scholarly journals Structural Study of Nano-Sized Gahnite (ZnAl2O4): From the Average to the Local Scale

Nanomaterials ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 824
Author(s):  
Giorgia Confalonieri ◽  
Nicola Rotiroti ◽  
Andrea Bernasconi ◽  
Monica Dapiaggi
Keyword(s):  
Grain Size ◽  
High Resolution ◽  
Structural Model ◽  
Rietveld Method ◽  
Synthesis Method ◽  
European Synchrotron Radiation Facility ◽  
Local Region ◽  
Scattering Data ◽  
Total Scattering ◽  
Average Structure

Spinel gahnite (ZnAl2O4) has been obtained through a hydrothermal synthesis method with a grain size of about 2 nm. The sample was calcined for a few hours at two different temperatures (800 and 900 °C) in order to obtain larger grain sizes to be analyzed by means of powder diffraction with the Rietveld method, and by means of total scattering with the Pair Distribution Function (PDF) method. The idea is to compare the average to the local structure, as a function of increasing grain size. The total scattering data were collected at the European Synchrotron Radiation Facility (ESRF), Grenoble. The samples have been also characterised by means of high resolution Transmission Electron Microscopy (TEM), showing an increasing grain size up to about 9 nm. The average structure presented variations in the inversion degree and an increase in grain size. TEM observations demonstrated that the small crystals are well crystallised: the high resolution images neatly showed the atomic planes, even in the smallest particles. However, the average structure did not properly fit the PDF data in the local region, owing to a slightly different coordination among the octahedra. A new structural model is proposed for the local region of the PDF, that helped our understanding of the differences between a real nanostructured sample and that of a microcrystalline one. The oxygen disorder, due to the inversion grade of the spinel, is demonstrates to be at the basis of the local deviation. No signals of interstitial Zn atoms were detected.

Comparison of total scattering data from various sources: the case of a nanometric spinel

2015 ◽  
Vol 30 (S1) ◽  
pp. S65-S69 ◽  
Author(s):  
Giorgia Confalonieri ◽  
Monica Dapiaggi ◽  
Marco Sommariva ◽  
Milen Gateshki ◽  
Andy N. Fitch ◽  
...  
Keyword(s):  
High Resolution ◽  
High Energy ◽  
European Synchrotron Radiation Facility ◽  
Distribution Functions ◽  
Scattering Data ◽  
Data Set ◽  
Total Scattering ◽  
X Ray ◽  
Fair Comparison ◽  
Pair Distribution Functions

Total scattering data of nanocrystalline gahnite (ZnAl2O4, 2–3 nm) have been collected with three of the most commonly used instruments: (i) ID31 high-resolution diffractometer at the European Synchrotron Radiation Facility (ESRF) (Qmax = 22 Å−1); (ii) ID11 high-energy beamline at the ESRF (Qmax = 26.6 Å−1); and (iii) Empyrean laboratory diffractometer by PANalytical with molybdenum anode X-ray tube (Qmax = 17.1 Å−1). Pair distribution functions (PDFs) for each instrument data-set have been obtained, changing some of the parameters, by PDFgetX3 software, with the aim of testing the software in the treatment of different total scattering data. The material under analysis has been chosen for its nanometric (and possibly disordered) nature, to give rise to a challenge for all the diffractometers involved. None of the latter should have a clear advantage. The PDF and F(Q) functions have been visually compared, and then the three PDF sets have been used for refinements by means of PDFgui suite. All the refinements have been made exactly in the same way for the sake of a fair comparison. Small differences could be observed in the experimental PDFs and the derived results, but none of them seemed to be significant.

scholarly journals Synchrotron total-scattering data applicable to dual-space structural analysis

IUCrJ ◽  
2021 ◽  
Vol 8 (3) ◽  
Author(s):  
Jonas Beyer ◽  
Kenichi Kato ◽  
Bo Brummerstedt Iversen
Keyword(s):  
Structural Analysis ◽  
Dual Space ◽  
Structural Model ◽  
Dynamic Range ◽  
Structural Parameters ◽  
Reciprocal Space ◽  
Scattering Data ◽  
Total Scattering ◽  
X Ray ◽  
Space Data

