• Bulletin of the Korean Chemical Society
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• 제14권1호
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• pp.137-143
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• 1993

The tetranuclear heterometallic complex CpMo$Os_3(CO)_{10}({\mu]-H)2[{\mu}3-{\eta}^2-C(O)CH_2Tol]\;(1,\;Cp={\eta}^5-C_5H_5,\;Tol=p-C_6H_4Me)$ has been examined by variable-temperature $^{13}$C-NMR spectroscopy and by a full three-dimensional X-ray structual analysis. Complex 1 crystallizes in the orthorhombic space group Pna2$_1$ with a = 12.960(1) ${\AA}$, b = 11.255(l) ${\AA}$, c = 38.569(10)${\AA}$, V = 5626(2) ${\AA}^3$ and ${\rho}$(calcd) = 2.71 gcm$^{-3}$ for Z = 8 and molecular weight 1146.9. Diffraction data were collectedon a CAD4 diffractometer, and the structure was refined to $R_F$ = 9.7% and $R_{W^F}$ = 9.9% for 2530 data (MoK${\alpha}$ radiation). There are two essentially equivalent molecules in the crystallographic asymmetric unit. The tetranuclear molecule contains a triangulated rhomboidal arrangement of metal atoms with Os(2) and Mo at the two bridgehead positions. The metal framework is planar; the dihedral angle between Os(l)-Os(2)-Mo and Os(3)-Os(2)-Mo planes is 180$^{\circ}$. A triply bridging (${\mu}_3,\;{\eta}^2$) acyl ligand lies above the Os(l)-Os(2)-Mo plane; the oxygen atom spans the two bridgehead positions, while the carbon atom spans one bridgehead position and an acute apical position. The molecular architecture is completed by an ${\eta}^5$-cyclopentadienyl ligand and a semi-triply bridging carbonyl ligand on the molybdenum atom, and nine terminal carbonyl ligands-four on Os(3), three on Os(l), and two on Os(2). The two hydride ligands are inferred to occupy the Os(l)-Os(2) and Mo-Os(3) edges from structural and NMR data.

• 한국재료학회지
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• 제29권2호
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• pp.116-120
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• 2019

We prepared $Y_3Al_5O_{12};Ce^{3+},Pr3^{+}$ transparent ceramic phosphor using a solid state reaction method. By XRD pattern analysis and SEM measurement, our phosphors reveal an Ia-3d(230) space group of cubic structure, and the transparent ceramic phosphor has a polycrystal state with some internal cracks and pores. In the Raman scattering measurement with an increasing temperature, lattice vibrations of the transparent ceramic phosphor decrease due to its more perfect crystal structure and symmetry. Thus, low phonon generation is possible at high temperature. Optical properties of the transparent ceramic phosphor have broader excitation spectra due to a large internal reflection. There is a wide emission band from the green to yellow region, and the red color emission between 610 nm and 640 nm is also observed. The red-yellow phosphor optical characteristics enable a high Color Rendering Index (CRI) in combination with blue emitting LED or LD. Due to its good thermal properties of low phonon generation at high temperature and a wide emission range for high CRI characteristics, the transparent ceramic phosphor is shown to be a good candidate for high power solid state white lighting.

• 한국표면공학회지
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• 제56권6호
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• pp.401-411
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• 2023

This study investigates the synthesis, characterization, and application of zinc oxide (ZnO) nanoparticles for corrosion resistance and stress corrosion cracking (SCC) mitigation in high-temperature and high-pressure environments. The ZnO nanoparticles are synthesized using plasma discharge in water, resulting in rod-shaped particles with a hexagonal crystal structure. The ZnO nanoparticles are applied to Alloy 600 tubes in simulated nuclear power plant atmospheres to evaluate their effectiveness. X-ray diffraction and X-ray photoelectron spectroscopy analysis reveals the formation of thermodynamically stable ZnCr₂O₄and ZnFe₂O₄ spinel phases with a depth of approximately 35 nm on the surface after 240 hours of treatment. Stress corrosion cracking (SCC) mitigation experiments reveal that ZnO treatment enhances thermal and mechanical stability. The ZnO-treated specimens exhibit increased maximum temperature tolerance up to 310 ℃ and higher-pressure resistance up to 60 bar compared to non-treated ZnO samples. Measurements of crack length indicate reduced crack propagation in ZnO-treated specimens. The formation of thermodynamically stable Zn spinel structures on the surface of Alloy 600 and the subsequent improvements in surface properties contribute to the enhanced durability and performance of the material in challenging high-temperature and high-pressure environments. These findings have significant implications for the development of corrosion-resistant materials and the mitigation of stress corrosion cracking in various industries.

