High-throughput Powder Diffraction Research Articles

Remote and automated high-throughput powder diffraction measurements enabled by a robotic sample changer at SSRL beamline 2-1.

The general-purpose powder diffractometer beamline (BL2-1) at the Stanford Synchrotron Radiation Lightsource (SSRL) is described. The evolution of design and performance of BL2-1 are presented, in addition to current operating specifications, applications and measurement capabilities. Recent developments involve a robotic sample changer enabling high-throughput X-ray diffraction measurements, applicable to mail-in and remote operations. In situ and operando capabilities to measure samples with different form factors (e.g. capillary, flat plate or thin film, and transmission) and under variable experimental conditions are discussed. Several example datasets and accompanying Rietveld refinements are presented.

High-Throughput Powder Diffraction Using White X-Ray Beam and a Simulated Energy-Dispersive Array Detector

High-throughput powder X-ray diffraction (XRD) with white X-ray beam and an energy-dispersive detector array is demonstrated in this work on a CeO2 powder sample on a bending magnet synchrotron beamline at the Shanghai Synchrotron Radiation Facility (SSRF), using a simulated energy-dispersive array detector consisting of a spatially scanning silicon-drift detector (SDD). Careful analysis and corrections are applied to account for various experimental hardware-related and diffraction angle-related factors. The resulting diffraction patterns show that the relative strength between different diffraction peaks from energy-dispersive XRD (EDXRD) spectra is consistent with that from angle-resolved XRD (ARXRD), which is necessary for analyzing crystal structures for unknown samples. The X-ray fluorescence (XRF) signal is collected simultaneously. XRF counts from all pixels are integrated directly by energy, while the diffraction spectra are integrated by d-spacing, resulting in a much improved peak strength and signal-to-noise (S/N) ratio for the array detector. In comparison with ARXRD, the diffraction signal generated by a white X-ray beam over monochromic light under the experimental conditions is about 104 times higher. The full width at half maximum (FWHM) of the peaks in q-space is found to be dependent on the energy resolution of the detector, the angle span of the detector, and the diffraction angle. It is possible for EDXRD to achieve the same or even smaller FWHM as ARXRD under the energy resolution of the current detector if the experimental parameters are properly chosen.

High-throughput powder diffraction measurement system consisting of multiple MYTHEN detectors at beamline BL02B2 of SPring-8.

In this study, we developed a user-friendly automatic powder diffraction measurement system for Debye-Scherrer geometry using a capillary sample at beamline BL02B2 of SPring-8. The measurement system consists of six one-dimensional solid-state (MYTHEN) detectors, a compact auto-sampler, wide-range temperature control systems, and a gas handling system. This system enables to do the automatic measurement of temperature dependence of the diffraction patterns for multiple samples. We introduced two measurement modes in the MYTHEN system and developed new attachments for the sample environment such as a gas handling system. The measurement modes and the attachments can offer in situ and/or time-resolved measurements in an extended temperature range between 25 K and 1473 K and various gas atmospheres and pressures. The results of the commissioning and performance measurements using reference materials (NIST CeO2 674b and Si 640c), V2O3 and Ti2O3, and a nanoporous coordination polymer are presented.

