• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 1998년도 추계학술대회 논문집
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• pp.175-178
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• 1998

LiMn$_2$O$_4$-based spinels has been studied extensively as positive electrode materials for rechargeable lithium and lithium ion batteries. We describe here that LiMn$_2$O$_4$ cathode active materials is preparated by sol-gel process using water as solvent, which often yields inorganic oxides of excellent phase purity and well-controlled stoichiometry. Using this process, it has been possible to synthesize phase-pure crystalline spinel LiMn$_2$O$_4$ by calcining the appropriate precursors in air at 80$0^{\circ}C$ for several hours. The influence of different time have also been explored. LiMn$_2$O$_4$ preparated in the present study exhibit the single phase of cubic and active reaction at 400 ~ $600^{\circ}C$. Electrochemical studies show that the this method- synthesized materials appear to present reversible oxidation and reduction reactions at 3.0V ~ 4.5V and cycle stability during 50 cycle.

• 한국표면공학회지
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• 제49권2호
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• pp.191-195
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• 2016

Among the lithium metal oxides for hybrid-capacity, $Li_4Ti_5O_{12}(LTO)$ is an emerging electrode material as zero-stain material in volume change during the with the charging and discharging processes. However, LTO has a limitation of low ionic and electronic conductivity. To enhance the ionic and electronic properties of $Li_4Ti_5O_{12}(LTO)$, we synthesized the spherical LTO/CNT composite by sol-gel process for hybrid capacitors. CNT interconnection networks between CNT-LTO particles enhanced electronic conductivity and electrochemical charging/discharging properties. All of the LTO samples was observed to show the spinel structure and spherical morphology with the diameter of $5{\sim}10{\mu}m$. Especially, spherical LTO/CNT composite of the CNT-3 wt% showed the enhanced capacity from 110 mAh/g to 140 mAh/g at 10 C.

• Korean Chemical Engineering Research
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• 제57권5호
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• pp.701-705
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• 2019

알칼라인 조건에서의 산소발생 반응(oxygen-evolution reaction: OER)은 다양한 에너지 시스템에 중요한 반응으로 여겨지고 있다. 큰 overpotential을 감소시키기 위해 다양한 촉매들이 개발되고 있으며, 그 중 NiO는 높은 활성도에 대한 가능성으로 인해 연구가 활발하게 진행되고 있다. 촉매의 표면에서 OER에 대한 메커니즘은 정확하게 규명되지는 않았지만, 산화물 촉매에서 Ni 또는 O vacancy와 같은 결함들은 많은 전기화학반응에서 활성점으로 여겨진다. 따라서, 본 연구에서는 nitrogen을 ethylenediamine을 이용하여 NiO의 O위치에 치환하여 Ni vacancy를 형성하고 그로 인해서 OER의 activity와 내구성에 어떠한 영향을 미치는지에 대해 분석해 보았다.

• 청정기술
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• 제21권2호
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• pp.117-123
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• 2015

본 연구는 LNT (lean NOx trap)용 DeNOx 촉매를 개발하기 위해 시도하였다. 이를 위해서 예비실험을 통해 Pt등 귀금속류등의 PGM (platinum group metal)을 사용하지 않는 4개의 촉매, Al/Co/Mn, Al/Co/Ni/Mn, Al/Co/Mn/Ca, Al/Co/Ni 혼합 금속 산화물을 선정하였다. 또한, 이들의 물리화학적인 성질을 평가하기 위해 XRD, EDS, SEM, BET 및 TPD test를 실시하였다. 이러한 평가를 실시한 결과, 4종의 촉매들은 스피넬(spinel)구조를 가지는 결정으로 이루어졌으며 NOx 기체들의 산화-환원 반응이 이루어지기에는 충분한 기공부피와 기공크기를 갖고 있음을 알 수 있었다. 또한, TPD test를 통해서는 산화-환원이 일어날 수 있는 산점을 4종의 촉매가 모두 가지고 있음을 확인하였다. 더욱이 ramp test를 통해서는 상용(commercial) 촉매와 비슷한 NO 산화 능력을 가지고 있는 것도 확인할 수 있었다. 이상의 결과들을 바탕으로, 본 연구에서 선정된 촉매들을 기본으로 하여 조성성분의 변화 및 활성 성분 첨가 등을 한다면, 보다 개선된 LNT용 DeNOx 촉매를 얻을 수 있을 것이라 기대할 수 있었다.

