• Title/Summary/Keyword: powder X-ray diffraction

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Lithium-silicate coating on Lithium Nickel Manganese Oxide (LiNi0.7Mn0.3O2) with a Layered Structure

  • Kim, Dong-jin;Yoon, Da-ye;Kim, Woo-byoung;Lee, Jae-won
    • Journal of Powder Materials
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    • v.24 no.2
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    • pp.87-95
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    • 2017
  • Lithium silicate, a lithium-ion conducting ceramic, is coated on a layer-structured lithium nickel manganese oxide ($LiNi_{0.7}Mn_{0.3}O_2$). Residual lithium compounds ($Li_2CO_3$ and LiOH) on the surface of the cathode material and $SiO_2$ derived from tetraethylorthosilicate are used as lithium and silicon sources, respectively. Powder X-ray diffraction and scanning electron microscopy with energy-dispersive spectroscopy analyses show that lithium silicate is coated uniformly on the cathode particles. Charge and discharge tests of the samples show that the coating can enhance the rate capability and cycle life performance. The improvements are attributed to the reduced interfacial resistance originating from suppression of solid-electrolyte interface (SEI) formation and dissolution of Ni and Mn due to the coating. An X-ray photoelectron spectroscopy study of the cycled electrodes shows that nickel oxide and manganese oxide particles are formed on the surface of the electrode and that greater decomposition of the electrolyte occurs for the bare sample, which confirms the assumption that SEI formation and Ni and Mn dissolution can be reduced using the coating process.

Peculiarities of SHS and solid state synthesis of $ReBa_{2}Cu_{3}O_{7-x}$ materials

  • Sho, Dea-Wha;Li, Yingmei;Cho, Yong-Joon;Kim, Tae-Wan;Korobova, N.;Isaikina, O.;Mansurov, Z.;Baydeldinova, A.;Ksandopoulo, G.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2001.07a
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    • pp.620-623
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    • 2001
  • The peculiarities of using Self-propagating High-temperature Synthesis (SHS) and solid state phase synthesis for production of high temperature superconductor materials are discussed. Oxide superconductors with general formula $ReBa_2$$Cu_3$$O_{7-x}$ (Re= Y, Yb, Sm, Nd) have been made with using barium oxide initial powder instead of traditional barium carbonate. X-ray powder diffraction showed a single phase orthorhombic perovskite structure was produced in all reactions. Phenomena observed during the grinding of the reactant mixture are presented. Mechano-chemical activation - as a pretreatment of the reactant mixture - strongly influences the kinetic parameters, the reaction mechanism, and the composition and structure of the final product.

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PREFERRED ORIENTATION OF TIN FILM STUDIED BT A REAL TIME SYNCHROTRON X-RAY SCATTERING

  • Je, J.H.;Noh, D.Y.
    • Journal of the Korean institute of surface engineering
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    • v.29 no.5
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    • pp.399-406
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    • 1996
  • The orientational cross-over phenomena in an RF sputtering growth of TiN films were studied in an in-situ, real-time synchrotron x-ray scattering experiment. For the films grown with pure Ar sputtering gas, the cross-over from the more strained (002)-oriented grains to the less strained (111)-oriented grains occurred as the film thickness was increased. As the sputtering power was increased, the cross-over thickness, at which the growth orientation changes from the <002> to the <111> direction, was decreased. The addition of $N_2$ besides Ar as sputtering gas suppressed the cross-over, and consequently resulted in the (002) preferred orientation without exhibiting the cross-over. We attribute the observed cross-over phenomena to the competition between the surface and the strain energy. The x-ray powder diffraction, the x-ray reflectivity, and the ex-situ AFM surface topology study consistently suggest that the microscopic growth front was in fact always the (002) planes. In the initial stage of growth, the (002) planes were aligned to the substrate surface to minimize the surface energy. At later stages, however, the (002) growth front tilted away from the surface by about $60^{\circ}$ to relax the strain, which caused the cross-over of the preferred growth direction to the <111> direction.