Robust Nanostructure from High Throughput Powder Diffraction Data

Journal Article Robust Nanostructure from High Throughput Powder Diffraction Data Get access Simon J L Billinge, Simon J L Billinge Department of Applied Physics and Applied Mathematics, Columbia University, New York, NY, USACondensed Matter Physics and Materials Science Department, Brookhaven National Laboratory, Upton, NY, USA Search for other works by this author on: Oxford Academic Google Scholar Christopher J Wright, Christopher J Wright Department of Applied Physics and Applied Mathematics, Columbia University, New York, NY, USA Search for other works by this author on: Oxford Academic Google Scholar Chia-Hao Liu, Chia-Hao Liu Department of Applied Physics and Applied Mathematics, Columbia University, New York, NY, USA Search for other works by this author on: Oxford Academic Google Scholar Michael Waddell, Michael Waddell Department of Applied Physics and Applied Mathematics, Columbia University, New York, NY, USA Search for other works by this author on: Oxford Academic Google Scholar Pavol Juhas, Pavol Juhas Computational Science Initiative, Brookhaven National Laboratory, Upton, NY, USA Search for other works by this author on: Oxford Academic Google Scholar Eric Dooryhee, Eric Dooryhee National Synchrotron Light Source-II, Brookhaven National Laboratory, Upton, NY, USA Search for other works by this author on: Oxford Academic Google Scholar Sanjit Ghose, Sanjit Ghose National Synchrotron Light Source-II, Brookhaven National Laboratory, Upton, NY, USA Search for other works by this author on: Oxford Academic Google Scholar Milinda Abeykoon, Milinda Abeykoon National Synchrotron Light Source-II, Brookhaven National Laboratory, Upton, NY, USA Search for other works by this author on: Oxford Academic Google Scholar Arman Arkilic, Arman Arkilic National Synchrotron Light Source-II, Brookhaven National Laboratory, Upton, NY, USA Search for other works by this author on: Oxford Academic Google Scholar Daniel Allan, Daniel Allan National Synchrotron Light Source-II, Brookhaven National Laboratory, Upton, NY, USA Search for other works by this author on: Oxford Academic Google Scholar ... Show more Thomas Caswell Thomas Caswell National Synchrotron Light Source-II, Brookhaven National Laboratory, Upton, NY, USA Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 23, Issue S1, 1 July 2017, Pages 172–173, https://doi.org/10.1017/S1431927617001544 Published: 04 August 2017

High-throughput powder diffraction on beamline I11 at Diamond

A new capability designed for high-throughput (HT) structural analysis using the synchrotron powder diffraction beamline (I11) at Diamond Light Source is reported. With a high-brightness X-ray beam, multi-analyser detectors and fast data-acquisition procedures, high-quality diffraction data can be collected at a speed of ∼15–30 min per powder pattern for good crystalline materials. Fast sample changing at a rate of a few seconds per specimen is achieved with a robotic arm and pre-loaded capillary specimens on a multi-tray carousel (200-sample capacity). Additional equipment, such as an automatic powder-loading machine and a pre-alignment jig for the sample capillaries, is available to reduce preparation time. For demonstration purposes, the first results presented here are those from standard reference powders of Si, TiO2and TiO2/Si mixtures, obtained by analysing the data using Le Bail (instrumental calibration) and Rietveld refinements (quantitative agreement within 1%). The HT hardware was then used to study the structural phase evolution of a library of 31 La4Ni3−xFexO10heterometallic ceramic powders in less than 1 d. The powders were generated from a single heat treatment (at 1348 K in air for 12 h) of nanoceramic oxide co-precipitate precursors, made using a newly developed HT synthesis robot. Crystallographic details (symmetry and lattice parameters) were obtained as a function of Fe concentration. The results revealed that this approach was able to produce a pure Ruddlesden–Popper-type phase with an iron content of up tox= 0.5, significantly higher than has been achieved previously using more conventional synthesis routes and thus demonstrating the power of using the HT approach.

High-throughput powder diffraction V: the use of Raman spectroscopy with and without X-ray powder diffraction data

In high-throughput crystallography it is possible to accumulate large numbers of powder diffraction patterns on a series of related compounds, often polymorphs, salts or co-crystals. In previous papers [Gilmore, Barr & Paisley (2004).J. Appl. Cryst.37, 231–242; Barr, Dong & Gilmore (2004).J. Appl. Cryst.37, 243–252] it has been shown how such data can be analysed by generating an (n×n) correlation matrix,ρ, by correlatingnfull powder diffraction patterns, point by point. Theρmatrix is used as a source of dendrograms and metric multidimensional plots in three or more dimensions which classify the patterns into sets related by similarity. In this paper, it is shown how Raman spectroscopy data can be used by themselves or as an adjunct to powder diffraction data by combining the two techniques using the individual differences scaling method (INDSCAL) of Carroll & Chang [Psychometria, (1970),35, 283–319]. The method is very robust, and can be extended to other forms of spectroscopy. It is available as an option in the commercialPolySNAP3computer program.

A dedicated powder diffraction beamline at the Advanced Photon Source: Commissioning and early operational results

A new dedicated high-resolution high-throughput powder diffraction beamline has been built, fully commissioned, and opened to general users at the Advanced Photon Source. The optical design and commissioning results are presented. Beamline performance was examined using a mixture of the NIST Si and Al(2)O(3) standard reference materials, as well as the LaB6 line-shape standard. Instrumental resolution as high as 1.7 x 10(-4) (DeltaQQ) was observed.

