• Title/Summary/Keyword: X-ray Structure Analysis

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Polyimide Multilayer Thin Films Prepared via Spin Coating from Poly(amic acid) and Poly(amic acid) Ammonium Salt

  • Ha, You-Ri;Choi, Myeon-Cheon;Jo, Nam-Ju;Kim, Il;Ha, Chang-Sik;Han, Dong-Hee;Han, Se-Won;Han, Mi-Jeong
    • Macromolecular Research
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    • v.16 no.8
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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.

Synthesis, Characterization and Property Studies on a Dinuclear Copper(II) Complex with Dipyridine Derivate and Acetylacetone

  • Zhao, Pu Su;Guo, Zhi Yan;Sui, Jing;Wang, Jing;Jian, Fang Fang
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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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.

Characterization of Microstructure and Thermal property of Ash Deposits on Fire-side Boiler Tube

  • Bang, Jung Won;Lee, Yoon-Joo;Shin, Dong-Geun;Kim, Younghee;Kim, Soo-Ryong;Baek, Chul-Seoung;Kwon, Woo-Teck
    • Journal of the Korean Ceramic Society
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    • v.53 no.6
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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.

Characterization and Synthesis of BN Fibers According to the Content of BN Nanopowder by Electrospinning Method (전기방사에 의한 질화붕소 나노분말의 함량에 따른 질화붕소 나노섬유 합성 및 특성 평가)

  • Lee, Jong Hyeok;Chun, Myoung Pyo;Hwang, Jin Ah;Jung, Young Geun;Chu, Jae Uk
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.31 no.7
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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.

A Study on the Microwave Absorber Properties of Ni-Cu-Zn Ferrites Composite (Ni-Cu-Zn Ferrite의 복합형 전파흡수체 특성 연구)

  • Min, Eui-Hong;Kim, Moon-Suk;Koh, Jae-Gui
    • Journal of the Korean Magnetics Society
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    • v.17 no.6
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    • pp.238-241
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    • 2007
  • Ni-Cu-Zn ferrites were prepared by the co-precipitation. Physical properties and Microwave absorbing properties were investigated in Ni-Cu-Zn ferrite for the aim of microwave absorbers. From the analysis of X-ray diffraction patterns, we can see that all the particles have only a single phase spinel structure. The loss factor was maximum at sintering temperature $1100^{\circ}C$. The initial permeability of sintered ferrite obtained was an average of 50. We found that the $(Ni_{0.7}Cu_{0.2}Zn_{0.1}O)_{1.02}(Fe_2O_3)_{0.98}$ can be used in ferrite rubber composite microwave absorber when sintering temperature at $1100^{\circ}C$.

Characterization of Fe-ACF/$TiO_2$ composite Photocatalysts Effect Via Degradation of MB Solution (Fe-ACF/$TiO_2$ 복합체의 특성과 MB용액의 분해에서 포토-펜톤 효과)

  • Zhang, Kan;Meng, Ze-Da;Ko, Weon-Bae;Oh, Won-Chun
    • Elastomers and Composites
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    • v.44 no.3
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    • pp.290-298
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    • 2009
  • In this paper, the Fe-activated carbon fiber (ACF)/$TiO_2$ composite catalysts were prepared by a sol-gel method. The synthesized photocatalysts were used for the photo degradation of Methylene blue solution under UV light. From Brunauer-Emmett-Teller measurements (BET) data, it was shown the blocking of the micropores on the surface of ACF by treatment of Fe and Ti compound. As shown in SEM images, the ferric compounds and titanium dioxides were fixed onto the ACF surfaces. The result of X-ray powder diffraction showed that the crystal phase contained a mixing anatase and rutile structure and the 'FeO+$TiO_2$' from the composites. The EDX spectra for the elemental analysis showed the presence of C, O, and Ti with Fe peaks. Degradation activity of MB could be attributed to +OH radicals derived from electron/hole pair's reactions due to photolysis of $TiO_2$ and photo-Fenton effect of Fe.

Syntheses, Structures and Luminescent Properties of Two Novel M(II)-Phen-SIP Supramolecular Compounds (M = Co, Ni)

  • Zhu, Yu-Lan;Shao, Shuai;Ma, Kui-Rong;Tang, Xue-Ling;Cao, Li;Zhao, Hui-Chao
    • Bulletin of the Korean Chemical Society
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    • v.33 no.4
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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).