• 한국재료학회지
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• 제25권2호
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• pp.95-99
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• 2015

$NiAl_2O_4$ nanoparticle was synthesized by a reverse micelle processing for inorganic pigment. $Ni(NO_3)_2{\cdot}6H_2O$ and $Al(NO_3)_3{\cdot}9H_2O$ were used for the precursor in order to synthesize $NiAl_2O_4$ nanoparticles. The aqueous solution, which consisted of a mixing molar ratio of Ni/Al, was 1:2 and heat treated at $800{\sim}1100^{\circ}C$ for 2h. The average size and distribution of synthesized $NiAl_2O_4$ powders are in the range of 10-20 nm and narrow, respectively. The average size of the synthesized $NiAl_2O_4$ powders increased with an increasing water-to-surfactant molar ratio and heating temperature. The crystallinity of synthesized $NiAl_2O_4$ powder increased with an increasing heating temperature. The synthesized $NiAl_2O_4$ powders were characterized by X-ray diffraction analysis(XRD), a field emission scanning electron microscopy(FE-SEM), and a color spectrophotometer. The properties of synthesized powders were affected as a function such as a molar ratio and heating temperature. Results indicate that synthesis using a reverse miclle processing is a favorable process to obtain $NiAl_2O_4$ spinels at low temperatures. The procedure performed suggests that this new synthesis route for producing these oxides has the advantage of being fast and simple. Colorimetric coordinates indicate that the pigments obtained exhibit blue colors.

• 보존과학회지
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• 제35권2호
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• pp.145-152
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• 2019

The metal-manufacturing method and smelting temperature of ancient metal-production processes have been studied by analyzing the principal elements and microstructures of slag. However, the microstructure of slag varies according to the solidification cooling rate and types and relative amounts of various oxides contained within the smelting materials. Hence, there is a need for accurate analysis methods that allow slag to be distinguished by more than its composition or microstructure. In this study, the microstructures of slag discharged as a result of smelting iron sands collected from Pohang and Gyeongju, as well as the slag excavated from the Ungyo site in Wanju, were analyzed by using metalloscopy, scanning election microscopy-energy dispersine X-ray spectroscopy(SEM-EDS) and wavelength dispersive X-ray fluorenscence(WD-XRF). Furthermore, the microcrystals were accurately characterized by performing Raman micro-spectroscopy, which is a technique that can be used to identify the microcrystals of slags. SEM-EDS analysis of Pohang slag indicated that its white polygonal crystals could be Magnetite; however, Raman micro-spectroscopy revealed that these crystals were actually $ulv{\ddot{o}}spinel$. Raman micro-spectroscopy and SEM-EDS were also used to verify that the coarse white dendritic structures observed in the Gyeongju-slag were $W{\ddot{u}}stites$. Additionally, the Wanju slag was observed to have a glassy matrix, which was confirmed by Raman micro-spectroscopy to be Augite. Thus, we have demonstrated that Raman micro-spectroscopy can accurately identify slag microcrystals, which are otherwise difficult to distinguish as solely based on their chemical composition and crystal morphology. Therefore, we conclude that it has excellent potential as a slag analysis technique.

• Journal of Electrochemical Science and Technology
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• 제12권1호
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• pp.112-125
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• 2021

The new emerging "High entropy materials" attract the attention of the scientific society because of their simpler structure and spectacular applications in many fields. A novel nanocrystalline high entropy (Be,Mg,Ca,Sr,Zn,Ni)3O4 oxide has been successfully synthesized through mechanochemical treatment followed by sintering and air quenching. The present research work focuses on the possibility of single-phase formation in the aforementioned high entropy oxide despite the great difference in the atomic sizes of reactant alkaline earth and 3d transition metal oxides. Structural properties of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide were explored by confirmation of its single-phase Fd-3m spinel structure by x-ray diffraction (XRD). Further, nanocrystalline nature and morphology were analyzed by scanning electron microscopy (SEM). Among thermal properties, thermogravimetric analysis (TGA) revealed that the (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is thermally stable up to a temperature of 1200℃. Whereas phase evolution in (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide before and after sintering was analyzed through differential scanning calorimetry (DSC). Electrochemical studies of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide consists of a comparison of thermodynamic and kinetic parameters of water and hydrazine hydrate oxidation. Values of activation energy for water oxidation (9.31 kJ mol-1) and hydrazine hydrate oxidation (13.93 kJ mol-1) reveal that (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is catalytically more active towards water oxidation as compared to that of hydrazine hydrate oxidation. Electrochemical impedance spectroscopy is also performed to get insight into the kinetics of both types of reactions.

