• Bulletin of the Korean Chemical Society
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• 제18권10호
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• pp.1061-1066
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• 1997

The complexes M(CO)4-1,2-(PPh2)2-1,2-C2B10H10 (M=Cr 2a, Mo 2b, W 2c) have been prepared in good yields from readily available bis-diphenylphosphino-o-carboranyl ligand, closo-1,2-(PPh2)2-1,2-C2B10H10 (1), by direct reaction with Group Ⅵ metal carbonyls. The infrared spectra of the complexes indicate that there is an octahedral disposition of chelate bis-diphenylphosphino-o-carboranyl ligand around the metal atom. The crystal structure of 2a was determined by X-ray diffraction. Complex 2a crystallizes in the monoclinic space group P21/n with cell parameters a = 12.2360(7), b = 17.156(1), c = 16.2040(6) Å, V = 3354.1(3) Å3, and Z =4. Of the reflections measured a total of 2514 unique reflections with F2 > 3σ(F2) was used during subsequent structure refinement. Refinement converged to R1 = 0.066 and R2 = 0.071. Structural studies showed that the chromium atom had a slightly distorted pseudo-octahedral configuration about the metal center with two phosphine groups of o-carborane occupying the equatorial plane cis-orientation to each other. These metal carbonyl complexes are rapidly converted to the corresponding metal carbene complexes, [(CO)3M=C(OCH3)(CH3)]-1,2-(PPh2)2-1,2-C2B10H10 (M= Cr 3a, Mo 3b, W 3c), via alkylation with methyllithium followed by O-methylation with CF3SO3CH3.

• 한국건설순환자원학회논문집
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• 제9권3호
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• pp.367-374
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• 2021

본 연구는 기계·화학적 에너지를 활용하는 메카노케미칼 공정기술을 자기치유 혼화재에 적용하기 위한 목적으로 진행되었다. 기계·화학적 공정기술을 자기치유 혼화재 제조 공정에 적용하여 치유 소재의 활성화 에너지를 증가시켜 치유성능에 미치는 영향을 확인하고자 하였다. 자기치유 모르타르에 사용한 자기치유 소재는 팽창/팽윤제를 주요 구성물로 선정하고 탄산염 촉진제와 무기염 첨가제를 기타 첨가제로 혼입하였으며, 기계·화학 처리공정 적용에 의한 치유 소재의 활성화도 및 개질화 반응이 가능한 재료로 선택하였다. 기계·화학 처리공정에 대한 자기치유 혼화재의 기초평가는 XRD, FT-IR 분석으로 확인하였으며, 자기치유 모르타르의 치유 성능평가는 정수위 투수시험을 이용하여 치유율을 확인하였다. 치유성능 확인결과 기계·화학 처리 공정을 적용한 WM3 시료(MC360min)가 공정처리 하지 않은 WM1 시료에 대비 치유성능이 4.1% 증가하였으며, 자기치유율은 평균 94.3%로 확인되었다.

• 한국분말재료학회지
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• 제26권1호
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• pp.49-57
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• 2019

Layered $LiNi_{0.83}Co_{0.11}Mn_{0.06}O_2$ cathode materials single- and dual-doped by the rare-earth elements Ce and Nd are successfully fabricated by using a coprecipitation-assisted solid-phase method. For comparison purposes, non-doping pristine $LiNi_{0.83}Co_{0.11}Mn_{0.06}O_2$ cathode material is also prepared using the same method. The crystal structure, morphology, and electrochemical performances are characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) mapping, and electrochemical techniques. The XRD data demonstrates that all prepared samples maintain a typical ${\alpha}-NaFeO_2$-layered structure with the R-3m space group, and that the doped samples with Ce and/or Nd have lower cation mixing than that of pristine samples without doping. The results of SEM and EDS show that doped elements are uniformly distributed in all samples. The electrochemical performances of all doped samples are better than those of pristine samples without doping. In addition, the Ce/Nd dual-doped cathode material shows the best cycling performance and the least capacity loss. At a 10 C-rate, the electrodes of Ce/Nd dual-doped cathode material exhibit good capacity retention of 72.7, 58.5, and 45.2% after 100, 200, and 300 cycles, respectively, compared to those of pristine samples without doping (24.4, 11.1, and 8.0%).

