• Title/Summary/Keyword: In situ X-ray diffraction

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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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Effect of Various Supports on the Physico-chemical Properties of V-Sb Oxides in the Oxidative Dehydrogenation of Isobutane

  • Shamilov, N.T.;Vislovskiy, V.P.
    • Journal of the Korean Chemical Society
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    • v.55 no.5
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    • pp.812-818
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    • 2011
  • [ $V_{0.9}Sb_{0.1}O_x$ ]systems, bulk and deposited on different supports (five types of ${\gamma}$-aluminas, ${\alpha}$-alumina, silica-alumina, silica gel, magnesium oxide), have been tested in the oxidative dehydrogenation (ODH) of iso-butane. This statement is derived from the data obtained by a set of characterisation techniques(specific surface area measurements, X-ray diffraction, X-ray photoelectron spectroscopy, laser Raman spectroscopy, in situ differential scanning calorimetry and in situ diffuse reflectance-absorption infrared Fourier transform spectroscopy).

Oxidation Process of Epitaxial Ni(111) Thin Films Deposited on GaN/Sapphire(0001) Substrates (GaN/Sapphire(0001) 기판위에 증착한 epitaxial Ni(111) 박막의 산화 과정)

  • Seo, S.H.;Kang, Hyon-Chol
    • Journal of the Korean Society for Heat Treatment
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    • v.22 no.6
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    • pp.354-360
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    • 2009
  • This paper reports the oxidation mechanism of epitaxial Ni thin films grown on GaN/sapphire(0001) substrates, investigated by real-time x-ray diffraction and scanning electron microscopy. At the initial stage of oxidation process, a thin NiO layer with a thickness of ${\sim}50\;{\AA}$ was formed on top of the Ni films. The growth of such NiO layer was saturated and then served as a passive oxide layer for the further oxidation process. For the second oxidation stage, host Ni atoms diffused out to the surfaces of initially formed NiO layer through the defects running vertically to form NiO grains, while the sites that were occupied by host Ni, became voids. The crystallographic properties of resultant NiO films, such as grain size and mosaic distribution, rely highly on the oxidation temperatures.

Vapor Phase Epitaxy of Magnesium Oxide on Si(001) Using a Single Precursor

  • Lee, Sun-Sook;Lee, Sung-Yong;Kim, Chang G.;Lee, Sang-Heon;Nah, Eun-Ju;Kim, Yunsoo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.122-122
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    • 2000
  • Magnesium oxide is thermodynamically very stable, has a low dielectric constant and a low refractive index, and has been widely used as substrate for growing various thin film materials, particulary oxides of the perovskite structure. There has been a considerable interest in integrating the physical properties of these oxides with semiconductor materials such as GaAs and Si. In this regard, it is considered very important to be able to grow MgO buffer layers epitaxially on the semiconductors. Various oxide films can then be grown on such buffer layers eliminating the need for using MgO single crystal substrates. Vapor phase epitaxy of magnesium oxide has been accomplished on Si(001) substrates in a high vacuum chamber using the single precursor methylmagnesium tert-butoxide in the temperature range 750-80$0^{\circ}C$. For the epitaxy of the MgO films, SiC buffer layers had to be grown on Si(001). The films were characterized by reflection high energy electron diffraction (RHEED) in situ in the growth chamber, and x-ray diffraction (XRD), x-ray pole figure analysis, scanning electron microscopy (SEM), and x-ray photoelectron spectroscopy (XPS) after the growth.

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Metal-insulator Transition in $(Sr_{0.75},\;La_{0.25})TiO_3$ Ultra-thin Films

  • Choi, Jae-Du;Choi, Eui-Young;Lee, Yun-Sang;Lee, Jai-Chan
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.10a
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    • pp.19.2-19.2
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    • 2011
  • The $(Sr_{0.75},\;La_{0.25})TiO_3$ (SLTO) ultra-thin films with various thicknesses have been grown on Ti-O terminated $SrTiO_3$(100) substrate using Laser-Molecular Beam Epitaxy (Laser MBE). By monitoring the in-situ specular spot intensity oscillation of reflection high energy electron diffraction (RHEED), we controlled the layer-by-layer film growth. The film structure and topography were verified by atomic force microscopy (AFM) and high resolution thin film x-ray diffraction by the synchrotron x-ray radiation. We have also investigated the electronic band structure using x-ray absorption spectroscopy (XAS). The ultra thin SLTO film exhibits thickness driven metal-insulator transition around 8 unit cell thickness when the film thickness progressively reduced to 2 unit cell. The SLTO thin films with an insulating character showed band splitting in Ti $L_3-L_2$ edge XAS spectrum which is attributed to Ti 3d band splitting. This narrow d band splitting could drive the metal-insulator transition along with Anderson Localization. In optical conductivity, we have found the spectral weight transfer from coherent part to incoherent part when the film thickness was reduced. This result indicates the possibility of enhanced electron correlation in ultra thin films.

