• Title/Summary/Keyword: X-ray structure analysis

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Cycloplatinated Complexes of Thiosemicarbazones. Synthesis and Crystal Structure of [$Ph_2PC_6H_4CHNNC(S)NHCH_3PtCl$]

  • 유동원;강상욱;고재정;최문근
    • Bulletin of the Korean Chemical Society
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    • v.18 no.3
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    • pp.305-310
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    • 1997
  • The synthesis and characterization of the platinum heterocyclic carboxaldehyde thiosemicarbazone complexes [NC5H4CRNNC(S)NHR'PtCl] (R=H, R'=CH3(1); R=CH3, R'=CH3(2); R=CH3, R=H(3)) and diphenylphosphinophenyl carboxaldehyde thiosemicarbazone complexes [Ph2PC6H4CHNNC(S)NHRPtCl] (R=CH3(5); R=iC3H7(6); R=Ph(7)) are described. Compounds 1-3 were prepared by reaction of Pt(SEt2)2Cl2 with 2-acetylpyridine-4-alkylthiosemicarbazone in the presence of NEt3. Compounds 5-7 were prepared using Pt(SEt2)2Cl2 in toluene with diphenylphosphinophenyl carboxaldehyde alkylthiosemicarbazone. The compounds have been characterized by microanalysis, NMR (1H, 13C, 31P) spectroscopy, and single-crystal X-ray diffraction. X-ray single crystal diffraction analysis reveals that compound 5 is a mononuclear platinum compound with P,N,S-coordination mode.

The Crystallograpic and Magnetic Properties of EuFeO3 Doped with in ions (In 이온을 첨가한 $EuFeO_{3}$의 결정구조 및 자기적 성질)

  • 김정기;서정철;한은주
    • Journal of the Korean Magnetics Society
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    • v.4 no.4
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    • pp.335-339
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    • 1994
  • The crystallograpic and magnetic properties of $Eu(Fe_{1-x}In_{x})O_{3}$ (x=0, 0.03과 0.05) have been studied by the methods of X-ray diffraction, $M\"{o}ssbauer$ spectroscopy, and magnetic hysteresis measurement at room temperature. The X-ray results show that the samples have a crystal structure of orthorhombic and unit cell volume of the crystal with the exception of the sample of x=0 increases as increasing the In concentration. In the analysis assuming two sets of six-line of $M\"{o}ssbauer$ spectra, it is found that the magnetic hyperfine field in each of sets decreases increasing x. The linewidth of the absorption lines for the samples increased as increasing x. This implies that the data involve a sum of several hyperfine patterns which have intensity being proportional to $_{n}P_{z}(x)$, the probability of an environment with z such Fe neighbors. The magnetic hysteresis curves show decrease of $M_{s}$ and increase of $H_{c}$ of the samples with increasing x.

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Growth of GaN epilayer on the Si(001) substrate by hot wall epitaxy (Si(001) 기판 위에 HWE 방법으로 성장한 GaN 박막 성장)

  • Lee, H.;Youn, C.J.;Yang, J.W.;Shin, Y.J.
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.3
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    • pp.273-279
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    • 1999
  • The home-made hot wall epitaxy (HWE) system was utilized for GaN epitaxial layer growth on the Si(001) substrate. It was appeared that GaN epilayer grow with mixed phase of Zinc blende and Wurtzite structure from photoluminescence (PL) and x-ray diffraction (XRD) analysis at the room temperature. We found that intial growth layer has Wurtzite structure from photoluminescence (PL) and x-ray diffractio (XRD) analyses at the room temperature. Wefound that initial growth layer has Wurtzite structure when initial deposition time, the temperature of substrate and source are 4 min, $720^{\circ}C$ and $860^{\circ}C$ respectively, and at the epi growth process GaN, epilayer was grown with relatively stable Wurtzite structure when the temperature of substrate and source are $1020^{\circ}C$ and $910^{\circ}C$ respectively.