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Crystal Structures and Electrochemical Properties of LiNi1-xMgxO2 (0≤x≤0.1) for Cathode Materials of Secondary Lithium Batteries (리튬 이차전지의 양극 활물질 LiNi1-xMgxO2 (0≤x≤0.1)의 결정구조 및 전기화학적 특성)

  • Kim, Deok-Hyeong;Jeong, Yeon Uk
    • Korean Journal of Metals and Materials
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    • v.48 no.3
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    • pp.262-267
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    • 2010
  • $LiNi_{1-x}Mg_xO_2$(x=0, 0.025, 0.05, 0.075, 0.1) samples were synthesized by the solid-state reaction method. The crystal structure was analyzed by X-ray powder diffraction and Rietveld refinement. $LiNi_{1-x}Mg_xO_2$samples give single phases of hexagonal layered structures with a space group of R-3m. The calculated cation-anion distances and angles from the Rietveld refinement were changed with Mg contents in $LiNi_{1-x}Mg_xO_2$. The thicknesses of $NiO_2$ slabs were increased and the distances between the $NiO_2$ slabs were decreased with the increase in Mg contents in the samples. The electrical conductivities of sintered $LiNi_{1-x}Mg_xO_2$ samples were around $10^{-2}$ S/cm at room temperature. The electrochemical performances of $LiNi_{1-x}Mg_xO_2$were evaluated by coin cell test. Compared to $LiNiO_2$, $LiNi_{0.95}Mg_{0.05}O_2$ exhibited improved high-rate capability and cyclability due to the well-ordered layered structure by doping of Mg ion.

Mineral Composition of the Sediment of Ulleung Basin, Korea (울릉분지 퇴적물의 광물조성)

  • Son, Byeong-Kook;Kim, Hag-Ju;Ahn, Gi-Oh
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.2
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    • pp.115-127
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    • 2009
  • Mineral quantification was performed on sediments of the Ulleung basin by X-ray powder diffraction and the computer software based on Rietveld quantification method. The sediments are dominated by amorphous opal-A with quartz, feldspars, micas, clays, calcite, and pyrite. The opal-A shows iterative variation in abundance with increasing burial depth. In addition, the relative abundance of opal-A is coincident with abundance of organic carbon contents, indicating that the Ulleung sediment consists mostly of amorphous silica derived from organism in the pelagic environment. Upward increase in the abundance of opal-A is markedly shown in the cores located in the slope region. On the other hand, there is a distinct tendency that the abundance of calcite is inversely proportional to that of opal-A. This indicates that the abundance of opal-A increases during the rise of sea level. Also, the fall of sea level lowers the abundance of opal-A.

X-ray / gamma ray radiation shielding properties of α-Bi2O3 synthesized by low temperature solution combustion method

  • Reddy, B. Chinnappa;Manjunatha, H.C.;Vidya, Y.S.;Sridhar, K.N.;Pasha, U. Mahaboob;Seenappa, L.;Sadashivamurthy, B.;Dhananjaya, N.;Sathish, K.V.;Gupta, P.S. Damodara
    • Nuclear Engineering and Technology
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    • v.54 no.3
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    • pp.1062-1070
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    • 2022
  • In the present communication, pure and stable α-Bismuth Oxide (Bi2O3) nanoparticles (NPs) were synthesized by low temperature solution combustion method using urea as a fuel and calcined at 500℃. The synthesized sample was characterized by using powder X-ray Diffraction (PXRD), Scanning Electron Microscopy (SEM), Energy dispersive X-ray analysis (EDAX), Transmission Electron Microscopy (TEM), Fourier Transform Infrared Spectroscopy (FTIR) and UV-Visible absorption spectroscopy. The PXRD pattern confirms the formation of mono-clinic, stable and low temperature phase α-Bi2O3. The direct optical energy band gap was estimated by using Wood and Tauc's relation which was found to be 2.81 eV. The characterized sample was studied for X-ray/gamma ray shielding properties in the energy range 0.081-1.332 MeV using NaI (Tl) detector and multi channel analyzer (MCA). The measured shielding parameters agrees well with the theory, whereas, slight deviation up to 20% is observed below 356 keV. This deviation is mainly due to the influence of atomic size of the target medium. Furthermore an accurate theory is necessary to explain the interaction of X-ray/gamma ray with the NPs.The present work opens new window to use this facile, economical, efficient, low temperature method to synthesize nanomaterials for X-ray/gamma ray shielding purpose.

