I12 is the Joint Engineering, Environmental and Processing (JEEP) beamline, constructed during Phase II of the Diamond Light Source. I12 is located on a short (5 m) straight section of the Diamond ...storage ring and uses a 4.2 T superconducting wiggler to provide polychromatic and monochromatic X‐rays in the energy range 50–150 keV. The beam energy enables good penetration through large or dense samples, combined with a large beam size (1 mrad horizontally × 0.3 mrad vertically). The beam characteristics permit the study of materials and processes inside environmental chambers without unacceptable attenuation of the beam and without the need to use sample sizes which are atypically small for the process under study. X‐ray techniques available to users are radiography, tomography, energy‐dispersive diffraction, monochromatic and white‐beam two‐dimensional diffraction/scattering and small‐angle X‐ray scattering. Since commencing operations in November 2009, I12 has established a broad user community in materials science and processing, chemical processing, biomedical engineering, civil engineering, environmental science, palaeontology and physics.
The I21 beamline at Diamond Light Source is dedicated to advanced resonant inelastic X‐ray scattering (RIXS) for probing charge, orbital, spin and lattice excitations in materials across condensed ...matter physics, applied sciences and chemistry. Both the beamline and the RIXS spectrometer employ divergent variable‐line‐spacing gratings covering a broad energy range of 280–3000 eV. A combined energy resolution of ∼35 meV (16 meV) is readily achieved at 930 eV (530 eV) owing to the optimized optics and the mechanics. Considerable efforts have been paid to the design of the entire beamline, particularly the implementation of the collection mirrors, to maximize the X‐ray photon throughput. The continuous rotation of the spectrometer over 150° under ultra high vacuum and a cryogenic manipulator with six degrees of freedom allow accurate mappings of low‐energy excitations from solid state materials in momentum space. Most importantly, the facility features a unique combination of the high energy resolution and the high photon throughput vital for advanced RIXS applications. Together with its stability and user friendliness, I21 has become one of the most sought after RIXS beamlines in the world.
The design of the resonant inelastic X‐ray scattering beamline at Diamond Light Source, I21, is presented. X‐ray commissioning results are shown and compared with the optical simulations.
Fast X-ray powder diffraction on I11 at Diamond Thompson, Stephen P.; Parker, Julia E.; Marchal, Julien ...
Journal of synchrotron radiation,
July 2011, Letnik:
18, Številka:
4
Journal Article
Recenzirano
Odprti dostop
The commissioning and performance characterization of a position‐sensitive detector designed for fast X‐ray powder diffraction experiments on beamline I11 at Diamond Light Source are described. The ...detecting elements comprise 18 detector‐readout modules of MYTHEN‐II silicon strip technology tiled to provide 90° coverage in 2θ. The modules are located in a rigid housing custom designed at Diamond with control of the device fully integrated into the beamline data acquisition environment. The detector is mounted on the I11 three‐circle powder diffractometer to provide an intrinsic resolution of Δ2θ≃ 0.004°. The results of commissioning and performance measurements using reference samples (Si and AgI) are presented, along with new results from scientific experiments selected to demonstrate the suitability of this facility for powder diffraction experiments where conventional angle scanning is too slow to capture rapid structural changes. The real‐time dehydrogenation of MgH2, a potential hydrogen storage compound, is investigated along with ultrafast high‐throughput measurements to determine the crystallite quality of different samples of the metastable carbonate phase vaterite (CaCO3) precipitated and stabilized in the presence of amino acid molecules in a biomimetic synthesis process.
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, TiO2 and 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−xFexO10 heterometallic 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 to x = 0.5, significantly higher than has been achieved previously using more conventional synthesis routes and thus demonstrating the power of using the HT approach.
The identification of preferred binding domains within a host structure provides important insights into the function of materials. State-of-the-art reports mostly focus on crystallographic studies ...of empty and single component guest-loaded host structures to determine the location of guests. However, measurements of material properties (e.g., adsorption and breakthrough of substrates) are usually performed for a wide range of pressure (guest coverage) and/or using multi-component gas mixtures. Here we report the development of a multifunctional gas dosing system for use in X-ray powder diffraction studies on Beamline I11 at Diamond Light Source. This facility is fully automated and enables in situ crystallographic studies of host structures under (i) unlimited target gas loadings and (ii) loading of multi-component gas mixtures. A proof-of-concept study was conducted on a hydroxyl-decorated porous material MFM-300(VIII) under (i) five different CO2 pressures covering the isotherm range and (ii) the loading of equimolar mixtures of CO2/N2. The study has successfully captured the structural dynamics underpinning CO2 uptake as a function of surface coverage. Moreover, MFM-300(VIII) was incorporated in a mixed matrix membrane (MMM) with PIM-1 in order to evaluate the CO2/N2 separation potential of this material. Gas permeation measurements on the MMM show a great improvement over the bare PIM-1 polymer for CO2/N2 separation based on the ideal selectivity.
The identification of preferred binding domains within a host structure provides important insights into the function of materials. State-of-the-art reports mostly focus on crystallographic studies ...of empty and single component guest-loaded host structures to determine the location of guests. However, measurements of material properties (
e.g.
