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

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X-ray and dielectric study of the phase transition in PbFe1/2Nb1/2O3-PbCo1/2W1/2O3 ceramics

  • Park, Yung;Lee, Hong-Min;Kim, Ho-Gi
    • Proceedings of the KIEE Conference
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    • 1997.07d
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    • pp.1239-1243
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    • 1997
  • A phase analysis in the solid solution of (1-x) PbFe1/2Nb1/2O3-xPbCo1/2W1/2O3 is conducted by dielectric properties, heat capacity and E-P hysteresis at x=0.1 interval. Lattice constants and superlattice intensity are analyzed by the x-ray diffraction, and the temperature - composition phase diagram is determined. The system is found to form a solid solution of perovskite structure throughout the entire composition range, but the nature of phase transitions changes from ferroelectric-paraelectric for $0{\leq}x{\leq}0.5$ to antiferroelectric-paraelectric for $0.6{\leq}x{\leq}1.0$. The transitions of ferroelectric-paraelectric and antiferroelectric-paraelectric for $0.2{\leq}x{\leq}0.5$ and for $0.6{\leq}x{\leq}0.8$, respectively, are diffuse, while those of the ferroelectric-paraelectric and the antiferroelectric-paraelectric for $0.0{\leq}x{\leq}0.1$ and $0.9{\leq}x{\leq}1.0$, respectively are sharp.

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Dielectric Properties of SCT Ceramics with the Sintering Temperature and the Thermal Treatment Time (소결온도와 열처리시간에 따른 SCT 세라믹스의 유전특성)

  • Gang, Jae-Hun;Choe, Un-Sik
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.50 no.11
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    • pp.539-543
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    • 2001
  • ln this paper, the $Sr_{l-x}Ca_xTiO_3(0\leqx\leq0.2)-based$ grain boundary layer ceramics were fabricated to measure dielectric properties with the sintering temperature and the thermal treatment time. The sintering temperature and time were $1420~15206{\circ}C$, 4hours, and the thermal treatment temperature and time of the specimen were $l150^{\circ}C$, 1, 2, 3hours, respectively. The structural and the dielectric properties were investigated by SEM, X-ray, HP4194A and K6517. The average grain size was increased with increasing the sintering temperature, but it decreased up to 15mo1% with increasing content of Ca. X-ray diffraction analysis results showed that all specimens were the cubic structure, and the main peaks were moved to right and the lattice constant were decreased with increasing content of Ca. The appropriate thermal treatment time and temperature of CuO to obtain dielectric properties of $\varepsilon_r>50000,\; tan \delta<0.05\; and \;\DeltaC<\pm10%$ were 2hrs and $l150^{\circ}C$, respectively.

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Synthesis and Crystal Structures of Di-nuclear Zinc(II) Diphenate Complexes with 1,10-Phenanthroline and 2,2'-Bipyridine

  • Koo, Bon-Kweon
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2617-2622
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    • 2011
  • Two new Zn(II) complexes, $[Zn_2(dpa)_2(phen)_2(H_2O)_2]{\cdot}H_2O$ (1) (dpa = dephenate, phen = 1,10-phenanthroline) and [$Zn_2(dpa)_2(bpy)_2(H_2O)_2$] (2) (bpy = 2,2'-bipyridine) have been synthesized and characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis, and single crystal X-ray diffraction. The X-ray analysis reveals that the structures of 1 and 2 are dinuclear zinc(II) complexes bridged by dpa dianions, respectively. The zinc ions in 1 exhibit a distorted square pyramidal environments, while the zinc ions in 2 exhibit a trigonal bipyramid geometry. In each complex, the dpa ligand is coordinated to zinc ions as a bis-monodentate.

