Computer‐assisted area detector masking

Area detectors have become the predominant type of detector for the rapid acquisition of X‐ray diffraction, small‐angle scattering and total scattering. These detectors record the scattering for a large area, giving each shot good statistical significance to the resulting scattered intensity I(Q) pattern. However, many of these detectors have pixel level defects, which cause error in the resulting one‐dimensional patterns. In this work, new software to automatically find and mask these dead pixels and other defects is presented. This algorithm is benchmarked with both ideal simulated and experimental datasets.     

A CCD based detector for quick detection of pressure induced phase transitions

Abstract

A high sensitivity CCD based two dimensional angle dispersive X-ray are a detector has been developed for quick detection of pressure induced phase transitions for a laboratory X-ray source such as a rotating anode generator. The performance of this detector was tested by successfully carrying out powder X-ray diffraction measurements on element Pd, intermetallics AuIn², AuGa² and low Z scatterer adamantane (C₁₀H_l6) at ambient conditions. Its utility for quick detection of phase transitions at high pressures with diamond anvil cell (DAC) is demonstrated by reproducing the known pressure induced structural phase transitions in RbI and KI. The importance of this detector system in search of unknown phase transitions has been established by observing new structural phase transitions in In_0.25Sn_0.75 and AuGa₂. Various softwares have also been developed such as interactive location of centre of diffraction rings, radial integration and image enhancement to analyze data from this detector.     

Eye Opening Degradation due to Sideband Suppression in Direct Detection Systems for Different Signaling Formats

Abstract

The intensity distortion resulting from sideband suppression in direct detection systems is investigated analytically and through numerical simulation for unipolar binary and alternate mark inversion formats. A method to calculate the sequence leading to the highest eye opening penalty is proposed, based on the characterization of the distortion originated by the Hilbert transform of an isolated pulse and constructive/destructive addition of the distortions of pulses in different time slots. The application of the proposed method to a practical transmitter is assessed, and accurate results are shown for signals without complete sideband suppression.     

Angle-dispersive powder diffraction at high pressure using an image-plate area detector

Abstract

An imaging-plate system designed for the full Rietveld refinement of crystal structures at high pressure is described. Emphasis is given to techniques that have been developed to obtain data free from contaminating diffraction peaks and to a general method of processing the diffraction data. The advantages of using pressure cells that allow full diffraction patterns to be collected are also described.

Presented at the IUCr Workshop on ‘Synchrotron Radiation Instrumentation for High Pressure Crystallography’, Daresbury Laboratory 20-21 July 1991     

High pressure,high resolution synchrotron x-ray powder diffraction with a position-sensitive detector

Abstract

We report results of high-pressure experiments with a new diamond-anvil cell in a monochromatic, high-resolution x-ray scattering geometry with alinear position-sensitive detector. The experiments make possible the study of factors controlling line widths of diffraction profiles at pressures in the 100 GPa range, and demonstrate the potential for the use of line profile analysis and Rietveld refinement techniques with high-pressure powder diffraction data. Combined data for various materials indicate that relative contributions to linewidths due to particle size, intrinsic material strength, pressure and state of stress in the sample can be resolved. With light rare-gas solids as pressure-transmitting media, measured FWHMs of the order 0.03? 2 θ corresponding to resolution Δd/d of 2.5 × 10^?3 for 2θ～10-15? are reported. Formation of a high pressure phase appears to involve growth of submicron domains, judging from substantially broadened diffraction peaks under quasihydrostatic conditions. Detailed analysis of complex, non-quenchable high-pressure phases will likely require annealing techniques such as thermal cycling at pressure.

Presented at the IUCr Workshop on ‘Synchrotron Radiation Instrumentation for High Pressure Crystallography’, Daresbury Laboratory 20-21 July 1991     

Application of a hybrid pixel detector to powder diffraction

Results obtained using a hybrid pixel photon‐counting detector in powder diffraction experiments are presented. The detector works at room temperature and its dynamic response ranges from 0.01 photons pixel^?1 s^?1 up to 10⁶ photons pixel^?1 s^?1. The pixel sizes are 0.33 mm × 0.33 mm for a total area of 68 mm × 68 mm. On recording high‐resolution diffraction patterns of powders, a reduction of the experimental time by more than a factor of 20 is obtained without loss of data quality. The example of an X‐zeolite shows that such detectors can be used for very demanding anomalous experiments. In situ experiments of quenching liquid oxides show that frames of 0.01 s can be achieved for studying such processes.     

