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

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.

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xINTERPDF: a graphical user interface for analyzing intermolecular pair distribution functions of organic compounds from X-ray total scattering data

Journal of Applied Crystallography ◽

10.1107/s1600576718012359 ◽

2018 ◽

Vol 51 (5) ◽

pp. 1498-1499

Author(s):

Chenyang Shi

Keyword(s):

User Interface ◽

Organic Compounds ◽

Graphical User Interface ◽

Distribution Functions ◽

Scattering Data ◽

Total Scattering ◽

X Ray ◽

Software Program ◽

Pair Distribution Functions

A new software program, xINTERPDF, that analyzes the intermolecular correlations in organic compounds via measured X-ray total scattering data is described.

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

Powder Diffraction ◽

10.1017/s0885715614001304 ◽

2014 ◽

Vol 30 (S1) ◽

pp. S2-S8 ◽

Cited By ~ 9

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.

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D-83 Element-Specific Structure of Nanosized Materials by High-Energy Resonant X-ray Diffraction and Differential Atomic Pair Distribution Functions

Powder Diffraction ◽

10.1154/1.3454959 ◽

2010 ◽

Vol 25 (2) ◽

pp. 212-212

Author(s):

V. Petkov ◽

S. Shastri

Keyword(s):

High Energy ◽

Distribution Functions ◽

Specific Structure ◽

X Ray Diffraction ◽

X Ray ◽

Nanosized Materials ◽

Atomic Pair ◽

Pair Distribution Functions ◽

D 83

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Extracting differential pair distribution functions usingMIXSCAT

Journal of Applied Crystallography ◽

10.1107/s0021889810009155 ◽

2010 ◽

Vol 43 (3) ◽

pp. 635-638 ◽

Cited By ~ 7

Author(s):

Caroline Wurden ◽

Katharine Page ◽

Anna Llobet ◽

Claire E. White ◽

Thomas Proffen

Keyword(s):

Distribution Functions ◽

Program Package ◽

Scattering Data ◽

X Ray ◽

Differential Structure ◽

Structure Factors ◽

Differential Pair ◽

User Friendly ◽

Pair Distribution Functions

Differently weighted experimental scattering data have been used to extract partial or differential structure factors or pair distribution functions in studying many materials. However, this is not done routinely partly because of the lack of user-friendly software. This paper presentsMIXSCAT, a new member of theDISCUSprogram package.MIXSCATallows one to combine neutron and X-ray pair distribution functions and extract their respective differential functions.

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Element-specific structure of materials with intrinsic disorder by high-energy resonant x-ray diffraction and differential atomic pair-distribution functions: A study of PtPd nanosized catalysts

Physical Review B ◽

10.1103/physrevb.81.165428 ◽

2010 ◽

Vol 81 (16) ◽

Cited By ~ 33

Author(s):

V. Petkov ◽

S. D. Shastri

Keyword(s):

Intrinsic Disorder ◽

High Energy ◽

Distribution Functions ◽

Specific Structure ◽

X Ray Diffraction ◽

X Ray ◽

Atomic Pair ◽

Nanosized Catalysts ◽

Pair Distribution Functions

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MCGRtof: Monte CarloG(r) with resolution corrections for time-of-flight neutron diffractometers

Journal of Applied Crystallography ◽

10.1107/s0021889801015345 ◽

2001 ◽

Vol 34 (6) ◽

pp. 780-782 ◽

Cited By ~ 14

Author(s):

Matthew G. Tucker ◽

Martin T. Dove ◽

David A. Keen

Keyword(s):

Pair Distribution Function ◽

Time Of Flight ◽

Distribution Functions ◽

Monte Carlo Algorithm ◽

Scattering Data ◽

Spallation Neutron Source ◽

Total Scattering ◽

Inverse Monte Carlo ◽

Pair Distribution Functions ◽

Neutron Total Scattering

A new implementation of the programMCGR[Pusztai & McGreevy (1997).Physica B,234–236, 357–358] for the calculation of pair distribution functions from neutron total scattering data using an inverse Monte Carlo algorithm is presented. The new implementation, calledMCGRtof, incorporates the resolution functions for time-of-flight neutron diffractometers, and is suitable for analysis of data from instruments such as GEM at the ISIS spallation neutron source. The effect of including resolution correctly is to increase the magnitude of the pair distribution function at larger distances. The working program is illustrated with total scattering measurements from crystalline AlPO4.

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

Nanomaterials ◽

10.3390/nano10050824 ◽

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.

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High-resolution atomic distribution functions of disordered materials by high-energy X-ray diffraction

Journal of Non-Crystalline Solids ◽

10.1016/s0022-3093(01)00864-x ◽

2001 ◽

Vol 293-295 ◽

pp. 726-730 ◽

Cited By ~ 22

Author(s):

V. Petkov ◽

S.J.L. Billinge ◽

S.D. Shastri ◽

B. Himmel

Keyword(s):

High Resolution ◽

High Energy ◽

Distribution Functions ◽

Disordered Materials ◽

X Ray Diffraction ◽

X Ray ◽

Atomic Distribution

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Building and refining complete nanoparticle structures with total scattering data

Journal of Applied Crystallography ◽

10.1107/s0021889811001968 ◽

2011 ◽

Vol 44 (2) ◽

pp. 327-336 ◽

Cited By ~ 55

Author(s):

Katharine Page ◽

Taylor C. Hood ◽

Thomas Proffen ◽

Reinhard B. Neder

Keyword(s):

Distribution Function ◽

Pair Distribution Function ◽

Function Analysis ◽

Structure Refinement ◽

High Energy ◽

Scattering Data ◽

Surface Relaxation ◽

Data Set ◽

Total Scattering ◽

Differential Evolutionary Algorithm

High-energy X-ray and spallation neutron total scattering data provide information about each pair of atoms in a nanoparticle sample, allowing for quantitative whole-particle structural modeling based on pair distribution function analysis. The realization of this capability has been hindered by a lack of versatile tools for describing complex finite structures. Here, the implementation of whole-particle refinement for complete nanoparticle systems is described within two programs,DISCUSandDIFFEV, and the diverse capabilities they present are demonstrated. The build-up of internal atomic structure (including defects, chemical ordering and other types of disorder), and nanoparticle size, shape and architecture (including core–shell structures, surface relaxation and ligand capping), are demonstrated using the programDISCUS. The structure refinement of a complete nanoparticle system (4 nm Au particles with organic capping ligands at the surface), based on neutron pair distribution function data, is demonstrated usingDIFFEV, a program using a differential evolutionary algorithm to generate parameter values. These methods are a valuable addition to other probes appropriate for nanomaterials, adaptable to a diverse and complex set of materials systems, and extendable to additional data-set types.

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