, adsorption and breakthrough of substrates) are usually performed for a wide range of pressure (guest coverage) and/or using multi-component gas mixtures. Here we report the development of a multifunctional gas dosing system for use in X-ray powder diffraction studies on Beamline I11 at Diamond Light Source. This facility is fully automated and enables
in situ
crystallographic studies of host structures under (i) unlimited target gas loadings and (ii) loading of multi-component gas mixtures. A proof-of-concept study was conducted on a hydroxyl-decorated porous material MFM-300(V
III
) under (i) five different CO
2
pressures covering the isotherm range and (ii) the loading of equimolar mixtures of CO
2
/N
2
. The study has successfully captured the structural dynamics underpinning CO
2
uptake as a function of surface coverage. Moreover, MFM-300(V
III
) was incorporated in a mixed matrix membrane (MMM) with PIM-1 in order to evaluate the CO
2
/N
2
separation potential of this material. Gas permeation measurements on the MMM show a great improvement over the bare PIM-1 polymer for CO
2
/N
2
separation based on the ideal selectivity.
CO
2
binding and separation using porous MFM-300(V
III
) has been fully studied.
CO
2
binding and separation using porous MFM-300(V
III
) has been fully studied.
The identification of preferred binding domains within a host structure provides important insights into the function ...of materials. State-of-the-art reports mostly focus on crystallographic studies of empty and single component guest-loaded host structures to determine the location of guests. However, measurements of material properties (
e.g.
, adsorption and breakthrough of substrates) are usually performed for a wide range of pressure (guest coverage) and/or using multi-component gas mixtures. Here we report the development of a multifunctional gas dosing system for use in X-ray powder diffraction studies on Beamline I11 at Diamond Light Source. This facility is fully automated and enables
in situ
crystallographic studies of host structures under (i) unlimited target gas loadings and (ii) loading of multi-component gas mixtures. A proof-of-concept study was conducted on a hydroxyl-decorated porous material MFM-300(V
III
) under (i) five different CO
2
pressures covering the isotherm range and (ii) the loading of equimolar mixtures of CO
2
/N
2
. The study has successfully captured the structural dynamics underpinning CO
2
uptake as a function of surface coverage. Moreover, MFM-300(V
III
) was incorporated in a mixed matrix membrane (MMM) with PIM-1 in order to evaluate the CO
2
/N
2
separation potential of this material. Gas permeation measurements on the MMM show a great improvement over the bare PIM-1 polymer for CO
2
/N
2
separation based on the ideal selectivity.
The identification of preferred binding domains within a host structure provides important insights into the function of materials. State-of-the-art reports mostly focus on crystallographic studies ...of empty and single component guest-loaded host structures to determine the location of guests. However, measurements of material properties (
, adsorption and breakthrough of substrates) are usually performed for a wide range of pressure (guest coverage) and/or using multi-component gas mixtures. Here we report the development of a multifunctional gas dosing system for use in X-ray powder diffraction studies on Beamline I11 at Diamond Light Source. This facility is fully automated and enables
crystallographic studies of host structures under (i) unlimited target gas loadings and (ii) loading of multi-component gas mixtures. A proof-of-concept study was conducted on a hydroxyl-decorated porous material MFM-300(V
) under (i) five different CO
pressures covering the isotherm range and (ii) the loading of equimolar mixtures of CO
/N
. The study has successfully captured the structural dynamics underpinning CO
uptake as a function of surface coverage. Moreover, MFM-300(V
) was incorporated in a mixed matrix membrane (MMM) with PIM-1 in order to evaluate the CO
/N
separation potential of this material. Gas permeation measurements on the MMM show a great improvement over the bare PIM-1 polymer for CO
/N
separation based on the ideal selectivity.
Residual and intrinsic strains in granular materials have been studied extensively. However, understanding the dynamic strains that cause these resultant residual strains is key to developing better ...strain‐resistant materials. This investigation demonstrates a method for characterizing dynamic strain propagation in granular materials. The specimen is a zirconia‐based refractory composed of sol–gel‐derived zirconia nanoparticles in a potassium silicate glass binder. In situ synchrotron X‐ray powder diffraction in flat‐plate geometry is used to characterize the sample structure on timescales of the order of 1 ms. A 125 W CO2 laser is used to strain the sample with a 25 ms pulse length. To compensate for the poor flux on this timescale, a pump–probe method is repeated 1000 times and the resulting data are subsequently re‐binned to improve statistics. A Gaussian weighting function is also used to introduce better contrast between strained and unstrained frames. TOPAS Academic is used for fitting with a Le Bail model in `batch mode'. Lattice parameters and sample height are refined during fitting, along with a Lorentzian line width for extracting microstrain broadening. Microstrains, ɛ, in the range of 1.01 < ɛ < 1.46% are reported on a 1 ms timescale.
A variable frequency ferroelectric polarisation measurement system has been designed and built at the UK's Diamond Light Source. The electric field induced phase transitions in Pb(Zr1−xTix)O3 (PZT) ...have been used to test the facility via in-situ measurements of electric polarisation and XRD. Stroboscopic and real time data collection methods on polycrystalline samples were employed as a function of frequency to determine the dynamic ferroelectric response. The system has been shown to deliver XRD patterns of good statistical quality measured over 40 points of a ferroelectric PE loop. The system is now available on station I11 as a user facility at the Diamond Light Source.
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