Performance of the micro‐PIC gaseous area detector in small‐angle X‐ray scattering experiments

The application of a two‐dimensional photon‐counting detector based on a micro‐pixel gas chamber (µ‐PIC) to high‐resolution small‐angle X‐ray scattering (SAXS), and its performance, are reported. The µ‐PIC is a micro‐pattern gaseous detector fabricated by printed circuit board technology. This article describes the performance of the µ‐PIC in SAXS experiments at SPring‐8. A dynamic range of >10⁵ was obtained for X‐ray scattering from a polystyrene sphere solution. A maximum counting rate of up to 5 MHz was observed with good linearity and without saturation. For a diffraction pattern of collagen, weak peaks were observed in the high‐angle region in one accumulation of photons.     

DIOPTAS: a program for reduction of two-dimensional X-ray diffraction data and data exploration

The amount of data collected during synchrotron X-ray diffraction (XRD) experiments is constantly increasing. Most of the time, the data are collected with image detectors, which necessitates the use of image reduction/integration routines to extract structural information from measured XRD patterns. This step turns out to be a bottleneck in the data processing procedure due to a lack of suitable software packages. In particular, fast-running synchrotron experiments require online data reduction and analysis in real time so that experimental parameters can be adjusted interactively. Dioptas is a Python-based program for on-the-fly data processing and exploration of two-dimensional X-ray diffraction area detector data, specifically designed for the large amount of data collected at XRD beamlines at synchrotrons. Its fast data reduction algorithm and graphical data exploration capabilities make it ideal for online data processing during XRD experiments and batch post-processing of large numbers of images.     

LiNbO3晶体在75℃附近赝考塞耳线衍射异常

用X射线发散束背反射赝考塞耳线衍射方法发现纯LiNbO₃和扩Ti的LiNbO₃晶体在75℃附近的衍射花样有明显的异常。(11010),(01110),(0118),(1108),(03312),(33012)等衍射面的考塞耳花样出现成对的大范围非断裂的畸变。畸变接近二次对称,对称面为x面。破坏了沿z轴方向的三次对称性。同时发现高角度的衍射面畸变α较小,或不畸变。布喇格角较小的衍射面畸变较甚。 关键词：     

Backscattering from different objects in turbulent media

Abstract

The connection between diffraction characteristics of the scatterer and distribution of average backscattered intensity of a spherical wave is considered. In experiments with an ‘infinite’ plane mirror it is shown that the distribution of average backscattered intensity coincides with the correlation function of the intensity fluctuation of a virtual point source located at the mirror and observed from the real source plane. Non-monotonic dependence (with a minimum at the Fresnel number of scattered mirror?1) between the enhancement factor and the size of reflected mirror is observed in experiments.     

High temperature—high pressure neutron scattering experiments on expanded liquid alkali metals

Abstract

We present neutron diffraction investigation of the static structure factor S(Q) of liquid alkali metals expanded by heating towards conditions close to their liquid-vapour critical point. The experiments were designed to obtain the characteristic changes of the macroscopic structure as a function of temperature and density. The data give information on the density dependent changes in the interatomic forces. as the metal-nonmental transition is approached in the expanded liquid metal.     

Effects of the deformation of reflection volume Bragg gratings on the M-factor of super-Gaussian laser beams

When high-power laser beams pass through a volume Bragg grating (VBG), the surface of VBG occurs distortion because of thermal effects, and it results in the decline of the grating’s performance. Considering distortion of the surface induces differences of the index and period, the scalar wave equations for super-Gaussian (SG) laser beams propagating in the reflection VBG have been solved by using finite-different and sparse matrix methods. The changes of the total power reflection coefficient, the beam width, the far-field beam angle and the M²-factor for the laser beams through the reflection VBG with deformation have been analyzed quantitatively. It can be shown that the deformation of the VBG affects evidently on the intensity and phase distributions, the total power reflection coefficient, the beam width, the far-field divergence angle and the M²-factor. The beam width, the far-field divergence angle, and the M²-factor of the output beams increase significantly with the distortions of the grating. The influence of the distortions of the VBG on the power reflection coefficient, the far-field divergence angle and the M²-factor of the output beams are smaller for higher beam orders.     

