball milling BN nanoparticles and polyvinylpyrrolidone (PVP, Mw~1,300,000) in ethanol, which was electrospun and then calcined to produce BN fibers. High-quality BN nanofibers were well fabricated at a BN concentration of 15 wt% with their diameters in the range of 500 nm to 800 nm; the viscosity of the precursor solution was $400mPa{\cdot}S$. The calcination of the as-electrospun BN fibers seemed to be completed by holding them at $350^{\circ}C$ for 2 h considering the TGA data. The morphologies and phases of the BN fibers were investigated by scanning electron microscopy (SEM) and X-ray diffractometry (XRD), respectively; Fourier transform infrared (FT-IR) was also used for structure analysis.

• 한국자기학회지
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• 제17권6호
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• pp.238-241
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• 2007

복합 전파흡수체로 사용할 Ni-Cu-Zn ferrite는 공침법을 사용하여 제조 하였고,제조 시편의 물리적 특성 및 전파흡수특성은 소결온도 변화에 따라 고찰하였다. Ni-Cu-Zn ferrite의 스피넬 구조는 XRD pattern을 통하며 확인하였다. 소결온도가 $1100^{\circ}C$에서 흡수 능력도 좋아짐을 알 수 있었으며, 소결된 페라이트의 초투자율은 평균 50 정도로 나타났다. $Ni_{0.7}Cu_{0.2}Zn_{0.1}Fe_2O_4$ 조성에서 소결 온도가 $1100^{\circ}C$ 일 때가 복합 전파흡수체로 사용할 조성임을 확인할 수 있었으며, 그 결과 복합 전파흡수체에서 사용할 수 있다고 사료된다.

• Elastomers and Composites
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• 제44권3호
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• pp.290-298
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• 2009

본 논문에서 Fe-활성탄소 섬유(ACF)/$TiO_2$ 복합체 광촉매를 졸-겔 방법에 의하여 제조하였다. 합성된 광촉매는 UV조사하에서 MB용액의 광분해에 사용되었다. BET 데이터는 Fe와 Ti의 여러 가지 농도를 가지고 처리된 ACF의 표면에서 흡착 특성을 보여준다. SEM 사진에서 보여지는 것처럼, 철 혼합물과 $TiO_2$는 ACF 표면에 활착되어 있음을 나타내었다. X선 분말 회절법으로부터 얻어진 결과는 복합체로부터 FeO+$TiO_2$, Anatase 및 Rutile 구조의 결정상을 나타내었다. 원소분석을 위한 EDX spectra는 Fe와 함께 C, O, Ti의 peak들이 존재함을 나타내었다. MB 분해에 대한 활성은 $TiO_2$의 광분해와 Fe의 photo-Fenton 효과로 인해 전자/hole쌍 반응으로부터 파생된 -OH 라디칼들에 의한 것으로 여겨진다.

• Bulletin of the Korean Chemical Society
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• 제33권4호
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• pp.1259-1263
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• 2012

Two metal compounds, $[Co(phen)_2(H_2O)_2]{\cdot}2H_2SIP{\cdot}2H_2O$ 1 and $[Ni(phen)_3]{\cdot}2H_2SIP{\cdot}3H_2O$ 2, have been obtained by incorporating 1,10-phenanthroline (phen) and 5-sulfoisophthalic acid monosodium salt ($NaH_2SIP$) ligands under hydrothermal conditions. Meanwhile, the two compounds were characterized by element analysis, IR, XRD, TG-DTA and single-crystal X-ray diffraction. Both 1 and 2 present 3D supramolecular structures via O-H${\cdots}$O hydrogen bond interactions. Luminescent properties for 1 and 2 were also studied. The compound 1 has two fluorescence emission peaks centered at 398 nm attributed to the intraligand emission from the SIP ligand and at 438 nm assigned to the combined interaction of intraligand ${\pi}^*-{\pi}$ transitions of the phen ligand and ligand-to-metal-charge-transfer (LMCT) transitions (${\lambda}_{ex}$ = 233 nm). The compound 2 shows one emission band centered at 423 nm with a shoulder peak at 434 nm which may be originated from the intraligand ${\pi}^*-{\pi}$ transitions of the phen ligand (${\lambda}_{ex}$ = 266 nm).