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

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Synthesis, Crystal Structures and Properties of Two Binuclear Supramolecular Complexes Based on Biphenyl-2,2'-dicarboxylic Acid Ligand

  • Tang, Jin-Niu;Pan, Gang-Hong;Li, Long;Tian, Wei-Man;Huang, Zhong-Jing
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.374-378
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    • 2013
  • Two novel binuclear metal-organic coordination complexes [$Cd_2(Hdpa)_4(bpy)_2$] (1), [$Dy_2(dpa)_2(bpy)_2(NO_3)_2-(H_2O)_2$](bpy) (2) (where $H_2dpa$ = biphenyl-2,2'-dicarboxylic acid, bpy = 2,2'-bipyridine) have been synthesized under hydrothermal conditions and characterized by single crystal X-ray diffraction, spectral method (IR), elemental analysis (EA), powder X-ray diffraction (XRD), electronic spectra (UV-vis), fluorescent in the solid state and thermogravimetric analysis (TGA). Complexes 1-2 crystallizes isomorphously in the Triclinic space group P-1. The ${\pi}-{\pi}$ stacking interactions and hydrogen-bonds play a vital role in determining the crystal packing and construction of the extended 3-D supramolecular network.

Pitting Corrosion Inhibition of Sprinkler Copper Tubes via Forming of Cu-BTA Film on the Inner Surface of Corrosion pits

  • Suh, Sang Hee;Suh, Youngjoon;Kim, Sohee;Yang, Jun-Mo;Kim, Gyungtae
    • Corrosion Science and Technology
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    • v.18 no.2
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    • pp.39-48
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    • 2019
  • The feasibility of using benzotriazole (BTAH) to inhibit pitting corrosion in the sprinkler copper tubes was investigated by filling the tubes with BTAH-water solution in 829 households at an eight-year-old apartment complex. The water leakage rate was reduced by approximately 90% following BTAH treatment during 161 days from the previous year. The leakage of one of the two sprinkler copper tubes was investigated with optical microscopy, scanning electron microscopy, energy dispersive spectroscopy, X-ray photoelectron spectroscopy, and X-ray diffraction analysis to determine the formation of Cu-BTA film inside the corrosion pits. All the inner components of the corrosion pits were coated with Cu-BTA films suggesting that BTAH molecules penetrated the corrosion products. The Cu-BTA film was about 2 nm in thickness at the bottom of a corrosion pit. A layer of CuCl and $Cu_2O$ phases lies under the Cu-BTA film. This complex structure effectively prevented the propagation of corrosion pits in the sprinkler copper tubes and reduced the water leakage.

One-Dimensional MgO Nanostructures with Various Morphologies Grown by Thermal Evaporation Method under Atmospheric Environment (대기 분위기에서 열증발법에 의해 성장된 여러 가지 형상의 일차원 MgO 나노구조)

  • Nam-Woo Kim;Jin-Su Kim;Geun-Hyoung Lee
    • Korean Journal of Materials Research
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    • v.33 no.7
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    • pp.279-284
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    • 2023
  • One-dimensional MgO nanostructures with various morphologies were synthesized by a thermal evaporation method. The synthesis process was carried out in air at atmospheric pressure, which made the process very simple. A mixed powder of magnesium and active carbon was used as the source powder. The morphologies of the MgO nanostructures were changed by varying the growth temperature. When the growth temperature was 700 ℃, untapered nanowires with smooth surfaces were grown. As the temperature increased to 850 ℃, 1,000 ℃ and 1,100 ℃, tapered nanobelts, tapered nanowires and then knotted nanowires were sequentially observed. X-ray diffraction analysis revealed that the MgO nanostructures had a cubic crystallographic structure. Energy dispersive X-ray analysis showed that the nanostructures were composed of Mg and O elements, indicating high purity MgO nanostructures. Fourier transform infrared spectra peaks showed the characteristic absorption of MgO. No catalyst particles were observed at the tips of the one-dimensional nanostructures, which suggested that the one-dimensional nanostructures were grown in a vapor-solid growth mechanism.