Single crystal diffraction with X-rays and neutrons: High quality at high pressure?

Abstract

Single crystal X-ray and neutron diffraction is essential for determining occupancies, positional as well as static and dynamic displacement parameters in crystalline matter by measuring Bragg, satellite or diffuse reflections. In our contribution a new low-temperature high pressure cell for neutron single crystal diffraction will be presented. It is designed to operate from a few K to ambient temperature in “orange” cryostats at pressures up to at least 3 GPa. We will present first neutron diffraction results obtained at E4/HMI Berlin and discuss the quality of the data and the significance of the results. A software package has been written (as a part of the PROMETHEUS system), which deals with the data reduction for both X-ray and neutron high pressure cell single crystal data. Likewise a data collection program has been developed for single crystal data collection on four-circle diffractometers using Merrill-Bassett cells. A series of single crystal experiments on H₂O and D₂O ice VI and KDP (KH₂PO₄) show that results of very high quality can be obtained routinely including even higher order terms in the atomic displacement parameters.     

Performance of different types of detectors in a high-pressure X-ray study of phase transition

Abstract

Phase transitions in praseodymium and lanthanum under pressure have been studied using a synchrotron powder X-ray diffraction technique. A structure refinement of the distorted fcc phase of Pr using diffraction data collected with an imaging plate (IP) detector demonstrate that among some possible structures the rhombohedral structure with space group R3m best reproduces the observed diffraction pattern. The distorted fcc-fcc phase transition in La was observed as a function of the temperature at 23 GPa using a CCD-based detector. A five-minute exposure sufficiently long to measure the intensities of very weak superlattice reflections from the distorted fcc phase, which has been found to transform to the fcc phase at 550 K. The performance of the IP and a CCD-based detector are compared and their future developments discussed.     

Effect of reflections on phase hologram recording in amorphous As-S-Se films

Experimental and theoretical studies of phase hologram recording in amorphous As-S-Se films with slightly wedge-shaped thickness profile are presented. It is shown that Fabry-Perot resonator effect caused by the interference of multiply reflected light beams inside the sample strongly changes the values of diffraction efficiency and its growth rate as well as the exposure time dependences of diffraction efficiency and transmissivity making them site-dependent and sample-dependent. Absorptivity and recording light intensity inside the sample are also significantly changed. The obtained results can be used to explain the holographic and optical experiments also in other materials with Fabry-Perot resonator effect such as other transparent thin films and photorefractive crystals.     

High‐energy X‐ray diffraction using the Pixium 4700 flat‐panel detector

The Pixium 4700 detector represents a significant step forward in detector technology for high‐energy X‐ray diffraction. The detector design is based on digital flat‐panel technology, combining an amorphous Si panel with a CsI scintillator. The detector has a useful pixel array of 1910 × 2480 pixels with a pixel size of 154 µm × 154 µm, and thus it covers an effective area of 294 mm × 379 mm. Designed for medical imaging, the detector has good efficiency at high X‐ray energies. Furthermore, it is capable of acquiring sequences of images at 7.5 frames per second in full image mode, and up to 60 frames per second in binned region of interest modes. Here, the basic properties of this detector applied to high‐energy X‐ray diffraction are presented. Quantitative comparisons with a widespread high‐energy detector, the MAR345 image plate scanner, are shown. Other properties of the Pixium 4700 detector, including a narrow point‐spread function and distortion‐free image, allows for the acquisition of high‐quality diffraction data at high X‐ray energies. In addition, high frame rates and shutterless operation open new experimental possibilities. Also provided are the necessary data for the correction of images collected using the Pixium 4700 for diffraction purposes.     

Crystal structure of NaNO3 at high pressure

Abstract

Effect of high pressure on the crystal structure of rhombohedral NaNO₃ was investigated by X-ray diffraction of single crystals mounted in a miniature diamond-anvil cell on synchrotron radiation source. Diffraction intensity measurements were made at three pressures across a suggested transition pressure 4.3 GPa. No change was observed in an overall distribution of reflections in the reciprocal space with increasing pressure, but there was a systematic variation in diffraction intensity for particular groups of reflections. An analysis based on the structure factor calculation showed that a structure change induced by pressure is mainly a rotation of the nitrate groups in the alternate layers along the threefold axis in opposite directions. Least-squares refinement of the atomic positional parameters yielded the angle of the rotation to be 4.3 and 7.0 deg at pressures of 4.4 and 5.0 GPa, respectively. It has also been shown that the positions of the sodium and nitrogen atoms are slightly displaced along the axis, resulting in the formation of dipoles in the high pressure phase.     