• 한국분말재료학회지
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• 제26권1호
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• pp.40-44
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• 2019

Tungsten trioxide ($WO_3$) is a promising candidate as a photocatalyst because of its outstanding electrical and optical properties. In this study, we prepare $WO_3$ thin films by electrodeposition and characterize the photocatalytic degradation of methylene blue using these films. Depending on the voltage conditions (static and pulse), compact and porous $WO_3$ films are fabricated on a transparent ITO/glass substrate. The morphology and crystal structure of electrodeposited $WO_3$ thin films are investigated by scanning electron microscopy, atomic force microscopy, and X-ray diffraction. An application of static voltage during electrodeposition yields a compact layer of $WO_3$, whereas a highly porous morphology with nanoflakes is produced by a pulse voltage process. Compared to the compact film, the porous $WO_3$ thin film shows better photocatalytic activities. Furthermore, a much higher reaction rate of degradation of methylene blue can be achieved after post-annealing of $WO_3$ thin films.

• 한국재료학회지
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• 제29권8호
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• pp.469-476
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• 2019

A lead-free bulk ceramic having a chemical formula $Ba_{0.8}Ca_{0.2}(Ti_{0.8}Zr_{0.1}Ce_{0.1})O_3$ (further termed as BCTZCO) is synthesized using mixed oxide route. The structural, dielectric, impedance, and conductivity properties, as well as the modulus of the synthesized sample are discussed in the present work. Analysis of X-ray diffraction data obtained at room temperature reveals the existence of some impurity phases. The natural surface morphology shows close packing of grains with few voids. Attempts have been made to study the (a) effect of microstructures containing grains, grain boundaries, and electrodes on impedance and capacitive characteristics, (b) relationship between properties and crystal structure, and (c) nature of the relaxation mechanism of the prepared samples. The relationship between the structure and physical properties is established. The frequency and temperature dependence of the dielectric properties reveal that this complex system has a high dielectric constant and low tangent loss. An analysis of impedance and related parameters illuminates the contributions of grains. The activation energy is determined for only the high temperature region in the temperature dependent AC conductivity graph. Deviation from the Debye behavior is seen in the Nyquist plot at different temperatures. The relaxation mechanism and the electrical transport properties in the sample are investigated with the help of various spectroscopic (i.e., dielectric, modulus, and impedance) techniques. This lead free sample will serve as a base for device engineering.

• 한국환경과학회지
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• 제28권6호
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• pp.561-570
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• 2019

A zeolitic material (Z-Y2) was synthesized from Coal Fly Ash (CFA) using a fusion/hydrothermal method under low-alkali condition (NaOH/CFA = 0.6). The adsorption performance of the prepared zeolite was evaluated by monitoring its removal efficiencies for Sr and Cs ions, which are well-known as significant radionuclides in liquid radioactive waste. The XRD (X-ray diffraction) patterns of the synthesized Z-Y2 indicated that a Na-A type zeolite was formed from raw coal fly ash. The SEM (scanning electron microscope) images also showed that a cubic crystal structure of size $1{\sim}3{\mu}m$ was formed on its surface. In the adsorption kinetic analysis, the adsorption of Sr and Cs ions on Z-Y2 fitted the pseudo-second-order kinetic model well, instead of the pseudo-first-order kinetic model. The second-order kinetic rate constant ($k_2$) was determined to be $0.0614g/mmol{\cdot}min$ for Sr and $1.8172g/mmol{\cdot}min$ for Cs. The adsorption equilibria of Sr and Cs ions on Z-Y2 were fitted successfully by Langmuir model. The maximum adsorption capacity ($q_m$) of Sr and Cs was calculated as 1.6846 mmol/g and 1.2055 mmol/g, respectively. The maximum desorption capacity ($q_{dm}$) of the Na ions estimated via the Langmuir desorption model was 2.4196 mmol/g for Sr and 2.1870 mmol/g for Cs. The molar ratio of the desorption/adsorption capacity ($q_{dm}/q_m$) was determined to be 1.44 for Na/Sr and 1.81 for Na/Cs, indicating that the amounts of desorbed Na ions and adsorbed Sr and Cs ions did not yield an equimolar ratio when using Z-Y2.