Analysis of crystalline structure of autogenous tooth bone graft material: X-Ray diffraction analysis (자가치아골이식재의 결정구조 분석: X선 회절 분석)

  • Kim, Gyung-Wook;Yeo, In-Sung;Kim, Su-Gwan;Um, In-Woong;Kim, Young-Kyun
    • Journal of the Korean Association of Oral and Maxillofacial Surgeons
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    • v.37 no.3
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    • pp.225-228
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    • 2011
  • This study evaluated the mineral crystalline structure of an autogenous tooth bone graft material. The crystalline structures of the autogenous tooth bone graft material enamel (AutoBT E+), dentin (AutoBT D+), xenograft (BioOss), alloplastic material (MBCP), allograft (ICB) and autogenous mandibular cortical bone were compared using XRD. The XRD pattern of AutoBT dentin and ICB was similar to that of autogenous bone.

Di- and Triorganotin(IV) Complexes of Sulfur-containing Ylidenemalonates

  • Jung, Ok-Sang;Lee, Young-A;Hong, Jong-Ki;Jeong, Jong-Hwa;Sohn, Youn-Soo
    • Bulletin of the Korean Chemical Society
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    • v.14 no.6
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    • pp.722-726
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    • 1993
  • Organotin(IV) complexes of ylidenemalonates $(R_xSn)_{x-1}(O_2C)_2C=C(SR')_2\;(R=n-C_4H_9,\;C_6H_5,\;cyclo-C_6H_{11},\;CH_3OOCCH_2CH_2;\;x=2,3;\;R'=CH_3,\;R_2'=-CHCH-,\;-CH_2CH_{2^-})$ have been synthesized and characterized by means of various spectroscopic methods. The X-ray crystal structure of $(Ph_3Sn)_2(O_2C)_2C=C(SCH_3)_2$ has been determined (Pi; a= 9.704(2) ${\AA}$, b= 14.412(1) ${\AA}$, c= 14.760(3) ${\AA}$, ${alpha}$=74.26(1)$^{\circ}$, ${beta}$=99.38(l)$^{\circ}$, ${\gamma}$=79.09(1)$^{\circ}$, $V= 1950.7(7){\AA}^3$) and refined to R= 0.045. The crystal structure discloses a discrete molecule with bidentate-like carboxylate ligand. For diorganotin analogues, the structures are discussed in terms of IR, $^1H-NMR,\;^{13}C-NMR$, and FAB mass spectrometry. The mass spectrum indicates that the diorganotin complexes of ylidenemalonates are dimeric.

A Study of Oxidation Behavior on the Surface of Nd-Fe-B Ribbon Alloy by X-ray Photoelectron Spectroscopy (X-선 광전자 분광법에 의한 Nd-Fe-B 리본합금으 표면 산화거동 연구)

  • Chung, Kang-Sup;Sung, Hak-Je;Kim, Kun-Han;Park, Yun-Chang;Lee, Kyoung-Chul;Shu, Su-Jeong
    • Analytical Science and Technology
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    • v.8 no.3
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    • pp.351-358
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    • 1995
  • Oxidation behavior on the surface of Nd-Fe-B ribbon alloy has been studied by X-ray Photoelectron Spectroscopy. In the incipient stage of oxidation on the surface of "as-received" ribbon Nd-oxide film was formed from the fast oxidation of Nd and Fe was metal state in bulk. In process of oxidation time Fe was more abundant in the outmost surface of ribbon from the defused Fe through Nd-oxide film and layer structure of oxidation film was formed.

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Characterization and Conversion Electron Mössbauer Spectroscopy of HoMn1-x-FexO3 Thin Films by Pulsed Laser Deposition (PLD를 이용한 HoMn1-x-FexO3 박막 제조 및 후방 산란형 뫼스바우어 분광 연구)

  • Choi, Dong-Hyeok;Shim, In-Bo;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.17 no.1
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    • pp.18-21
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    • 2007
  • The hexagonal $HoMn_{1-x}-Fe_xO_3$(x=0.00, 0.05) thin films were prepared using pulsed laser deposition(PLD) method on $Pt/Ti/SiO_2/Si$ substrate. The microstructure and magnetic properties have been studied by x-ray diffraction(XRD), atomic force microscopy (AFH), scanning electron microscope(SEM:), x-ray photoelectron spectroscopy(XPS), and conversion electron $M\"{o}ssbauer$ spectroscopy(CEMS). From the analysis of the x-ray diffraction patterns, the crystal structure for all films was found to be a hexagonal($P6_3cm$), which was preferentially grown along(110) direction. The lattice constant $c_0$ of the film with x=0.05 was close to that of single crystal, whereas lattice constant $a_0$ with respect to single crystal shows a slight decrease. This difference of lattice parameters between film and single crystal was caused by the lattice mismatch between the film and $Pt/Ti/SiO_2/Si$ substrate. Conversion electron $M\"{o}ssbauer$ spectrum of $HoMn_{0.95}Fe_{0.05}O_3$ thin film shows an asymmetry doublet absorption ratio at room temperature, which is due to the oriented direction of crystallographic domains. This is corresponding with analysis of x-ray diffraction. The quadrupole splitting(${\Delta}E_Q$) at room temperature is found to be $1.62{\pm}0.01mm/s$. This large ${\Delta}E_Q$ was caused by asymmetry environment surrounding Fe ion.