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A Study on the Structural and Electrochemical Properties of Li0.99Ni0.46Mn1.56O4 Cathode Material Using Synchrotron based in-situ X-ray Diffraction

  • Choi, Sol;Yoon, JeongBae;Muhammad, Shoaib;Yoon, Won-Sub
    • Journal of Electrochemical Science and Technology
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    • v.4 no.1
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    • pp.34-40
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    • 2013
  • The structural and electrochemical properties of $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ ($Fd{\bar{3}}m$, disordered spinel) cathode material were studied and compared with stoichiometric $LiNi_{0.5}Mn_{1.5}O_4$ ($P4_332$, ordered spinel). First cycle discharge capacity of $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ was similar to that of $LiNi_{0.5}Mn_{1.5}O_4$ at C/3 and 1C rate, but cycling performance of $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ was better than that of $LiNi_{0.5}Mn_{1.5}O_4$ especially at high rate of 1C. This can be explained by performing synchrotron based in-situ XRD and results of GITT measurements. It is considered that faster lithium ion diffusion in the $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ cathode results in the improvement of the rate capability. To study structural changes during cycling, synchrotron in-situ XRD patterns of both the samples were recorded at C/3 and 1C rate. Compared to stoichiometric $LiNi_{0.5}Mn_{1.5}O_4$, disordered $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ spinel sample has pseudo one phase behavior and one step phase transition between two cubic phases. So, $LiNi_{0.5}Mn_{1.5}O_4$ would experience a much greater strain and stress, originating from the two phase transitions between three cubic phases and suffer from capacity loss during cycling especially at high rate.

Synthesis of Fe-TiB2 Nanocomposite by a combination of mechanical activation and heat treatment

  • Hyunh, Xuan Khoa;Nguyen, Quoc Tuan;Kim, Ji-Sun;Gang, Tae-Hun;Kim, Jin-Cheon;Gwon, Yeong-Sun
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2012.05a
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    • pp.91.2-91.2
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    • 2012
  • The TiB2-reinforced iron matrix nanocomposite (Fe-TiB2) was in-situ fabricated from titanium hydride (TiH2) and iron boride (FeB) powders by a simple and cost-effective process that combines the mechanical activation (MA) and a subsequent heat treatment (HT). Effect of milling factors and synthesized temperatures on the formation of the nanocomposite were presented and discussed. A differential thermal analyser (DSC-TG) was employed for examination of thermal behavior of MAed powders. Phases of the nanocomposite were confirmed by X-ray diffraction analysis (XRD). The morphologies and microstructure of nanocomposite were investigated by field emission-scanning electron microscopy (FE-SEM) and energy-dispersive X-ray spectroscopy (EDS). Phase composition and distribution were analyzed by electron probe X-ray microanalysis (EPMA). Results showed that TiB2 particles formed in nanoscale were uniformly distributed in alloyed Fe matrix.

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Effects of Sputter Parameters on Electrochromic Properties of Tungsten Oxide Thin Films Grown by RF Sputtering

  • Nah, Yoon-Chae
    • Korean Journal of Materials Research
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    • v.21 no.12
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    • pp.703-707
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    • 2011
  • The electrochromic properties of tungsten oxide films grown by RF sputtering were investigated. Among the sputter parameters, first the $Ar:O_2$ ratios were controlled with division into only an $O_2$ environment, 1:1 and 4:1. The structure of each film prepared by these conditions was studied by X-ray diffraction, X-ray photoelectron spectroscopy and Rutherford backscattering spectroscopy. The sputter-deposited tungsten oxide films had an amorphous structure regardless of the $Ar:O_2$ ratios. The chemical compositions, however, were different from each other. The stoichiometric structure and low-density film was obtained at higher $O_2$ contents. Electrochemical tests were performed by cyclic voltammetry and chronoamperometry at 0.05 M $H_2SO_4$ solutions. The current density and charge ratio was estimated during the continuous potential and pulse potential cycling at -0.5 V and 1.8 V, respectively. The film grown in a higher oxygen environment had a higher current density and a reversible charge reaction during intercalation and deintercalation. The in-situ transmittance tests were performed by He-Ne laser (633 nm). At higher oxygen contents, a big transmittance difference was observed but the response speed was too slow. This was likely caused by higher film resistivity. Furthermore, the effect of sputtering pressure was also investigated. The structure and surface morphology of each film was observed by X-ray diffraction and scanning electron microscopy. A rough surface was observed at higher sputtering pressure, and this affected the higher transmittance difference and coloration efficiency.