• 한국분말재료학회지
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• 제28권5호
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• pp.423-428
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• 2021

Here, we report the development of a new and low-cost core-shell structure for lithium-ion battery anodes using silicon waste sludge and the Ti-ion complex. X-ray diffraction (XRD) confirmed the raw waste silicon sludge powder to be pure silicon without other metal impurities and the particle size distribution is measured to be from 200 nm to 3 ㎛ by dynamic light scattering (DLS). As a result of pulverization by a planetary mill, the size of the single crystal according to the Scherrer formula is calculated to be 12.1 nm, but the average particle size of the agglomerate is measured to be 123.6 nm. A Si/TiO₂ core-shell structure is formed using simple Ti complex ions, and the ratio of TiO₂ peaks increased with an increase in the amount of Ti ions. Transmission electron microscopy (TEM) observations revealed that TiO₂ coating on Si nanoparticles results in a Si-TiO₂ core-shell structure. This result is expected to improve the stability and cycle of lithium-ion batteries as anodes.

• Bulletin of the Korean Chemical Society
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• 제9권6호
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• pp.345-349
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• 1988

The polycrystalline powder of (CaLa) (MgMo)$O_6$ has been prepared at $1350^{\circ}C$ in $H_2/H_2O$ and $N_2$ flowing atmosphere. The powder X-ray diffraction pattern indicates that (CaLa) (MgMo)$O_6$ has a monoclinic perovskite structure with the lattice constants $a_0=b_0=7.901(1){\AA}$, $c =7.875(1){\AA}\;and\;{\gamma}=89^{\circ}$16'(1'), which can be reduced to orthorhombic unit cell, a = 5.551(1) ${\AA}$, b = 5.622(1) ${\AA}$ and c = 7.875(1) ${\AA}$. The infrared spectrum shows two strong absorption bands with their maxima at 590($ν_3$) and 380($ν_4$) cm, which are attributed to $2T_{1u}$ modes indicating the existence of highly charged molybdenum octahedron $MoO_6$ in the crystal lattice. According to the magnetic susceptibility measurement, the compound follows the Curie-Weiss law below room temperature with the effective magnetic moment 1.83(1)$_{{\mu}B}$, which is well consistent with that of spin only value (1.73 $_{\mu}_B$) for $Mo^{5+}$ with $4d^1$-electronic configuration within the limit of experimental error. From the thermogravimetric analysis, it has been confirmed that (CaLa) (MgMo)$O_6$ decomposes gradually into $CaMoO_4,\;MoO_3,\;MgO,\;La_2O_3$ and unidentified phases due to the oxidation of $Mo^{5+}$ to $Mo^{6+}$.

• Current Applied Physics
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• 제18권12호
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• pp.1571-1576
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• 2018

Recent study shows that the main reason for limiting CZTS device performance lies in the low open circuit voltage, and crucial factor that could affect the $V_{oc}$ is secondary phases like ZnS existing in absorber layer and its interfaces. In this work, the $Cu_2ZnSnS_4$ thin film solar cells were prepared by sputtering CuSn and CuZn alloy targets. Through tuning the Zn/Sn ratios of the CZTS thin films, the crystal structure, morphology, chemical composition and phase purity of CZTS thin films were characterized by X-Ray Diffraction (XRD), scanning electron microscopy (SEM) equipped with an energy dispersive spectrometer (EDS) and Raman spectroscopy. The statistics data show that the CZTS solar cell with a ratio of Zn/Sn = 1.2 have the best power convention efficiency of 5.07%. After HCl etching process, the CZTS thin film solar cell with the highest efficiency 5.41% was obtained, which demonstrated that CZTS film solar cells with high efficiency could be developed by sputtering CuSn and CuZn alloy targets.

• 대한금속재료학회지
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• 제47권9호
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• pp.586-590
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• 2009

The effects of additives on the surface morphology and physical properties of copper electrodeposited on polyimide(PI) film were investigated here. Two kinds of additives, an activator(additive A) and a leveler(additive B),were used in this study. Electrochemical experiments, in conjunction with scanning electron microscopy(SEM), X-ray diffraction(XRD) and a four-point probe, were performed to characterize the morphology and mechanical characteristics of copper electrodeposited in the presence of the additives. The surface roughness, crystal growth orientation and resistivity could be controlled using various quantities of additive B. High resistivity and lower peel strength were observed on the surface of the copper layer electroplated onto the electrolyte with no additive B. However, a uniform surface, lower resistivity and high flexibility were obtained with a combination of 20 ppm of additive A and 100 ppm of additive B.