• 한국분말재료학회지
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• 제28권2호
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• pp.110-119
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• 2021

In this study, the high-temperature oxidation properties of austenitic 316L stainless steel manufactured by laser powder bed fusion (LPBF) is investigated and compared with conventional 316L manufactured by hot rolling (HR). The initial microstructure of LPBF-SS316L exhibits a molten pool ~100 ㎛ in size and grains grown along the building direction. Isotropic grains (~35 ㎛) are detected in the HR-SS316L. In high-temperature oxidation tests performed at 700℃ and 900℃, LPBF-SS316L demonstrates slightly superior high-temperature oxidation resistance compared to HR-SS316L. After the initial oxidation at 700℃, shown as an increase in weight, almost no further oxidation is observed for both materials. At 900℃, the oxidation weight displays a parabolic trend and both materials exhibit similar behavior. However, at 1100℃, LPBF-SS316L oxidizes in a parabolic manner, but HR-SS316L shows a breakaway oxidation behavior. The oxide layers of LPBF-SS316L and HR-SS316L are mainly composed of Cr₂O₃, Fe-based oxides, and spinel phases. In LPBF-SS316L, a uniform Cr depletion region is observed, whereas a Cr depletion region appears at the grain boundary in HR-SS316L. It is evident from the results that the microstructure and the high-temperature oxidation characteristics and behavior are related.

• 청정기술
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• 제21권3호
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• pp.184-190
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• 2015

대부분의 LNT 촉매는 낮은 온도 영역에서의 NO_x 산화를 위하여 Pt와 같은 귀금속류를 사용하는 것은 경제적인 부담을 가지고 있다. 따라서, 본 연구는 이러한 문제를 해결하기 위하여 시도되었다. 즉, Pt, Pd, Rh 등과 같은 귀금속류(platinum group metal, PGM)를 사용하지 않는 LNT (lean NO_x trap)용 DeNO_x 촉매를 개발하기 위해 시도하였다. 이를 위해서 예비실험을 통해 Pt등 귀금속류등의 PGM (platinum group metal)을 사용하지 않는 Al/Co/Ni 혼합 금속 산화물을 선정하였다. 궁극적으로는, 선정된 촉매의 소성온도에 따른 물리화학적 특성 변화가 NO_x 전환율에 미치는 영향을 살펴보고자 하였다. 이들의 물리화학적인 성질을 평가하기 위해 XRD, EDS, SEM, BET 분석을 실시하였다. 이러한 평가를 실시한 결과, 모든 소성온도에서 혼합금속 산화물은 Co₂AlO₄ 및 NiAl₂O₄의 스피넬 구조가 혼재되어 있는 것으로 나타났고, NO_x 기체들의 산화-환원 반응이 이루어지기에는 충분한 기공부피와 기공크기를 갖고 있음을 알 수 있었다. 그러나 NH₃-TPD 분석 결과에서는 소성온도가 700 ℃ 이하를 유지해야 하는 것으로 판단되었다. 더욱이 ramp test를 통해서는 NO 및 NO_x 전환율을 동시에 만족할 수 있는 시료는 소성온도는 500 ℃에서 처리된 경우임을 알 수 있었다. 이러한 결과 등을 바탕으로, Al/Co/Ni=1.0/2.5/0.3 혼합 금속 산화물의 최적 소성온도는 500 ℃임을 알 수 있었다.

• 한국수소및신에너지학회논문집
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• 제28권1호
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• pp.1-8
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• 2017

Cu/Mn/Ce catalysts for water gas shift (WGS) reaction were synthesized by urea-nitrate combustion method with the fixed molar ratio of Cu/Mn as 1:4 and 1:1 with the doping concentration of Ce from 0.3 to 0.8 mol%. The prepared catalysts were characterized with SEM, BET, XRD, XPS, $H_2$-TPR, $CO_2$ TPD, $N_2O$ chemisorption analysis. The catalytic activity tests were carried out at a GHSV of $28,000h^{-1}$ and a temperature range of 200 to $400^{\circ}C$. The Cu/Mn(CM) catalysts formed Cu-Mn mixed oxide of spinel structure ($Cu_{1.5}Mn_{1.5}O_4$) and manganese oxides ($MnO_x$). However, when a small amount of Ce was doped, the growth of $Cu_{1.5}Mn_{1.5}O_4$ was inhibited and the degree of Cu dispersion were increased. Also, the doping of Ce on the CM catalyst reduced the reduction temperature and the base site to induce the active site of the catalyst to be exposed on the catalyst surface. From the XPS analysis, it was confirmed that maintaining the oxidation state of Cu appropriately was a main factor in the WGS reaction. Consequently, Ce as support and dopant in the water gas shift reaction catalysts exhibited the enhanced catalytic activities on CM catalysts. We found that proper amount of Ce by preparing catalysts with different Cu/Mn ratios.