High-throughput powder diffraction. IV. Cluster validation using silhouettes and fuzzy clustering

In two previous papers [Gilmore, Barr & Paisley (2004).J. Appl. Cryst.37, 231–242; Barr, Dong & Gilmore (2004).J. Appl. Cryst.37, 243–252], it was demonstrated how to generate a correlation matrix by comparing full powder diffraction patterns, and then partition the diffractograms into groups using multivariate statistics and associated classification procedures. For clustering the patterns into related sets, dendrograms, metric multidimensional scaling and three-dimensional principal-components analysis score plots are employed. However, sometimes cluster membership for certain patterns is not always very clear or other ambiguities may arise; this paper describes cluster validation techniques using silhouettes and fuzzy clustering. The two methods operate in a complementary way: in some cases silhouettes are the most useful, and in others fuzzy clustering is more applicable. These procedures are available as options in the commercial computer programPolySNAP.

High-throughput powder diffraction. III. The application of full-profile pattern matching and multivariate statistical analysis to round-robin-type data sets

Powder pattern matching techniques, using all the experimentally measured data points, coupled with cluster analysis, fuzzy clustering and multivariate statistical methods are used, with appropriate visualization tools, to analyse a set of 27 powder diffraction patterns of alumina collected at seven different laboratories on different instruments as part of an International Center for Diffraction Data Grant-in-Aid program. In their original form, the data factor into six distinct clusters. However, when a non-linear shift of the form \Delta \left({2\theta } \right)\, = \,a_0 \, + \,a_1 \sin \theta (wherea0anda1are refinable constants) is applied to optimize the correlations between patterns, clustering produces a large 25-pattern set with two outliers. The first outlier is a synchrotron data set at a different wavelength from the other data, and the second is distinguished by the absence ofKα2lines,i.e.it uses Ge-monochromated incident X-rays. Fuzzy clustering, in which samples may belong to more than one cluster, is introduced as a complementary method of pinpointing problematic diffraction patterns. In contrast to the usual methodology associated with the analysis of round-robin data, this process is carried out in a routine way, with minimal user interaction or supervision, using thePolySNAPsoftware.

PolySNAP: a computer program for analysing high-throughput powder diffraction data

In high-throughput crystallography experiments, it is possible to measure over 1000 powder diffraction patterns on a series of related compounds, often polymorphs or salts, in less than one week. The analysis of these patterns poses a difficult statistical problem. A computer program is presented that can analyse such data, automatically sort the patterns into related clusters or classes, characterize each cluster and identify any unusual samples containing, for example, unknown or unexpected polymorphs. Mixtures may be analysed quantitatively if a database of pure phases is available. A key component of the method is a set of visualization tools based on dendrograms and pie charts, as well as principal-component analysis and metric multidimensional scaling as a source of three-dimensional score plots. The procedures have been incorporated into the computer programPolySNAP, which is available commercially from Bruker-AXS.

High-throughput powder diffraction. II. Applications of clustering methods and multivariate data analysis

In high-throughput crystallography, it is possible to accumulate over 1000 powder diffraction patterns on a series of related compounds, often polymorphs. A method is presented that can analyse such data, automatically sort the patterns into related clusters or classes, characterize each cluster and identify any unusual samples containing, for example, unknown or unexpected polymorphs. Mixtures may be analysed quantitatively if a database of pure phases is available. A key component of the method is a set of visualization tools based on dendrograms, cluster analysis, pie charts, principal-component-based score plots and metric multidimensional scaling. Applications to pharmaceutical data and inorganic compounds are presented. The procedures have been incorporated into thePolySNAPcommercial computer software.

High-throughput powder diffraction. I. A new approach to qualitative and quantitative powder diffraction pattern analysis using full pattern profiles

A new integrated approach to full powder diffraction pattern analysis is described. This new approach incorporates wavelet-based data pre-processing, non-parametric statistical tests for full-pattern matching, and singular value decomposition to extract quantitative phase information from mixtures. Every measured data point is used in both qualitative and quantitative analyses. The success of this new integrated approach is demonstrated through examples using several test data sets. The methods are incorporated within the commercial software programSNAP-1D, and can be extended to high-throughput powder diffraction experiments.