Powder diffraction at ALBA synchrotron

This talk is devoted to explain the uses of powder diffraction at MSPD (material science and powder diffraction) of ALBA synchrotron light source. General characteristics of the beamline are: Station 1 - High Pressure Diffraction on powders with diamond anvil cell (DAC) and CCD detector. Microdiffraction; and Station 2 - High Resolution Powder Diffraction with Multicrystal- and Silicon-Strip detector. Energy Range: 8-50keV; Typical beam size: 4x1mm; all typical sample geometries possible: capillary, reflection and flat sample in transmission. Initially the setups are described in detail both in the optics hutch and in the experimental hutch. In the high-pressure end station, we can highlight: i) sample alignment semi-automatic; ii) data acquisition and reduction integrated within the beamline control system; iii) online pressure calibration system operational and several upgrades which are under commissioning: i) system for Membrane DAC, Automatic Drive System (change the pressure from outside the hutch); ii) Gas Membrane kit for Almax-Boehler DAC cell (from screw-driven to gas membrane driven); iii) low temperature cryostat and high temperature DAC cell projects are on-going. In the high resolution powder diffraction end station, we can highlight: i) a diffractometer with 3 concentric rotary stages (for two detectors); ii) one very high resolution detector MAD26 (10 – 50KeV), devoted to high resolution ~0.005° [13 channels with 1.5 deg pitch, Si111 Bragg crystals, YAP scintillator + PMT]; iii) MythenII (8 – 30 keV) for fast acquisitions [6 modules that cover 40 deg 0.005 pitch angle, with millisecond resolution]; iv) Temperature range 80 – 900K; v) Eulerian Cradle optional. Then, the main applications will be dealt with based on examples that expands from structure solution of zeolites to the in-situ studies of perovskite catalyst under H2 atmosphere at high temperatures. The high-pressure studies will be exemplified by studies of materials in DAC.Universidad de Málaga. Campus de Excelencia Internacional Andalucía Tech

Powder diffraction at ALBA synchrotron

This talk is devoted to explain the uses of powder diffraction at MSPD (material science and powder diffraction) of ALBA synchrotron light source. General characteristics of the beamline are: Station 1 - High Pressure Diffraction on powders with diamond anvil cell (DAC) and CCD detector. Microdiffraction; and Station 2 - High Resolution Powder Diffraction with Multicrystal- and Silicon-Strip detector. Energy Range: 8-50keV; Typical beam size: 4x1mm; all typical sample geometries possible: capillary, reflection and flat sample in transmission. Initially the setups are described in detail both in the optics hutch and in the experimental hutch. In the high-pressure end station, we can highlight: i) sample alignment semi-automatic; ii) data acquisition and reduction integrated within the beamline control system; iii) online pressure calibration system operational and several upgrades which are under commissioning: i) system for Membrane DAC, Automatic Drive System (change the pressure from outside the hutch); ii) Gas Membrane kit for Almax-Boehler DAC cell (from screw-driven to gas membrane driven); iii) low temperature cryostat and high temperature DAC cell projects are on-going. In the high resolution powder diffraction end station, we can highlight: i) a diffractometer with 3 concentric rotary stages (for two detectors); ii) one very high resolution detector MAD26 (10 – 50KeV), devoted to high resolution ~0.005° [13 channels with 1.5 deg pitch, Si111 Bragg crystals, YAP scintillator + PMT]; iii) MythenII (8 – 30 keV) for fast acquisitions [6 modules that cover 40 deg 0.005 pitch angle, with millisecond resolution]; iv) Temperature range 80 – 900K; v) Eulerian Cradle optional. Then, the main applications will be dealt with based on examples that expands from structure solution of zeolites to the in-situ studies of perovskite catalyst under H2 atmosphere at high temperatures. Total scattering (pair distribution function analysis) will also be presented. The high-pressure studies will be exemplified by studies of materials in DAC.Universidad de Málaga. Campus de Excelencia Internacional Andalucía Tech

Rietveld Quantitative Phase Analysis of Oil Well Cement: in Situ Hydration Study at 150 Bars and 150 °C