Synchrotron powder X-ray diffraction (PXRD) is a well established technique for investigating the atomic arrangement of crystalline materials. At modern beamlines, X-ray scattering data can be collected in a total-scattering setting, which additionally opens up the opportunity for direct-space structural analysis through the atomic pair distribution function (PDF). Modelling of PXRD and PDF data is typically carried out separately, but employing a concurrent structural model to both direct- and reciprocal-space data has the possibility to enhance total-scattering data analysis. However, total-scattering measurements applicable to such dual-space analyses are technically demanding. Recently, the technical demands have been fulfilled by a MYTHEN microstrip detector system (OHGI), which meets the stringent requirements for both techniques with respect to Q range, Q resolution and dynamic range. In the present study, we evaluate the quality of total-scattering data obtained with OHGI by separate direct- and reciprocal-space analysis of Si. Excellent agreement between structural parameters in both spaces is found, demonstrating that the total-scattering data from OHGI can be utilized in dual-space structural analysis e.g. for in situ and operando measurements.

scholarly journals Structure determination of riboflavin by synchrotron high-resolution powder X-ray diffraction

2021 ◽  
Vol 77 (12) ◽  
Author(s):  
Mathieu Guerain ◽  
Frédéric Affouard ◽  
Charline Henaff ◽  
Catherine Dejoie ◽  
Florence Danède ◽  
...  
Keyword(s):  
High Resolution ◽  
Structural Model ◽  
European Synchrotron Radiation Facility ◽  
Stable Form ◽  
X Ray Diffraction ◽  
Pxrd Pattern ◽  
X Ray ◽  
Monte Carlo Simulated Annealing ◽  
Hydroxy Groups

The crystal structure of the stable form of vitamin B2 or riboflavin (C17H20N4O6) was solved using high-resolution powder X-ray diffraction (PXRD). The high-resolution PXRD pattern of riboflavin was recorded at room temperature at the European Synchrotron Radiation Facility (Grenoble, France). The starting structural model was generated using a Monte Carlo simulated annealing method. The final structure was obtained through Rietveld refinement. The positions of the H atoms belonging to hydroxy groups were estimated from computational energy minimizations. The symmetry is orthorhombic with the space group P212121 and the following lattice parameters: a = 20.01308, b = 15.07337 and c = 5.31565 Å.

A Structural Model for a Quasi-Crystalline Material Derived from TEM

1990 ◽  
Vol 48 (1) ◽  
pp. 48-49
Author(s):  
Jan-Olov Bovin ◽  
Osamu Terasaki ◽  
Jan-Olle Malm ◽  
Sven Lidin ◽  
Sten Andersson
Keyword(s):  
High Resolution ◽  
Electron Diffraction ◽  
Structural Model ◽  
Image Intensifier ◽  
Crystalline Materials ◽  
Icosahedral Phases ◽  
Transmission Electron ◽  
Electron Microscopes ◽  
Diffraction Patterns ◽  
Quasi Crystals

High resolution transmission electron microscopy (HRTEM) is playing an important role in identifying the new icosahedral phases. The selected area diffraction patterns of quasi crystals, recorded with an aperture of the radius of many thousands of Ångströms, consist of dense arrays of well defined sharp spots with five fold dilatation symmetry which makes the interpretation of the diffraction process and the resulting images different from those invoked for usual crystals. The atomic structure of the quasi crystals is not established even if several models are proposed. The correct structure model must of course explain the electron diffraction patterns with 5-, 3- and 2-fold symmetry for the phases but it is also important that the HRTEM images of the alloys match the computer simulated images from the model. We have studied quasi crystals of the alloy Al65Cu20Fe15. The electron microscopes used to obtain high resolution electro micrographs and electron diffraction patterns (EDP) were a (S)TEM JEM-2000FX equipped with EDS and PEELS showing a structural resolution of 2.7 Å and a IVEM JEM-4000EX with a UHP40 high resolution pole piece operated at 400 kV and with a structural resolution of 1.6 Å. This microscope is used with a Gatan 622 TV system with an image intensifier, coupled to a YAG screen. It was found that the crystals of the quasi crystalline materials here investigated were more sensitive to beam damage using 400 kV as electron accelerating voltage than when using 200 kV. Low dose techniques were therefore applied to avoid damage of the structure.