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Study of Nonstoichiometry and Physical Properties of the $Ca_xEu_{1-x}FeO_{3-y}$ System

  • Roh, Kwon-Sun;Ryu, Kwang-Sun;Ryu, Kwang-Hyun;Yo, Chul-Hyun
    • Bulletin of the Korean Chemical Society
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    • v.15 no.7
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    • pp.541-545
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    • 1994
  • A series of samples of the ${Ca_xEu_{1-x}FeO_{3-y}$ (x=0.00, 0.25, 0.50, 0.75, and 1.00) system has been prepared at $1,250^{\circ}C$ under an atmospheric air pressure. X-ray diffraction analysis of the solid solution assigns the structure of the compositions of x=0.00, 0.25, 0.50, and 0.75 to the orthoferrite-type orthorhombic system, and that of x=1.00 to the brownmillerite-type orthorhombic one. The mole ratios of $Fe^{4+}$ ion in the solid solutions or ${\tau}$ values were determined by the Mohr's salt analysis and nonstoichiometric chemical formulas of the system were formulated from x, ${\tau}$, and y values. From the result of the Mossbauer spectroscopy, the coordination and magnetic property of the iron ion are discussed. The electrical conductivities are measured as a function of temperature. The activation energy is minimum at the composition of x=0.25. The conduction mechanism can be explained by the hopping of electrons between the mixed valences of $Fe^{3+}\;and\;Fe^{4+}$ ions.

Structural and electrical properties of lead free ceramic: Ba(Nd1/2Nb1/2)O3

  • Nath, K. Amar;Prasad, K.;Chandra, K.P.;Kulkarni, A.R.
    • Advances in materials Research
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    • v.2 no.2
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    • pp.119-131
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    • 2013
  • Impedance and electrical conduction studies of $Ba(Nd_{1/2}Nb_{1/2})O_3$ ceramic prepared using conventional high temperature solid-state reaction technique are presented. The crystal symmetry, space group and unit cell dimensions were estimated using Rietveld analysis. X-ray diffraction analysis indicated the formation of a single-phase cubic structure with space group $Pm\bar{3}m$. Energy dispersive X-ray analysis and scanning electron microscopy studies were carried to study the quality and purity of compound. The circuit model fittings were carried out using the impedance data to find the correlation between the response of real system and idealized model electrical circuit. Complex impedance analyses suggested the dielectric relaxation to be of non-Debye type and negative temperature coefficient of resistance character. The correlated barrier hopping model was employed to successfully explain the mechanism of charge transport in $Ba(Nd_{1/2}Nb_{1/2})O_3$. The ac conductivity data were used to evaluate the density of states at Fermi level, minimum hopping length and apparent activation energy.

Stage transformation characteristice of Li, K and Na-graphite intercalation compounds (Li, K과 Na-흑연 층간화합물의 stage 전이특성)

  • 오원춘;임창성;오근호;고영신
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.1
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    • pp.83-90
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    • 1998
  • Stage transformation characteristics of Li, K and Na-graphite deintercalation compounds (GDICs) were studied under consideration of a deintercalation mechanism of the intercalants between carbon layers. Li-graphite intercalation compounds (GICs) synthesized by a controlling temperatures and pressures have been spontaneously decomposed in the atmosphere. By X-ray differaction analysis the $d_{001}$-values of stage 1 and 2 were identified to be 3.71 and 7.06 $\AA$, respectively. After 6 weeks, the deintercalation reaction of the Li-GICs ceased and only residual compounds could be observed. K-GICs were synthesized by the modified two-bulb method resulting in structural stabilities and stage transitions. By X-ray diffraction analysis the very stable K-graphite residue compounds were observed after 10 weeks. Na-GICs with stage 1 and 2 were synthesized using the high temperature and pressure technique. The temperature dependence of a deintercalation reaction and a thermal stability of Na-GICs were discussed. The structure changes of the Na-GDICs depending on heating rates were identified by X-ray diffraction. According to the deintercalation process, the stage transformations could be attributed to irregular deintercalations of the GDICs with disordered stage.