Density Functional Theory Demonstration of Anomeric Effect and Structure: Conformational and Configurational Analysis of N-2-(1,4-Dioxane)-N'-(4-methylbenzenesulfonyl)-O-(4-methylphenoxy) Isourea

  • Dabbagh, Hossein A.;Najafi Chermahini, Ali Reza;Modarresi-Alam, Ali Reza
    • Bulletin of the Korean Chemical Society
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    • v.26 no.8
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    • pp.1229-1234
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    • 2005
  • The conformational, configurtational behavior and the structure of N-2-(1,4-Dioxane)-N'-(4-methylbenzenesulfonyl)-O-(4-methylphenoxy) isourea 1 has been studied using DFT method. Calculations predict the imidoyl amino group of the dioxane ring prefers axial conformation and that the tosyl and tolyl groups about the C=N bond retain E configuration. The anomeric effect controls the population of dioxane ring conformers, and anomers. Intramolecular hydrogen bonds contribute to the stability of E isomers. The computational analysis of 1 complements the X-ray findings.

3-D Structured Cu2ZnSn (SxSe1-x)4 (CZTSSe) Thin Film Solar Cells by Mo Pattern using Photolithography (Mo 패턴을 이용한 3-D 구조의 Cu2ZnSn (SxSe1-x)4 (CZTSSe) 박막형 태양전지 제작)

  • Jo, Eunjin;Gang, Myeng Gil;Shin, hyeong ho;Yun, Jae Ho;Moon, Jong-ha;Kim, Jin Hyeok
    • Current Photovoltaic Research
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    • v.5 no.1
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    • pp.20-24
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    • 2017
  • Recently, three-dimensional (3D) light harvesting structures are highly attracted because of their high light harvesting capacity and charge collection efficiencies. In this study, we have fabricated $Cu_2ZnSn(S_xSe_{1-x})_4$ based 3D thin film solar cells on PR patterned Molybdenum (Mo) substrates using photolithography technique. Specifically, Mo patterns were deposited on PR patterned Mo substrates by sputtering and the thin Cu-Zn-Sn stacked layer was deposited over this Mo patterns by sputtering technique. The stacked Zn-Sn-Cu precursor thin films were sulfo-selenized to form CZTSSe pattern. Finally, CZTSSe absorbers were coated with thin CdS layer using chemical bath deposition and ZnO window layer was deposited over CZTSSe/CdS using DC sputtering technique. Fabricated 3-D solar cells were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF) analysis, Field-emission scanning electron microscopy (FE-SEM) to study their structural, compositional and morphological properties, respectively. The 3% efficiency is achieved for this kind of solar cell. Further efforts will be carried out to improve the performance of solar cell through various optimizations.

$({\eta}^5-C_5Me_5)_2BiCl$, The First Organobismuth Compound with $\pi$-bonded Cyclopentadienyl Ring Analysized by X-ray Diffractometry (X-선 회절 분석법에 의한 고리화펜타디에닐 고리가 $\pi$-결합된 최초의 유기비스무트화합물의 구조결정)

  • Lorberth, J.;Shin, Sung-Hee;Kong, Young Kun
    • Analytical Science and Technology
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    • v.11 no.1
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    • pp.42-46
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    • 1998
  • The reaction of $({\eta}^5-C_5Me_5)_2K$ with $BiCl_3$ yielded $({\eta}^5-C_5Me_5)_2BiCl$[I], the first organobismuth compound with ${\pi}$-bonded cyclopentadienyl ring. The compound I which was the violet crystal (yield, 30%) was decomposed to $PCpBiCl_2$. The Structure of $({\eta}^5-C_5Me_5)_2BiCl$ was identified as single crystal by X-ray diffraction method. The eliminated product $C_{20}H_{30}$, triclinic crystal of space group p1(Z=2) which was attached with C-C ${\sigma}$-bond of two cyclopentadienyl was defined by the structural analysis.

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