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  • lattice parameters  (3)
  • resistive heating  (2)
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  • 1
    Publikationsdatum: 2024-02-05
    Beschreibung: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉Penetrating, high‐energy synchrotron X‐rays are in strong demand, particularly for high‐pressure research in physics, chemistry and geosciences, and for materials engineering research under less extreme conditions. A new high‐energy wiggler beamline P61 has been constructed to meet this need at PETRA III in Hamburg, Germany. The first part of the paper offers an overview of the beamline front‐end components and beam characteristics. The second part describes the performance of the instrumentation and the latest developments at the P61B endstation. Particular attention is given to the unprecedented high‐energy photon flux delivered by the ten wigglers of the PETRA III storage ring and the challenges faced in harnessing this amount of flux and heat load in the beam. Furthermore, the distinctiveness of the world's first six‐ram Hall‐type large‐volume press, Aster‐15, at a synchrotron facility is described for research with synchrotron X‐rays. Additionally, detection schemes, experimental strategies and preliminary data acquired using energy‐dispersive X‐ray diffraction and radiography techniques are presented.〈/p〉
    Beschreibung: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉The operation of the P61B endstation large‐volume press and optics of P61 are reviewed. The instrumentation at P61B, including the large‐volume press, detection systems and data acquisition for 〈italic〉in situ〈/italic〉 high‐pressure experiments are described.〈boxed-text position="anchor" content-type="graphic" xml:lang="en"〉〈graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:16005775:jsy2ju5040:jsy2ju5040-fig-0001"〉 〈/graphic〉〈/boxed-text〉〈/p〉
    Schlagwort(e): ddc:550.724 ; extreme conditions ; high‐pressure ; large‐volume press ; energy‐dispersive X‐ray diffraction ; radiography ; resistive heating ; ultrasonic interferometry ; acoustic emissions detection
    Sprache: Englisch
    Materialart: doc-type:article
    Standort Signatur Erwartet Verfügbarkeit
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  • 2
    Publikationsdatum: 2023-07-21
    Beschreibung: A band width determination using the first derivative of the band profile systematically underestimates the true Bragg angle. Corrections are proposed to compensate for the resulting offset Δa/a of the mean lattice parameters derived from as many Kikuchi band widths as possible. For dynamically simulated Kikuchi patterns, Δa/a can reach up to 8% for phases with a high mean atomic number Z, whereas for much more common low‐Z materials the offset decreases linearly. A predicted offset Δa/a = f(Z) is therefore proposed, which also includes the unit‐cell volume and thus takes into account the packing density of the scatterers in the material. Since Z is not always available for unknown phases, its substitution by Zmax, i.e. the atomic number of the heaviest element in the compound, is still acceptable for an approximate correction. For simulated Kikuchi patterns the offset‐corrected lattice parameter deviation is Δa/a 〈 1.5%. The lattice parameter ratios, and the angles α, β and γ between the basis vectors, are not affected at all.
    Beschreibung: Automatically determined band widths in simulated backscatter Kikuchi patterns exhibit differences from the double Bragg angles that correlate with the scatterer density. Corrections are proposed to compensate for this.
    Schlagwort(e): ddc:548 ; mean atomic number ; Kikuchi patterns ; lattice parameters ; automated Bragg angle determination ; lattice parameter determination ; dynamical theory of electron diffraction ; electron backscatter diffraction ; Funk transform
    Sprache: Englisch
    Materialart: doc-type:article
    Standort Signatur Erwartet Verfügbarkeit
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  • 3
    Publikationsdatum: 2023-07-20
    Beschreibung: A pseudosymmetric description of the crystal lattice derived from a single wide‐angle Kikuchi pattern can have several causes. The small size (〈15%) of the sector covered by an electron backscatter diffraction pattern, the limited precision of the projection centre position and the Kikuchi band definition are crucial. Inherent pseudosymmetries of the crystal lattice and/or structure also pose a challenge in the analysis of Kikuchi patterns. To eliminate experimental errors as much as possible, simulated Kikuchi patterns of 350 phases have been analysed using the software CALM [Nolze et al. (2021). J. Appl. Cryst.54, 1012–1022] in order to estimate the frequency of and reasons for pseudosymmetric crystal lattice descriptions. Misinterpretations occur in particular when the atomic scattering factors of non‐equivalent positions are too similar and reciprocal‐lattice points are systematically missing. As an example, a pseudosymmetry prediction depending on the elements involved is discussed for binary AB compounds with B1 and B2 structure types. However, since this is impossible for more complicated phases, this approach cannot be directly applied to compounds of arbitrary composition and structure.
    Beschreibung: Distinguishing between actual and apparent pseudosymmetry in electron backscatter diffraction patterns is nearly impossible, even for simulated patterns. However, the resulting lattice is always a superlattice as long as the signal is not a superposition of multiple patterns.