Oil and gas well cements are multimineral materials that hydrate under high pressure and temperature. Their overall reactivity at early ages is studied by a number of techniques including through the use of the consistometer. However, for a proper understanding of the performance of these cements in the field, the reactivity of every component, in real‐world conditions, must be analysed. To date, in situ high energy synchrotron powder diffraction studies of hydrating oil well cement pastes have been carried out, but the quality of the data was not appropriated for Rietveld quantitative phase analyses. Therefore, the phase reactivities were followed by the inspection of the evolution of non‐overlapped diffraction peaks. Very recently, we have developed a new cell specially designed to rotate under high pressure and temperature. Here, this spinning capillary cell is used for in situ studies of the hydration of a commercial oil well cement paste at 150 bars and 150 °C. The powder diffraction data were analysed by the Rietveld method to quantitatively determine the reactivities of each component phase. The reaction degree of alite was 90% after 7 hours, and that of belite was 42% at 14 hours. These analyses are accurate, as the in situ measured crystalline portlandite content at the end of the experiment, 12.9 wt%, compares relatively well with the value determined ex situ by thermal analysis, i.e., 14.0 wt%. The crystalline calcium silicates forming at 150 bars and 150 °C are also discussed.This research was funded by Spanish MINECO, grant number BIA2017‐82391‐R which is co‐funded by FEDER. We thank Marc Malfois for his help during the experiment performed at NCD‐SWEET beamline at ALBA synchrotron. We also thank Marcus Paul (Dyckerhoff GmbH) for providing the OWC sample with its characterization and helpful discussions

Development of powder diffraction apparatus for small-angle X-ray scattering measurements

A novel type of X-ray collimation system attached to commercial powder diffractometers makes the structural characterization of nanomaterials possible in a wide size range from <0.1 to 100 nm by combination of the small- and wide-angle X-ray scattering techniques. There is no dead interval in the detection between the small- and wide-angle regimes. This device can be attached to any existing 'θ/θ' powder diffractometer, providing a multi-functional small- and wide-angle X-ray scattering/diffraction (SWAXS) apparatus. After proper alignment and adjustment, the device can be removed and re-attached at any time to switch between normal and SWAXS functions. Copyright © International Union of Crystallography 2013

Evolution of Complexity in Out-of-Equilibrium Systems by Time-Resolved or Space-Resolved Synchrotron Radiation Techniques

Out-of-equilibrium phenomena are attracting high interest in physics, materials science, chemistry and life sciences. In this state, the study of structural fluctuations at different length scales in time and space are necessary to achieve significant advances in the understanding of structure-functionality relationship. The visualization of patterns arising from spatiotemporal fluctuations is nowadays possible thanks to new advances in X-ray instrumentation development that combine high resolution both in space and in time. We present novel experimental approaches using high brilliance synchrotron radiation sources, fast detectors and focusing optics, joint with advanced data analysis based on automated statistical, mathematical and imaging processing tools. This approach has been used to investigate structural fluctuations in out-of-equilibrium systems in the novel field of inhomogeneous quantum complex matter at the crossing point of technology, physics and biology. In particular, we discuss how nanoscale complexity controls the emergence of high temperature superconductivity (HTS), myelin functionality and formation of hybrid organic-inorganic nanostructures. The emergent complex geometries, opening novel venues to quantum technology and to development of quantum physics of living systems, are discussedComment: 18 pages, 7 figure

Various arsenic network structures in 112-type Ca1-xLaxFe1-yPdyAs2 revealed by synchrotron x-ray diffraction experiments

Two novel 112-type palladium doped iron arsenides were synthesized and identified using comprehensive studies involving synchrotron x-ray diffraction and x-ray absorption near edge structure (XANES) experiments. Whereas in-plane arsenic zigzag chains were found in 112-type superconducting iron arsenide, Ca1-xLaxFeAs2 with maximum Tc = 34 K, deformed arsenic network structures appeared in 112-type materials such as longitudinal arsenics zigzag chains in CaFe1-yPdyAs2 (y ~ 0.51) and arsenic square sheets constructed via hypervalent bonding in Ca1-xLaxFe1-yPdyAs2 (x ~ 0.31, y ~ 0.30). As K-edge XANES spectra clarified the similar oxidization states around FeAs4 tetrahedrons, expecting us the possible parents for high Tc 112-type iron arsenide superconductors.Comment: 9 pages, 5 figure