• 한국재료학회지
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• 제34권1호
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• pp.21-26
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• 2024

In this investigation, samples of the chemical (Hg_1-xPb_xBa₂Ca_1.8Mg_0.2Cu₃O_8+δ) were prepared utilizing a solid-state reaction technique with a range of lead concentrations (x = 0.0, 0.05, 0.10, and 0.20). Specimens were pressed at 8 tons per square centimeter and then prepared at 1,138 K in the furnace. The crystalline structure and surface topography of all samples were examined using X-ray diffraction (XRD) and atomic force microscopy (AFM). X-ray diffraction results showed that all of the prepared samples had a tetragonal crystal structure. Also, the results showed that when lead was partially replaced with mercury, an increase in the lead value impacted the phase ratio, and lattice parameter values. The AFM results likewise showed excellent crystalline consistency and remarkable homogeneity during processing. The electrical resistivity was calculated as a function of temperature, and the results showed that all samples had a contagious behavior, as the resistivity decreased with decreasing temperature. The critical temperature was calculated and found to change, from 102, 96, 107, and 119 K, when increasing the lead values in the samples from 0.0 to 0.05, 0.10, and 0.20, respectively.

• 분석과학
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• 제13권4호
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• pp.494-503
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• 2000

암 억제제인 $p16^{INK4A}$ 단백질의 활성부위 84-104번까지의 21개 아미노산으로 이루어진 펩타이드를 합성하여, 이것의 용액상 구조를 CD, $^1H$ NMR 분광법 그리고, 분자 모델링 방법으로 분석하였다. CDK4 그리고 CDK6와 함께 안정된 complex를 형성하는 p16의 활성 펩타이드(84-104 아미노산)는 in vitro에서 pRb를 인산화하는 CDK4/6의 능력을 차단하고, p16단백질의 기능에서 보여주듯이 G1/S상의 세포 Cycle을 차단한다. NOE를 포함하는 $^3J_{NH{\alpha}}$ 스핀결합 상수, $C_{\alpha}H$ 화학적 이동, 아마이드 화학적 이동의 평균 변화 폭 그리고 온도 계수 등은 p16 펩타이드의 이차구조가 helix-turn-helix의 구조를 구성하는 p16단백질과 유사한 2차 구조를 가지고 있음을 보여주었다. NOE에 근거한 거리 및 이면각을 이용한 3.D 기하구조는 p18이나 p19의 대응하는 부위에 대한 결정구조에서 보여준 바와 같이 아미노산 $Gly^{89}-Leu^{91}$(${\varphi}_{i+1}=-79.8^{\circ}$, ${\varphi}_{i+1}=60.2^{\circ}$)사이에는 ${\gamma}$-회전구조를 형성함을 보여주었다. 이렇게 비교적 단단한 구조를 형성하고 있는 ${\gamma}$-회전구조부위는 p16펩타이드 구조를 안정시키며, CDK를 인식하는 부위로 작용할 수 있다. 이러한 ${\gamma}$-회전구조는 항암제 선도물질을 개발하는데 유용하게 활용될 수 있을 것이다.

• KSBB Journal
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• 제19권1호
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• pp.42-49
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• 2004

Racemic epoxide에 대한 입체선택적 가수분해능을 가지고 있는 곰팡이, Aspergillus niger LK로부터 epoxide hydrolase (EH, EC 3.3.2.3) 유전자의 진화적 유연관계 분석을 행하였다. A. niger LK의 EH 염기서열로부터 유추한 EH 단백질 아미노산 서열은 여러 박테리아의 EH들 및 포유동물의 microsomal EH들과 유의적인 유사성을 가지고 있었으며 a/$\beta$ hydrolase fold family에 속하였다. A. niger LK의 EH 단백질의 입체구조예측은 Protein Data Bank에 수록된 lqo7의 3D 결정구조와 90.6% identity를 가지는 것으로 나타났으며 다른 EH들의 아미노산 서열비교를 행한 결과 Asp$^{192}$ , Asp$^{348}$ 및 His$^{374}$ 이 catalytic triad를 구성하고 있는 것으로 추정되었다. 여러 생물종의 EH서열을 기능적 및 구조적 domain 서열을 기초로 하여 multiple sequence alignment를 행하고 Neighbor-Joining/UPGMA method를 이용하여 계통수를 복원한 결과 다른 생물종들의 EH와의 진화거리는 서로 1.841∼2.682로 멀었으나 EH의 기능을 가지기 위한 oxyanion hole 및 a/$\beta$ hydrolase fold family의 catalytic triad는 잘 보존되고 있어 공통조상으로부터 진화되어 왔음을 알 수 있었다.