Small‐angle solution scattering using the mixed‐mode pixel array detector

Solution small‐angle X‐ray scattering (SAXS) measurements were obtained using a 128 × 128 pixel X‐ray mixed‐mode pixel array detector (MMPAD) with an 860 µs readout time. The MMPAD offers advantages for SAXS experiments: a pixel full‐well of >2 × 10⁷ 10 keV X‐rays, a maximum flux rate of 10⁸ X‐rays pixel^?1 s^?1, and a sub‐pixel point‐spread function. Data from the MMPAD were quantitatively compared with data from a charge‐coupled device (CCD) fiber‐optically coupled to a phosphor screen. MMPAD solution SAXS data from lysozyme solutions were of equal or better quality than data captured by the CCD. The read‐noise (normalized by pixel area) of the MMPAD was less than that of the CCD by an average factor of 3.0. Short sample‐to‐detector distances were required owing to the small MMPAD area (19.2 mm × 19.2 mm), and were revealed to be advantageous with respect to detector read‐noise. As predicted by the Shannon sampling theory and confirmed by the acquisition of lysozyme solution SAXS curves, the MMPAD at short distances is capable of sufficiently sampling a solution SAXS curve for protein shape analysis. The readout speed of the MMPAD was demonstrated by continuously monitoring lysozyme sample evolution as radiation damage accumulated. These experiments prove that a small suitably configured MMPAD is appropriate for time‐resolved solution scattering measurements.     

Synchrotron applications of an amorphous silicon flat‐panel detector

A GE Revolution 41RT flat‐panel detector (GE 41RT) from GE Healthcare (GE) has been in operation at the Advanced Photon Source for over two years. The detector has an active area of 41 cm × 41 cm with 200 µm × 200 µm pixel size. The nominal working photon energy is around 80 keV. The physical set‐up and utility software of the detector system are discussed in this article. The linearity of the detector response was measured at 80.7 keV. The memory effect of the detector element, called lag, was also measured at different exposure times and gain settings. The modulation transfer function was measured in terms of the line‐spread function using a 25 µm × 1 cm tungsten slit. The background (dark) signal, the signal that the detector will carry without exposure to X‐rays, was measured at three different gain settings and with exposure times of 1 ms to 15 s. The radial geometric flatness of the sensor panel was measured using the diffraction pattern from a CeO₂ powder standard. The large active area and fast data‐capturing rate, i.e. 8 frames s^?1 in radiography mode, 30 frames s^?1 in fluoroscopy mode, make the GE 41RT one of a kind and very versatile in synchrotron diffraction. The loading behavior of a Cu/Nb multilayer material is used to demonstrate the use of the detector in a strain–stress experiment. Data from the measurement of various samples, amorphous SiO₂ in particular, are presented to show the detector effectiveness in pair distribution function measurements.     

Effects of pressure on the two polymorphs of [Co(NH3)5NO2]I2: The anisotropy of lattice distortion and a phase transition

Abstract

The effect of pressure on the two polymorphs of [CO(NH₃)₅NO₂]I₂ (phase I-orthorhombic, S.G. Pnma; phase II-monoclinic, S.G. C2/m) was studied by X-ray powder diffraction in a diamond anvil cell (DAC). In the presence of the ethanol-methanol-water mixture used as a pressure-transmitting liquid polymorph I was shown to undergo a phase transition at pressures between 0.45 GPa and 0.65 GPa. The diffraction pattern of the high-pressure phase (phase III) could be indexed as tetragonal with lattice parameters similar to those, which were previously reported for polymorph II in a 'pseudotetragonal setting'. The lattice distortions of phases II and III were studied at pressures up to 3.2 GPa and 3.7 GPa, correspondingly, and were shown to be very similar. Phases II and III were supposed to be very closely related. If poly(chlortrifluorethylen)-oil was used as a pressure-transmitting medium, no phase transitions were observed in phase I of [CO(NH₃)₅NO₂I₂ at least up to 1.8 GPa (the point when poly(chlortrifluorethylen)-oil becomes solid), and the anisotropy of lattice distortion could be measured.