• Mass Spectrometry Letters
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• v.14 no.3
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• pp.110-115
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• 2023

The reaction of (COD)PdCl₂ with new C₃-symmetric tridentate L (COD = 1,5-cyclooctadien; L = 1,3,5-tris(picolinoyloxyethyl)cyanurate) in a mixture of acetone and dichloromethane produces single crystals consisting of unprecedented monometallacyclic [PdCl₂(L)]. This cyclic compound arises from trans-chelation of two of three donating pyridyl groups of L, while the third pyridyl group remains uncoordinated. Electrospray ionization mass spectrometry (ESI-MS) data on L exhibited the major peak corresponding to [C₂₇H₂₄N₆O₉ + H⁺]⁺. Fast atom bombardment mass spectrometry (FABMS) data on [PdCl₂(L)], however, showed the mass peak corresponding to the L instead of the present palladium(II) compound species, due to the insolubility and dissociation in solution. The physicochemical properties of the present palladium(II) compound were fully characterized by means of infrared (IR) and nuclear magnetic resonance (NMR) spectroscopy, thermal analysis, single-crystal X-ray diffraction (SC-XRD) measurement.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.8 no.3
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• pp.435-441
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• 1998

Li-SGICs as a anode of lithium ion battery were synthesized by high-pressure method as a function of the Li-contents. The characteristics of these prepared compounds were determined from the studies with X-ray diffraction method and differential scanning calorimeter (DSC) analysis. From the results of X-ray diffraction, it was found that the lower stage intercalation compounds were formed with increase of Li-contents. The mixed stages in these compounds were also observed. In the case of the $Li_{30;wt%}$-SGIC, the compounds in the stage 1 structure were formed predominantly, but the structure of only pure stage 1, due to the structural defect of synthetic graphite, was not observed. The enthalpy and entropy changes of the compounds could be obtained from the differential scanning calorimetric analysis results. From the results, it was found that exothermic and endothermic reactions of Li-SGICs are related to thermal stability of lithium between artificial graphite layers.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.3 no.2
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• pp.167-175
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• 1993

Lithium-Carbon Intercalation Compounds(Li-CICs) have been synthesized from various carbon ma-terials by use of the modified stainless steel two-bulbs methods. These compounds had various colours by structural character of starting materials. The synthesized Li-CICs were identified to stage formation process by X-ray diffraction data. At these results, well-oriented natural graphite and graphite fiber are formed lower stages(Stage 1, Stage 2), but poor-oriented carbon fiber and petroleum cokes are also formed higher stages(Stage 3, Stage 4, Stage 5). And when we compared with measured d value and calculated d value, these values agreed with each other. But poor-oriented carbon materials are some difference from them. The stage stability and energy stage of Li-CICs were obtained by UV/VIS Spectrophotometric data. X-ray diffraction and UV/VIS Spectrophotometric data suggested that well-oriented carbon materials has distingushible curve between energy and reflectance. In these results, we know that many charge carriers between carbon layers are related to concentration of intercalants. And then, this paper also provides information on high efficiency energy storing materials at intercalation process of Li-CICs.

• Proceedings of the Optical Society of Korea Conference
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• 1999.08a
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• pp.220-221
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• 1999

Single crystals of Yttrium Calcium Oxyborate (YCOB) doped with different concentrations of Er3+ and Yb3+ ions were growth by Czochralski method. High qualities of crystals in morphology and transparency were obtained . Analysis on crystal structure and lattice parameters were performed by X-ray diffraction method. It was found that congruent melting composition is YCA4.2O1.2(BO3)3. Absorption and fluorescence properties of grown crystals were also reported.

• The Korean Journal of Ceramics
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• v.6 no.1
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• pp.21-26
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• 2000

Nanosized powders of trimetallic orthoferrites containing La and Sm in different ratios were synthesised by the thermal decomposition at low temperatures of the corresponding hexacyanocomplexes. The precursors and their decomposition products were analyzed by simultaneous thermogravimetric and differential thermal analysis (TG/DTA), x-ray diffraction (XRD) and Raman spectroscopy. Single phase trimetallic precursors and oxides were obtained. The crystal structure of the perovskitic oxides was orthorhombic, and the lattice parameters were affected by the ionic size of the rare earth elements present in the oxides. Raman spectroscopy showed a disorder effect in the vibrational bands with increasing the La content.

• Bulletin of the Korean Chemical Society
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• v.5 no.4
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• pp.135-140
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• 1984

The reduction of vacuum-dehydrated $Na_xAg_{12-x}-A, 0 {\le} x {\le} 9.2$, and its reoxidation by O$_2$, have been studied by X-ray powder diffraction. Also, the structure of $Na_6Na_6-A$ treated with hydrogen at room temperature has been studied by single crystal methods in the cubic space group Pm3m at $24{\circ}C (a = 12.221(2) {\AA})$. The diffraction pattern of dehydrated Ag$_{12}$-A reduced by H$_2$ contains only the (111) and (200) reflections of silver metal, indicationg that the zeolite structure has been lost, but the zeolite's diffraction pattern and structural integrity can be fully restored by oxidation with O$_2$ at 100 or 200${\circ}C$. In contrast, the structures of $Na_xAg_{12-x}-A$, x = 4.5 and 9.2, were not destroyed by treatment with hydrogen. Dehydrated Na$_6Ag_6$-A treated with 50 Torr of hydrogen gas at 24${\circ}C$ for 30 minutes has $6\; Na^+\;and\;1.27\;Ag^+$ ions at 6-ring sites. These $Ag^+ ions are associated with 2.54 Ag${\circ}$ atoms to form 1.27 $Ag_3^+$ clusters per unit cell. Also found were 0.7 $Ag_3^{2+}$ clusters per unit cell near the 8-rings. The structure was refined to the final error indices R$_1$ = 0.134 and R$_2$ (weighted) = 0.147, using 168 independent reflections for which $I_0 >3{\sigma}(I_0)$.