• 분석과학
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• 제6권2호
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• pp.157-165
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• 1993

강 중 석출물을 추출분리한 후 이를 정량분석하는 것을 목적으로 개발된 정전위 전해법을 304 스테인레스 판재 및 선재 제조시에 발생한 결함 원인 분석에 활용하여 시료의 조직을 관찰하였으며, 결함 원인을 조사하였다. 스테인레스 선재 및 판재의 균열 전파 양상은 정전위 전해법을 이용하여 에칭한 후 주사전자현미경으로 관찰하였고, 입계를 따라서 존재하는 조대한 석출물은 EDS 및 EPMA를 이용하여 성분분석을 행하였다. 이들 조대한 석출물의 구조분석은 X-선 회절 패턴을 이용하여 행하였다. 판재 및 선재 두 경우 모두 균열은 입계를 따라서 전파하고 있었으며, 입계에는 $M_{23}(C,\;B)_6$ 이외에 조대한 $M_2C$ 석출물이 존재하는 것으로 확인되었다. 이들 석출물들의 분석에 정전위 전해에칭법을 이용함으로써 양호한 시료를 얻을 수 있었다.

• Journal of Pharmaceutical Investigation
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• 제27권2호
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• pp.119-123
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• 1997

The physicochemical and structural properties of new capsaicin derivative, DA-5018, were examined. The reference standard of this compound was obtained by the recrystallization. A method for the determination of the dissociation constant of the compound is described. pH-solubility and distribution coefficient were determined by chromatographic method. Fundamental properties on thermal behaviors were investigated by TG, DTA and DSC. Structural analysis based on spectroscopic method coincided with the chemical structure of DA-5018. Approximate dissociation constant of the compound determined by UV spectral method was 9.35. Solubilities and partition coefficients in various pH buffer solution appeared pH-dependency. No crystal transition or further transition was found in the thermal analysis. This compound showed good stability, but pH 13 buffer and acetone made some degradative products.

• 공업화학
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• 제30권5호
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• pp.615-619
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• 2019

통계학적 실험계획법을 이용하여 다공성 구조체인 MOF-235 합성 공정 최적화를 수행하였다. 합성에 사용되는 주성분인 terephthalic acid (TPA), Iron (III) chloride hexahydrate, N,N-dimethylformamide (DMF) 및 ethanol의 농도가 MOF-235의 결정구조를 형성하는데 중요한 요소가 되었다. 다양한 농도의 4가지 성분을 이용하여 MOF-235를 합성한 후 XRD를 이용하여 결정도를 측정하였다. 16가지 실험조건을 통해 합성한 MOF-235의 결정도 결과를 통계학적 해석을 통해 주성분의 조성이 입자의 합성에 미치는 영향을 분석하였다. F 검정법을 이용한 분산분석에서 에탄올의 농도가 입자의 결정도에 가장 큰 영향을 미치고 TPA가 가장 영향력이 작은 것으로 분석되었다. 결정도를 예측할 수 있는 회귀모델을 도출하였고 2가지 합성변수에 대한 예측결과를 등고선도를 이용하여 제시하였다. 마지막으로 혼합물법을 이용하여 3가지 합성인자가 미치는 결정도를 예측하여 제시하였다.

• 한국재료학회지
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• 제34권1호
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• pp.27-33
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• 2024

Al₂O₃ has excellent sintering properties and is important in semiconductor manufacturing processes that require high-temperature resistance and chemical inertness in a plasma environment. In this study, a comprehensive analysis of the chemical characteristics, physical properties, crystal structure, and dispersion stability of three commercially available Al₂O₃ powders was conducted. The aim was to provide a technological foundation for selecting and utilizing appropriate Al₂O₃ powders in practical applications. All powders exhibited α-Al₂O₃ as the main phase, with the presence of beta-phase Na₂O-11Al₂O₃ as the secondary phase. The highest Na⁺ ion leaching was observed in the aqueous slurry state due to the presence of the secondary phase. Although the average particle size difference among the three powders was not significant, distinct differences in particle size distribution were observed. ALG-1SH showed a broad particle size distribution, P162 exhibited a bimodal distribution, and AES-11 displayed a uniform unimodal distribution. High-concentration Al₂O₃ slurries showed differences in viscosity due to ion release when no dispersant was added, affecting the electrical double-layer thickness. Polycarboxylate was found to effectively enhance the dispersion stability of all three powders. In the dispersion stability analysis, ALG-1SH exhibited the slowest sedimentation tendency, as evidenced by the low TSI value, while P162 showed faster precipitation, influenced by the particle size distribution.