15 research outputs found
Magnetotransport Properties of Antiferromagnetic YBa_2Cu_3O_6.25 Single Crystals
In-plane and out-of-plane magnetoresistivities (MR) of antiferromagnetic
YBa_2Cu_3O_6.25 single crystals were measured in magnetic fields H applied
along the (ab) plane. In-plane MR is a superposition of two components: The
first component is strongly in-plane anisotropic, changing sign from negative
when H is parallel to the electrical current I to positive when H is
perpendicular to I. The second component is positive, quadratic in H, and
isotropic in the (ab)-plane. The out-of-plane MR displays a fourfold symmetry
upon in-plane rotation of the magnetic field, with maxima along the easy axes
of antiferromagnetic spin ordering and minima along unfavorable directions of
spin orientation (45 degrees from the Cu-O-Cu bonds).Comment: 8 pages, 4 figure
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X-ray photoemission spectroscopy (XPS) study of uranium, neptunium and plutonium oxides in silicate-based glasses
Using XPS as the principal investigative tool, we are in the process of examining the bonding properties of selected metal oxides added to silicate glass. In this paper, we present results of XPS studies of uranium, neptunium, and plutonium in binary and multicomponent silicate-based glasses. Models are proposed to account for the very diverse bonding properties of 6+ and 4+ actinide ions in the glasses
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Strains in Thermally Growing Alumina Films Measured in-situ using Synchrotron X-rays
Strains in thermally grown oxides have been measured in-situ, as the oxides develop and evolve. Extensive data have been acquired from oxides grown in air at elevated temperatures on different model alloys that form Al{sub 2}O{sub 3}. Using synchrotron x-rays at the Advanced Photon Source (Beamline 12BM, Argonne National Laboratory), Debye-Scherrer diffraction patterns from the oxidizing specimen were recorded every 5 minutes during oxidation and subsequent cooling. The diffraction patterns were analyzed to determine strains in the oxides, as well as phase changes and the degree of texture. To study a specimen's response to stress perturbation, the oxidizing temperature was quickly cooled from 1100 to 950 C to impose a compressive thermal stress in the scale. This paper describes this new experimental approach and gives examples from oxidized {beta}-NiAl, Fe-20Cr-10Al, Fe-28Al-5Cr and H{sub 2}-annealed Fe-28Al-5Cr (all at. %) alloys to illustrate some current understanding of the development and relaxation of growth stresses in Al{sub 2}O{sub 3}
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Growth strains and stress relaxation in alumina scales during high temperature oxidation
A novel X-ray technique was used, exploiting synchrotron radiation at the Advanced Photon Source at Argonne National Laboratory, to investigate the growth stresses in {alpha}-Al{sub 2}O{sub 3}. In-situ measurements of Debye-Scherrer diffraction patterns from the scale were recorded during oxidation and cooling, and the elliptical distortion of the diffraction rings was analyzed to yield the in-plane strain. Fe-28Al, Fe-40Al, Fe-40Al-0.2Hf, Fe-20Cr-10Al and Ni-50Al (at. %) were studied. Data were acquired in air at temperatures between 950-1100 C and during cool down. In all cases, the steady stage growth strain was relatively low (<0.1%) and was either tensile or compressive depending on the alloy. A higher tensile strain often existed during the initial oxidation period when transition alumina was present. Thermal stresses imposed on NiAl by reducing the sample temperature to 950 C for a period of time showed noticeable stress relaxation by creep. Different degrees of relaxation were also found during cooling depending on alloy composition and scale microstructure. On all Fe-based alloys, the first formed {alpha}-Al{sub 2}O{sub 3} was highly textured with the degree of texture decreasing with further oxidation. The relationships between stress development, scale wrinkling, oxide phase changes, and the effect of reactive element addition on growth stresses are discussed. Results are compared with other reports of growth stresses in Al{sub 2}O{sub 3} scales
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Stress Development and Relaxation in Al2O3 during Early Stage Oxidation of beta-NiAl
Using a glancing synchrotron X-ray beam (Advanced Photon Source, Beamline 12BM, Argonne National Laboratory), Debye-Scherrer diffraction patterns from thermally grown oxides on NiAl samples were recorded during oxidation at 1000 or 1100 C in air. The diffraction patterns were analyzed to determine strain and phase changes in the oxide scale as it developed and evolved. Strain was obtained from measurements of the elliptical distortion of the Debye-Scherrer rings, where data from several rings of a single phase were used. Results were obtained from {alpha}-Al{sub 2}O{sub 3} as well as from the transition alumina, in this case {theta}-Al{sub 2}O{sub 3}, which formed during the early stage. Compressive stress was found in the first-formed transition alumina, but the initial stress in {alpha}-Al{sub 2}O{sub 3} was tensile, with a magnitude high enough to cause