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Spectral and Geometrical Study of Two Cadmium Complexes, mer-R,S-[Cd(aepn)2]X2 (X: I-, Cl-, aepn: N-(2-Aminoethyl)-1,3-propanediamine) Supported by Solution Experiments

  • Hakimi, Mohammad;Mardani, Zahra;Moeini, Keyvan
    • Journal of the Korean Chemical Society
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    • v.57 no.4
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    • pp.447-454
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    • 2013
  • In this research, two new complexes of N-(2-aminoethyl)-1,3-propanediamine (aepn), $[Cd(aepn)_2]I_2$ (1) and $[Cd(aepn)_2]Cl_2{\cdots}H_2O$ (2), were prepared and identified by elemental analysis, FT-IR, Raman spectroscopy and single-crystal X-ray diffraction. Geometry around the cadmium atom in two complexes by coordination of six nitrogen atoms of two aepn is distorted octahedral. If distortion in the mer-$[Cd(aepn)_2]^{2+}$ cation is disregarded, it has a $C_2$ axis and $C_2$ symmetry. The cyclic voltammetry experiments were carried out to study the complexation process. Two structural surveys on coordination modes and complexes of aepn are presented. A study was carried out using CSD data to estimate the averages of bond lengths for different types of the Cd-N bonds. It was found that the intermolecular $N-H{\cdots}I$, $C-H{\cdots}I$ hydrogen bonds in 1 and $N-H{\cdots}Cl$, $N-H{\cdots}O$, $C-H{\cdots}O$, $O-H{\cdots}Cl$ in 2 stabilized the crystal networks.

A study on the mechanical properties of structure rolled steel and stainless steel for the CO2 welding (구조용 압연강재와 스테인리스강재의 CO2 용접에 대한 기계적 특성연구)

  • Lim, Jong Young;Yoon, Myung Jin;Kim, Tae Hyun;Kim, Sang Youn;Kim, Tae Gyu
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.4
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    • pp.207-212
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    • 2013
  • It is well known that fatigue failure occur on welded structures in industrial application due to the repetitive load force. In order to decrease the fatigue failure, we analysed the mechanical properties based on their structural aspect, roll steel (SS 400) welded onto stainless steels (STS 304) by $CO_2$ gas as well as structure roll steel welded onto itself. We compared the hardness, tensile and fatigue properties with two kinds of samples which had no defects on the welding part observed by X-ray topographic analysis. It was recognized that the tensile and fatigue strength of SS 400 welded onto itself by $CO_2$ gas was higher than that of SS 400 welded onto STS 304.

The influence of X ray beam angulation on the fractal analysis of trabecular architecture in human dry mandible using standardized tile counting method

  • Lee Kyung-Hee;Lee Sun-Bok;An Chang-Hyeon;Heo Min-Suk;Yi Won-Jin;Huh Kyung-Hoe;Park Moo-Soon;Lee Sam-Sun;Choi Soon-Chul
    • Imaging Science in Dentistry
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    • v.34 no.4
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    • pp.179-182
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    • 2004
  • Purpose: The purpose of this study is to examine the effects of X-ray beam angulation on the fractal dimension of trabecular bone structure of human dry mandible using the tile counting method. Materials and Methods: We divided 5 human dry mandibles into an angle and a molar groups depending on the regions and deciding the region of interest (ROI). When contrasted with the ROI, the inferior cortex was appointed to be low and the lines perpendicular to the buccal cortex were appointed to be the standard angle. Direct digital intraoral radiographs were obtained from 9 different projection angles. We analyzed statistically the fractal dimension using the tile counting method. Results: There was a statistically significant difference in the fractal dimension of the regions and the mandibles, but there was no statistically significant difference in the fractal dimension according to the X-ray beam angulation. Conclusion : There is no statistically significant effect of the angle of the projection on the fractal dimension of trabecular bone structure of a human dry mandible according to the tile counting method.

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Synthesis and Structural Analysis of a New Layered Cobalt(II) Compound with p-Toluenesulfonic Acid : $[Co(H_2O)_6](CH_3C_6H_4SO_3)_2$ (p-Toluenesulfonate를 가진 새로운 코발트(II) 층상 화합물의 합성과 구조 분석)

  • Kim, Chong-Hyeak;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.534-538
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    • 2000
  • The title compound, $[Co(H_2O)_6](CH_3C_6H_4SO_3)_2$, has been prepared and characterized by X-ray crystallography. The crystal structure of the compound demonstrates a layered material constituted by hexaaquacobalt (II) cations and p-toluenesulfonate anions. Geometrical environment of the cobalt atom is octahedrally coordinated by water molecules. The p-toluenesulfonate anions are arranged with the sulfonate groups turned toward opposite side of the layer, alternately. The layered structure is stabilized by the hydrogen bondings between the ligated water molecules and the anionic sulfonate oxygen atoms.

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