Crystal Structures of Ba-ferrites Synthesize by Coprecipitation-Oxidation Method (공침-산화법으로 합성된 바륨페라이트의 결정구조)

  • 신형섭
    • Journal of the Korean Ceramic Society
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    • v.34 no.10
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    • pp.1045-1052
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    • 1997
  • Barium ferrites (BaFe12O19) were synthesized at the various temperature by the coprecipitation-oxidation method. X-ray diffraction Rietveld analysis for barium ferrites were performed, their microstructures were observed and their magnetic properties were measured, in order to analyze the crystal structures and determine the optimal temperature of heat-treatment. The barium ferrite, its average particle size 80 nm, was formed at 600℃ through the hematite (α-Fe2O3), but the site occupations of the Fe's in tetrahedral and bipyramidal sites and of the Ba relatively low. Increasing the heating temperature, these occupations and the magnetization increased, and the crystal c-axis decreased. These changes were very small at the heat treatment of above 800℃, but the particles were rapidly grown. It is suggested that the optimal temperature of heat-treatment is 800℃, at which temperature crystal structure is relatively stable and the particles hardly ever grow.

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Physical and Dyeing Properties of PET Ultramicrofiber Treated with DMF (DMF 처리한 초극세 PET 섬유의 물성 및 염색성)

  • 정동석;이문철
    • Textile Coloration and Finishing
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    • v.14 no.5
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    • pp.277-283
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    • 2002
  • Poly(ethylene terephthalate)(PET) filaments of regular(monodenier 2.08d) and ultramicrofiber (monodenier 0.05d) were treated with dimethylformamide(DMF) to observe the structure change of the PET such as shrinkage, density, X-ray diffraction of the UMF treated with DMF were measured. Also, dyeing experiments were performed to see the effects of DMF. The dyeability was improved by DMF treatments, and the equilibrium dye uptake increased in spite of the increase in the density and birefringence and crystallinity. The heat shrinkage appeared in PET UMF treated PET UMF treated with DMF at $80^\circ{C}$ by TMA, DSC, and Reovibron analysis and $T_m$ peak was shown by DSC analysis.

7Li-NMR and Thermal Analysis for Lithium Inserted into Artificial Carbon Material

  • O, Won Chun
    • Bulletin of the Korean Chemical Society
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    • v.22 no.4
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    • pp.367-371
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    • 2001
  • Lithium inserted into artificial carbon has been synthesized as a function of the Li concentration. The characteristics of these prepared compounds were determined from the studies using X-ray diffraction(XRD), solid nuclear magnetic resonance (NM R) spectrophotometric and differential scanning calorimeter(DSC) analysis. X-ray diffraction showed that lower stage intercalation compounds were formed with increasing Li concentration. In the case of the AG3, most compounds formed were of the stage 1 structure. Pure stage 1 structural defects of artificial graphite were not observed. 7Li-NMR data showed that bands are shifted toward higher frequencies with increasing lithium concentration; this is because non-occupied electron shells of Li increased in charge carrier density. Line widths of the Li inserted carbon compounds decreased slowly because of nonhomogeneous local magnetic order and the random electron spin direction for located Li between graphene layers. The enthalpy and entropy changes of the compounds can be obtained from the differential scanning calorimetric analysis results. From these results, it was found that exothermic and endothermic reactions of lithium inserted into artificial carbon are related to the thermal stability of lithium between artificial carbon graphene layers.

Study of Nonstoichiometry and Physical Properties of the $Nd_{1-x}(Ba_{0.40}Mg_{0.60})_{1+x}FeO_{4-y}$ System

  • 요철현;노권순;장순호
    • Bulletin of the Korean Chemical Society
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    • v.16 no.3
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    • pp.261-264
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    • 1995
  • A series of samples of the Nd1-x(Ba0.40Mg0.60)1+xFeO4-y (x=0.00, 0.10, 0.20, and 0.30) system has been synthesized at 1450 ℃ under an atmospheric air pressure. The x-ray powder diffraction analysis of the solid solutions assigns the structure of all the compositions to orthorhombic system. Mohr salt analysis shows that τ and y values increase with x value and nonstoichiometric chemical formulas of the system can be formulated from the x, τ, and y values. Oxygen vacancies are distributed along c-axis in the perovskite layer. The magnetic ordering temperature remains unchanged with x value. Electrical conductivity and activation energy depend only on the mixed valence state of Fe ion. Conduction mechanism can be suggested as the hopping of electron between eg orbitals of Fe3+ and Fe4+ ions through Fe3+-O-Fe4+ bonds. Magnetic susceptibility and electrical conductivity are discussed with the nonstoichiometric chemical formulas.