Al{sub 2}O{sub 3} fracture. New {alpha}-Al{sub 2}O{sub 3} patches nucleated at the scale/alloy interface and spread laterally and upward. This transformation not only puts the alpha alumina in tension, but can also cause the transition alumina to be in tension. After a complete {alpha}-Al{sub 2}O{sub 3} layer formed at the interface, the strain level in {alpha}-Al{sub 2}O{sub 3} became compressive, reaching a steady state level around -75 MPa at 1100 C. To study a specimen's response to stress perturbation, samples with different thickness, after several hours of oxidation at 1100 C, were quickly cooled to 950 C to impose a compressive thermal stress in the scale. The rate of stress relaxation was the same for 1 and 3.5 mm thick samples, having a strain rate of {approx} 1 x 10{sup -8}/s. This behavior indicates that oxide creep is the major stress relaxation mechanism
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XPS study of CaO in sodium silicate glass
This paper shows that CaO added to silicate glasses behaves much like Na/sub 2/O in converting bridging oxygen sites to nonbridging sites. Good correspondence with model predictions was obtained but deviations were still sufficiently large to warrant attention. We speculate that some CaO may remain unreacted or that small-scale phase separation may occur. XPS core level shifts were monitored and possible charge-transfer effects were considered. Preliminary theoretical calculations utilizing a molecular-cluster approach were presented. XPS spectra for various glass compositions were simulated by appropriately combining local densities of state calculated for individual atoms. Dominant spectral features observed experimentally were found in the simulations. In conjunction with experiments, more carefully refined calculations will be subsequently examined. 7 figures
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Early stages in the high temperature cyclic oxidation of {beta}-NiAl: An x-ray reflectivity study
Early stages in the cyclic oxidation of {beta}-NiAl at 500{degrees}C, 600{degrees}C, 700{degrees}C and 800{degrees}C were investigated using the technique of x-ray reflectivity. By fitting the data to a model function, oxide layer thickness, roughness of the oxide-vapor interface, and the roughness of the oxide-substrate interface were obtained as a function of oxidation time and temperature of oxidation. The time dependence of the oxide thickness was observed to be logarithmic at lower temperatures (500{degrees}C and 600{degrees}C) while a conventional t{sup 0.5} kinetics was observed at the higher temperatures. Comparison of the roughness of the oxide-substrate interface with that of the oxide-vapor interface shows that for comparable oxide thicknesses and identical substrate conditions, the oxide-vapor interface was rougher than the oxide-substrate interface at all temperatures. This is consistent with the previously postulated growth mechanism (outward diffusion of cations) for oxide growth during the early stages of oxidation at these temperatures. Thus, x-ray reflectivity offers a convenient way of determining the oxide growth rates, and the roughness of the interfaces when the oxide layer is thin; this regime cannot be easily studied with the techniques that are currently used for oxidation studies
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Mechanically reliable surface oxides for high-temperature corrosion resistance
Corrosion is widely recognized as being important, but an understanding of the underlying phenomena involves factors such as the chemistry and physics of early stages of oxidation, chemistry and bonding at the substrate/oxide interface, role of segregants on the strength of that bond, transport processes through scale, mechanisms of residual stress generation and relief, and fracture behavior at the oxide/substrate interface. Because of this complexity a multilaboratory program has been initiated under the auspices of the DOE Center of Excellence for the Synthesis and Processing of Advanced Materials, with strong interactions and cross-leveraging with DOE Fossil Energy and US industry. Objective is to systematically generate the knowledge required to establish a scientific basis for designing and synthesizing improved protective oxide scales/coatings (slow-growing, adherent, sound) on high-temperature materials without compromising the requisite properties of the bulk materials. The objectives of program work at Argonne are to (1) correlate actual corrosion performance with stresses, voids, segregants, interface roughness, initial stages of oxidation, and microstructures; (2) study such behavior in growing or as-grown films; and (3) define prescriptive design and synthesis routes to mechanically reliable surface oxides. Several techniques, such as Auger electron spectroscopy, X-ray diffraction, X-ray grazing incidence reflectance, grazing-angle X-ray fluorescence, optical fluorescence, and Raman spectroscopy, are used in the studies. Tne project has selected Fe-25 wt.% Cr-20 wt.% Ni and Fe-Cr-Al alloys, which are chromia- and alumina-formers respectively, for the studies. This paper presents some of the results on early stages of oxidation and on surface segregation of elements