Virtual Screening of Tubercular Acetohydroxy Acid Synthase Inhibitors through Analysis of Structural Models

  • Le, Dung Tien;Lee, Hyun-Sook;Chung, Young-Je;Yoon, Moon-Young;Choi, Jung-Do
    • Bulletin of the Korean Chemical Society
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    • v.28 no.6
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    • pp.947-952
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    • 2007
  • Mycobacterium tuberculosis is a pathogen responsible for 2-3 million deaths every year worldwide. The emergence of drug-resistant and multidrug-resistant tuberculosis has increased the need to identify new antituberculosis targets. Acetohydroxy acid synthase, (AHAS, EC 2.2.1.6), an enzyme involved in branched-chain amino acid synthesis, has recently been identified as a potential anti-tuberculosis target. To assist in the search for new inhibitors and “receptor-based” design of effective inhibitors of tubercular AHAS (TbAHAS), we constructed four different structural models of TbAHAS and used one of the models as a target for virtual screening of potential inhibitors. The quality of each model was assessed stereochemically by PROCHECK and found to be reliable. Up to 89% of the amino acid residues in the structural models were located in the most favored regions of the Ramachandran plot, which indicates that the conformation of each residue in the models is good. In the models, residues at the herbicide-binding site were highly conserved across 39 AHAS sequences. The binding mode of TbAHAS with a sulfonylurea herbicide was characterized by 32 hydrophobic interactions, the majority of which were contributed by residue Trp516. The model based on the highest resolution X-ray structure of yeast AHAS was used as the target for virtual screening of a chemical database containing 8300 molecules with a heterocyclic ring. We developed a short list of molecules that were predicted to bind with high scores to TbAHAS in a conformation similar to that of sulfonylurea derivatives. Five sulfonylurea herbicides that were calculated to efficiently bind TbAHAS were experimentally verified and found to inhibit enzyme activity at micromolar concentrations. The data suggest that this time-saving and costeffective computational approach can be used to discover new TbAHAS inhibitors. The list of chemicals studied in this work is supplied to facilitate independent experimental verification of the computational approach.

Highly Efficient Red Emissive Heteroleptic Cyclometalated Iridium(III) Complexes Bearing Two Substituted 2-Phenylquinoxaline and One 2-Pyrazinecarboxylic Acid

  • Sengottuvelan, Nallathambi;Yun, Seong-Jae;Kim, Dae-Young;Hwang, In-Hye;Kang, Sung Kwon;Kim, Young-Inn
    • Bulletin of the Korean Chemical Society
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    • v.34 no.1
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    • pp.167-173
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    • 2013
  • A series of highly efficient red phosphorescent heteroleptic iridium(III) complexes 1-6 containing two cyclometalating 2-(2,4-substitued phenyl)quinoxaline ligands and one chromophoric ancillary ligand were synthesized: (pqx)$_2Ir$(mprz) (1), (dmpqx)$_2Ir$(mprz) (2), (dfpqx)$_2Ir$(mprz) (3), (pqx)$_2Ir$(prz) (4), (dmpqx)$_2Ir$(prz) (5), (dfpqx)$_2Ir$(prz) (6), where pqx = 2-phenylquinoxaline, dfpqx = 2-(2,4-diflourophenyl)quinoxaline, dmpqx = 2-(2,4-dimethoxyphenyl)quinoxaline, prz = 2-pyrazinecarboxylate and mprz = 5-methyl-2-pyrazinecarboxylate. The absorption, emission, electrochemical and thermal properties of the complexes were evaluated for potential applications to organic light-emitting diodes (OLEDs). The structure of complex 2 was also determined by single-crystal X-ray diffraction analysis. Complex 2 exhibited distorted octahedral geometry around the iridium metal ion, for which 2-(2,4-dimethoxyphenyl)quinoxaline N atoms and C atoms of orthometalated phenyl groups are located at the mutual trans and cis-positions, respectively. The emission spectra of the complexes are governed largely by the nature of the cyclometalating ligand, and the phosphorescent peak wavelengths can be tuned from 588 to 630 nm with high quantum efficiencies of 0.64 to 0.86. Cyclic voltammetry revealed irreversible metal-centered oxidation with potentials in the range of 1.16 to 1.89 V as well as two quasi-reversible reduction waves with potentials ranging from -0.94 to -1.54 V due to the sequential addition of two electrons to the more electron-accepting heterocyclic portion of two distinctive cyclometalated C^N ligands.

Synthesis and Characterization of Nanosized of Spinel LiMn2O4 via Sol-gel and Freeze Drying Methods

  • Seyedahmadian, Masoud;Houshyarazar, Shadi;Amirshaghaghi, Ahmad
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.622-628
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    • 2013
  • Nanocrystalline spinel lithium manganese oxide ($LiMn_2O_4$) powders with narrow-size-distribution, pure-phase particles, and high crystallinity with an average crystallite size of about 70 nm were synthesized at $600^{\circ}C$ for 6 h in air by freeze drying method. Spinel $LiMn_2O_4$ is also prepared by sol-gel using citric acid as a chelating agent. The influence of different parameters such as pH conditions, solvent, molar ratio of citric acid to total metal ions, calcination temperature, starting material on the structure, morphology and purity of this oxide was investigated. The results of sol-gel method show that pure $LiMn_2O_4$ with average crystallite size of about 130 nm can be produced from nitrate salts as starting materials at $800^{\circ}C$ for 6 h in air. The optimum pH and molar ratio of chelating agent to total metal ions are $4{\leq}pH{\leq}6$ and 1.0, respectively. A possible mechanism on the formation of the nanocrystallines synthesized by sol-gel was also discussed. At the end a comparison of the differences between two methods was made on the basis of x-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) tests.