Pushing the Envelope

2018 ◽  
Author(s):  
Eaton E. Lattman ◽  
Thomas D. Grant ◽  
Edward H. Snell
Keyword(s):  
High Resolution ◽  
Electron Density ◽  
Structural Information ◽  
Hydration Shell ◽  
Three Dimensional ◽  
Scattering Data ◽  
Saxs Data ◽  
Electron Density Function ◽  
Angle Scattering ◽  
Iterative Structure

Direct electron density determination from SAXS data opens up new opportunities. The ability to model density at high resolution and the implicit direct estimation of solvent terms such as the hydration shell may enable high-resolution wide angle scattering data to be used to calculate density when combined with additional structural information. Other diffraction methods that do not measure three-dimensional intensities, such as fiber diffraction, may also be able to take advantage of iterative structure factor retrieval. While the ability to reconstruct electron density ab initio is a major breakthrough in the field of solution scattering, the potential of the technique has yet to be fully uncovered. Additional structural information from techniques such as crystallography, NMR, and electron microscopy and density modification procedures can now be integrated to perform advanced modeling of the electron density function at high resolution, pushing the boundaries of solution scattering further than ever before.

scholarly journals Paleoenvironments from robust loess stratigraphy using high-resolution color and grain-size data of the last glacial Krems-Wachtberg record (NE Austria)

2020 ◽  
Vol 248 ◽  
pp. 106602
Author(s):  
Tobias Sprafke ◽  
Philipp Schulte ◽  
Simon Meyer-Heintze ◽  
Marc Händel ◽  
Thomas Einwögerer ◽  
...  
Keyword(s):  
Grain Size ◽  
High Resolution ◽  
Last Glacial ◽  
Size Data ◽  
The Last Glacial

Calculation of the energy-averaged scattering function from high resolution low-energy neutron scattering data

1983 ◽  
Vol 27 (5) ◽  
pp. 1913-1926 ◽  
Author(s):  
C. H. Johnson ◽  
N. M. Larson ◽  
C. Mahaux ◽  
R. R. Winters
Keyword(s):  
High Resolution ◽  
Neutron Scattering ◽  
Low Energy ◽  
Scattering Data ◽  
Scattering Function ◽  
Energy Neutron

Total scattering experiments on glass and crystalline materials at the ESRF on the ID11 Beamline

2014 ◽  
Vol 30 (S1) ◽  
pp. S2-S8 ◽  
Author(s):  
Andrea Bernasconi ◽  
Jonathan Wright ◽  
Nicholas Harker
Keyword(s):  
High Energy ◽  
Real Space ◽  
European Synchrotron Radiation Facility ◽  
Small Sample ◽  
Distribution Functions ◽  
Total Scattering ◽  
Crystalline Materials ◽  
Space Resolution ◽  
Atomic Pair ◽  
Counting Statistics

ID11 is a multi-purpose high-energy beamline at the European Synchrotron Radiation Facility (ESRF). Owing to the high-energy X-ray source (up to 140 keV) and flexible, high-precision sample mounting which allows small sample–detector distances to be achieved, experiments such as total scattering in transmission geometry are possible. This permits the exploration of a wide Q range and so provides high real-space resolution. A range of samples (glasses and crystalline powders) have been measured at 78 keV, first putting the detector as close as possible to the sample (~10 cm), and then moving it vertically and laterally with respect to the beam in order to have circular and quarter circle sections of diffraction rings, with consequent QMAX at the edge of the detector of about 16 and 28 Å−1, respectively. Data were integrated using FIT2D, and then normalized and corrected with PDFgetX3. Results have been compared to see the effects of Q-range and counting statistics on the atomic pair distribution functions of the different samples. A Q of at least 20 Å−1 was essential to have sufficient real-space resolution for both type of samples while statistics appeared more important for glass samples rather than for crystalline samples.

Sign in / Sign up

Export Citation Format

Share Document