• Corrosion Science and Technology
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• v.22 no.1
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• pp.36-43
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• 2023

Single-crystal Ni-rich NCM is a material that has drawn attention in the field of lithium-ion batteries due to its high energy density and long cycle life. In this study, we investigated the properties of single-crystal NCM 811 and its potential for use in lithium-ion batteries. High-quality single crystals of NCM 811 were successfully synthesized by crystal growth via a flux method. The single-crystal nature of the samples was confirmed through detailed characterization techniques, such as scanning electron microscopy and x-ray diffraction with Rietveld refinement. The crystal structure and electrochemical performances of the single-crystal NCM 811 were analyzed and compared to its poly-crystal counterpart. The results indicated that single-crystal NCM 811 had electrochemical performance and thermal stability superior to poly-crystalline NCM 811, making it a suitable candidate for high-performance batteries. The findings of this study contribute to a better understanding of the characteristics and potential of single-crystal NCM 811 for lithium-ion batteries.

• Journal of Integrative Natural Science
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• v.7 no.3
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• pp.149-158
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• 2014

The crystal structure of the title compounds with both coumarin and sulfonamide moieties were examined. These two groups have very special for their pharmaceutical and medicinal properties have been determined from single crystal X-ray diffraction data. In the title compound crystallizes in the monoclinic space group $P2_1/c$ with unit cell dimension a=$8.5775(4){{\AA}$, b=$24.9943(13){\AA}$ and c=$13.7319(7){\AA}$ [alpha & gamma=$90^{\circ}$ beta=$103.558(2)^{\circ}$]. In the structure The S1 atom shows a distorted tetrahedral geometry, with O1-S1-O2 [$121.08(1)^{\circ}$] and N1-S1-C5 [$105.85(1)^{\circ}$] angles deviating from ideal tetrahedral values are attributed to the Thrope-Ingold effect. The sum of bond angles around N1 ($354.9^{\circ}$) indicates that N1 is in $sp^2$ hybridization. The Pyridine ring adopts boat conformation and pyran rings adopt a sofa conformation. Crystal structure is stabilized by C-H...O intra molecular hydrogen bond interactions.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.07a
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• pp.281-287
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• 2002

The stochiometric composition of AgGaS$_2$ polycrystal source materials for the AgGaS$_2$/GaAs epilayer was prepared from horizontal furnace. From the extrapolation method of X-ray diffraction patterns it was found that the polycrystal AgGaS$_2$ has tetragonal structure of which lattice constant a$\sub$0/ and c$\sub$0/ were 5.756 ${\AA}$ and 10.305 ${\AA}$, respectively. AgGaS$_2$/GaAs epilayer was deposited on throughly etched GaAs(100) substrate from mixed crystal AgGaS$_2$ by the Hot Wall Epitaxy (100) system. The source and substrate temperature were 590$^{\circ}C$ and 440$^{\circ}C$ respectively. The crystallinity of the grown AgGaS$_2$/GaAs epilayer was investigated by the DCRC (double crystal X-ray diffraction rocking curve). The optical energy gaps were found to be 2.61 eV for AgGaS$_2$/GaAs epilayer at room temperature. The temperature dependence of the photocurrent peak energy is well explained by the Varshni equation, then the constants in the Varshni equation are given by ${\alpha}$ : 8.695${\times}$10$\^$-4/ eV/K, and ${\beta}$ = 332 K. From the photocurrent spectra by illumination of polarized light of the AgGaS$_2$/GaAs epilayer, we have found that crystal field splitting ΔCr was 0.28 eV at 20 K. From the PL spectra at 20 K, the peaks corresponding to free and bound excitons and a broad emission band due to D-A pain are identified. The binding energy of the free excitons are determined to be 0.2676 eV and 0.2430 eV and the dissociation energy of the bound excitons to be 0.4695 eV.

• Journal of Integrative Natural Science
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• v.7 no.2
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• pp.92-102
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• 2014

The crystal structure of the title compounds with both coumarin and sulfonamide moieties were examined. These two groups have very special for their pharmaceutical and medicinal properties have been determined from single crystal X-ray diffraction data. In the title compound crystallizes in the monoclinic space group C2/c with unit cell dimension a = 28.633(3) ${\AA}$, b= 9.3215(7) ${\AA}$ and c= 24.590(2) ${\AA}$ [alpha & gamma=$90^{\circ}$ beta= $115.976(3)^{\circ}$]. In the structure The S1 atom shows a distorted tetrahedral geometry, with O1-S1-O2 [119.74 $(2)^{\circ}$] and N1-S1-C5 [$105.57(1)^{\circ}$] angles deviating from ideal tetrahedral values are attributed to the Thrope-Ingold effect. The sum of bond angles around N1 ($316.2(1)^{\circ}$) indicates that N1 is in sp2 hybridization. The Pyridine ring adopts boat conformation and pyran rings adopt a sofa conformation. The carboxylate group of atoms were disordered over two positions with site occupancy factors 0.598 (9):0.402 (9). Crystal structure and packing is stabilized by $C-H{\ldots}O$ intra and inter molecular hydrogen bond interactions.