    Schlagwort(e): ddc:548 ; Bravais lattices ; pseudosymmetry ; lattice point density ; ordered/disordered structures ; lattice distortion ; electron backscatter diffraction ; backscattered Kikuchi diffraction patterns ; lattice parameters ; Funk transform
    Sprache: Englisch
    Materialart: doc-type:article
    Standort Signatur Erwartet Verfügbarkeit
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  • 4
    Publikationsdatum: 2023-07-19
    Beschreibung: The derivation of a crystal structure and its phase‐specific parameters from a single wide‐angle backscattered Kikuchi diffraction pattern requires reliable extraction of the Bragg angles. By means of the first derivative of the lattice profile, an attempt is made to determine fully automatically and reproducibly the band widths in simulated Kikuchi patterns. Even under such ideal conditions (projection centre, wavelength and lattice plane traces are perfectly known), this leads to a lattice parameter distribution whose mean shows a linear offset that correlates with the mean atomic number Z of the pattern‐forming phase. The consideration of as many Kikuchi bands as possible reduces the errors that typically occur if only a single band is analysed. On the other hand, the width of the resulting distribution is such that higher image resolution of diffraction patterns, employing longer wavelengths to produce wider bands or the use of higher interference orders is less advantageous than commonly assumed.
    Beschreibung: The lattice parameters of more than 350 phases have been determined from simulated backscatter Kikuchi patterns. The deviations correlating with the mean atomic number correspond to those observed previously for experimental electron backscatter diffraction patterns.
    Schlagwort(e): ddc:548 ; Bragg angles ; Kikuchi bands ; Kikuchi patterns ; first derivative ; lattice parameters ; lattice parameter determination ; Bravais lattice type ; electron backscatter diffraction ; Radon transform
    Sprache: Englisch
    Materialart: doc-type:article
    Standort Signatur Erwartet Verfügbarkeit
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  • 5
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    Unbekannt
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Publikationsdatum: 2023-07-19
    Beschreibung: Since high‐pressure devices have been used at synchrotron facilities, accurate determination of pressure and temperature in the sample has been a crucial objective, particularly for experiments that simulate the Earth's interior. However, in some cases using a thermocouple may have a high likelihood of failure or is incompatible with a high‐pressure assembly. To address these challenges and similar issues, we aim to expand a previously proposed solution: to jointly estimate pressure and temperature (〈italic〉PT〈/italic〉) through 〈italic〉in situ〈/italic〉 X‐ray diffraction, to cover a wider range of internal 〈italic〉PT〈/italic〉 calibrants tested over larger 〈italic〉PT〈/italic〉 ranges. A modifiable Python‐based software is offered to quickly obtain results. To achieve these aims, 〈italic〉in situ〈/italic〉 large volume press experiments are performed on pellets of intimately mixed powders of a halide (NaCl, KCl, KBr, CsCl) or MgO and a metal (Pt, Re, Mo, W, Ni) in the pressure range 3–11 GPa and temperature range 300–1800 K. Although the pressure range was chosen for practical reasons, it also covers an equally important depth range in the Earth (down to 350 km) for geoscience studies. A thermocouple was used to validate the 〈italic〉PT〈/italic〉 conditions in the cell assemblies. The key results show that choosing the appropriate calibrant materials and using a joint 〈italic〉PT〈/italic〉 estimation can yield surprisingly small uncertainties (〈italic〉i.e.〈/italic〉 〈±0.1 GPa and 〈±50 K). This development is expected to benefit current and future research at extreme conditions, as other materials with high compressibility or high thermal pressure, stable over large 〈italic〉PT〈/italic〉 ranges, may be discovered and used as 〈italic〉PT〈/italic〉 calibrants.〈/p〉
    Beschreibung: Research in high‐pressure devices, such as the diamond anvil cell and the large volume press, requires knowledge of the pressure and temperature in the sample. Here, a large volume press and an internal resistive heater were used to generate high load and heat to various combinations of intimately mixed powders of materials. X‐ray diffraction and custom software were used to jointly estimate the pressures and temperatures in the samples and establish calibrants for 〈italic〉in situ〈/italic〉 experiments at extreme conditions.〈boxed-text position="anchor" content-type="graphic" xml:lang="en"〉〈graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:16005775:jsy2vl5008:jsy2vl5008-fig-0001"〉
    Beschreibung: https://gitlab.desy.de/robert.farla/eoscross
    Schlagwort(e): ddc:548 ; equations of state ; X‐ray diffraction ; large volume press ; high pressure ; resistive heating
    Sprache: Englisch
    Materialart: doc-type:article
    Standort Signatur Erwartet Verfügbarkeit
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