Mechanical Alloying Effect in Immiscible Cu30Mo70 Powders (비고용 Cu30Mo70계 혼합분말의 기계적 합금화 효과)

  • 이충효;이성희;이상진;권영순
    • Journal of Powder Materials
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    • v.10 no.1
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    • pp.46-50
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    • 2003
  • Lee et al. reported that a mixture of Cu and Ta, the combination of which is characterized by a positive heat of mixing, $\{Delta}H_{mix}$ of +2 kJ/㏖, can be amorphized by mechanical alloying(MA). It is our aim to investigate to what extent the MA is capable of producing a non-equilibrium phase with increasing the heat of mixing. The system chosen is the binary $Cu_{30}Mo_{70}$ with $\{Delta}H_{mix}$=+19 kJ/㏖. The mechanical alloying was carried out using a Fritsch P-5 planetary mill under Ar gas atmosphere. The vial and balls are made of Cu containing 1.8-2.0 wt.%Be to avoid contaminations arising mainly from Fe when steel balls and vial are used. The MA powders were characterized by the X-ray diffraction, EXAFS and thermal analysis. We conclude that two phase mixture of nanocrystalline fcc-Cu and bcc-Mo with grain size of 10 nm is formed by the ball-milling for a 3:7 mixture of pure Cu and Mo, the evidence for which has been deduced from the thermodynamic and structural analysis based on the DSC, X-ray diffraction and EXAFS spectra.

Synchrotron X-ray Reflectivity Studies on Nanoporous Low Dielectric Constant Organosilicate Thin Films

  • Oh, Weon-Tae;Park, Yeong-Do;Hwang, Yong-Taek;Ree, Moon-Hor
    • Bulletin of the Korean Chemical Society
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    • v.28 no.12
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    • pp.2481-2485
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    • 2007
  • Spatially resolved, quantitative, non-destructive analysis using synchrotron x-ray reflectivity (XR) with subnano-scale resolution was successfully performed on the nanoporous organosilicate thin films for low dielectric applications. The structural information of porous thin films, which were prepared with polymethylsilsesquioxane and thermally labile 4-armed, star-shaped poly(ε-caprolactone) (PCL) composites, were characterized in terms of the laterally averaged electron density profile along with a film thickness as well as a total thickness. The thermal process used in this work caused to efficiently undergo sacrificial thermal degradation, generating closed nanopores in the film. The resultant nanoporous films became homogeneous, well-defined structure with a thin skin layer and low surface roughness. The average electron density of the calcined film reduced with increase of the initial porogen loading, and finally leaded to corresponding porosity ranged from 0 to 22.8% over the porogen loading range of 0-30 wt%. In addition to XR analysis, the surface and the inner structures of films are investigated and discussed with atomic force and scanning electron microscopy images.

Spectral Analysis of $CO_2$ Corrosion Product Scales on 13Cr Tubing Steel

  • Lin, Guan-fa;Xu, Xun-yuan;Bai, Zhen-quan;Feng, Yao-rong
    • Corrosion Science and Technology
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    • v.7 no.4
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    • pp.201-207
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    • 2008
  • $CO_2$ corrosion product scales formed on 13 Cr tubing steel in autoclave and in the simulated corrosion environment of oil field are investigated in the paper. The surface and cross-section profiles of the scales were observed by scanning electron microscopy (SEM), the chemical compositions of the scales were analyzed using energy dispersion analyzer of X-ray (EDAX), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) to confirm the corrosion mechanism of the 13 Cr steel in the simulated $CO_2$ corrosion environment. The results show that the corrosion scales are formed by the way of fashion corrosion, consist mainly of four elements, i.e. Fe, Cr, C and O, and with a double-layer structure, in which the surface layer is constituted of bulky and incompact crystals of $FeCO_3$, and the inner layer is composed of compact fine $FeCO_3$ crystals and amorphous $Cr(OH)_3$. Because of the characteristics of compactness and ionic permeating selectivity of the inner layer of the corrosion product scales, 13 Cr steel is more resistant in $CO_2$ corrosion environment.