Crystallization of Forsterite Xerogel under Carbon Dioxide: A New Crystalline Material Synthesized by Homogeneous Distribution of Carbonaceous Component into Forsterite Xerogel

  • 송미영;김수주;권혜영;박선희;박동곤;권호진;권영욱;James M. Burlitch
    • Bulletin of the Korean Chemical Society
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    • v.20 no.5
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    • pp.517-524
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    • 1999
  • By heating the magnesiumsilicate (Mg2SiO4:forsterite) xerogel in carbon dioxide, carbonaceous component was intentionally introduced into the amorphous solid precursor. Carbon was introduced homogeneously as unidentate carbonate. Upon being heated at 800 。C in carbon dioxide, the xerogel which had homogeneously distributed carbonaceous component in it crystallized into a single phase product of a new crystalline material, which had approximate composition of Mg8Si4Ol8C. The powder X-ray diffraction pattern of the new crystalline material did not match with any known crystalline compound registered in the powder diffraction file. Crystallization from amorphous xeroget to the new crystalline phase occurred in a very narrow range of temperature, from 750 。C to 850 。C in carbon dioxide, or in dty oxygen. Upon being heated above 850 。C, carbonaceous component was expelled from the product, accompanied by irreversible transition from the new crystalline material to forsterite.

Syntheses of Cu-In-Ga-Se/S nano particles and inks for solar cell applications

  • Jung, Duk-Young
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.08a
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    • pp.295-295
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    • 2010
  • Nanoparticles of the compound semiconductor, Cu(In, Ga)Se2 (CIGS), were synthesized in solution under ambient pressure below $100^{\circ}C$ and characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), optical absorption spectroscopy and energy-dispersive X-ray (EDX) analyses. These materials have chalcopyrite crystal structures and the particle sizes less than 100 nm. Synthetic conditions were studied for the crystallized CIGS nanoparticles formation to prevent from side products of Cu2Se, Cu2-xSe, and CuSe etc. The single phase CIGS nanoparticles were applied to coating of thin films photovoltaic cells. The electro deposition of CIGS thin films is also a good non-vacuum technology and under investigation. In aqueous solutions, the different chemical compositions of CIGS thin films were obtained, depending on pH, concentration of starting materials and deposition potentials. The surface morphology of the prepared CIGS thin films depends on the complexing ligands to the solutions during the electrochemical deposition.

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In-situ Phase Transition Study of Minerals using Micro-focusing Rotating-anode X-ray and 2-Dimensional Area Detector (집속 회전형 X-선원과 이차원 검출기를 이용한 광물의 실시간 상전이 연구)

  • Seoung, Dong-Hoon;Lee, Yong-Moon;Lee, Yong-Jae
    • Economic and Environmental Geology
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    • v.45 no.2
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    • pp.79-88
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    • 2012
  • The increased brightness and focused X-ray beams now available from laboratory X-ray sources facilitates a variety of powder diffraction experiments not practical using conventional in-house sources. Furthermore, the increased availability of 2-dimensional area detectors, along with implementation of improved software and customized sample environmental cells, makes possible new classes of in-situ and time-resolved diffraction experiments. These include phase transitions under variable pressure- and temperature conditions and ion-exchange reactions. Examples of in-situ and time-resolved studies which are presented here include: (1) time-resolved data to evaluate the kinetics and mechanism of ion exchange in mineral natrolite; (2) in-situ dehydration and thermal expansion behaviors of ion-exchanged natrolite; and (3) observations of the phases forming under controlled hydrostatic pressure conditions in ion-exchanged natrolite. Both the quantity and quality of the in-situ diffraction data are such to allow evaluation of the reaction pathway and Rietveld analysis on selected dataset. These laboratory-based in-situ studies will increase the predictability of the follow-up experiments at more specialized beamlines at the synchrotron.

Detonation Initiation via Surface Chemical Reaction of Laser-Ablated Aluminum Sample (표면화학 반응을 통한 Laser-Ablated 알루미늄의 Detonation 현상 연구)

  • Kim, Chang-Hwan;Yoh, Jai-Ick
    • Transactions of the Korean Society of Mechanical Engineers B
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    • v.36 no.2
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    • pp.197-204
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    • 2012
  • We explore the evolution of metal plasma generated by high laser irradiances and its effect on the surrounding air by using shadowgraph images after laser pulse termination and X-ray diffraction (XRD) of aluminum plasma ablated by a high-power laser pulse (>1000 mJ/pulse) and oxygen from air. Hence, the formation of laser-supported detonation and combustion processes has been investigated. The essence of this paper is in observing the initiation of chemical reaction between the ablated aluminum plasma and oxygen from air by the high-power laser pulse (>1000 mJ/pulse) and in conducting a quantitative comparison of the chemically reactive laser-initiated waves with the classical detonation of an exploding aluminum (dust) cloud in air. The findings in this work may lead to a new method of initiating detonation from a metal sample in its bulk form without any need to mix nanoparticles with oxygen for initiation.