scholarly journals Synchrotron X-ray diffraction experiments with a prototype hybrid pixel detector

2011 ◽  
Vol 45 (1) ◽  
pp. 38-47 ◽  
Author(s):  
C. Le Bourlot ◽  
P. Landois ◽  
S. Djaziri ◽  
P.-O. Renault ◽  
E. Le Bourhis ◽  
...  

A prototype X-ray pixel area detector (XPAD3.1) has been used for X-ray diffraction experiments with synchrotron radiation. The characteristics of this detector are very attractive in terms of fast readout time, high dynamic range and high signal-to-noise ratio. The prototype XPAD3.1 enabled various diffraction experiments to be performed at different energies, sample-to-detector distances and detector angles with respect to the direct beam, yet it was necessary to perform corrections on the diffraction images according to the type of experiment. This paper is focused on calibration and correction procedures to obtain high-quality scientific results specifically developed in the context of three different experiments, namely mechanical characterization of nanostructured multilayers, elastic–plastic deformation of duplex steel and growth of carbon nanotubes.

2020 ◽  
Vol 27 (3) ◽  
pp. 608-615 ◽  
Author(s):  
Tim Brandt van Driel ◽  
Silke Nelson ◽  
Rebecca Armenta ◽  
Gabriel Blaj ◽  
Stephen Boo ◽  
...  

The ePix10ka2M (ePix10k) is a new large area detector specifically developed for X-ray free-electron laser (XFEL) applications. The hybrid pixel detector was developed at SLAC to provide a hard X-ray area detector with a high dynamic range, running at the 120 Hz repetition rate of the Linac Coherent Light Source (LCLS). The ePix10k consists of 16 modules, each with 352 × 384 pixels of 100 µm × 100 µm distributed on four ASICs, resulting in a 2.16 megapixel detector, with a 16.5 cm × 16.5 cm active area and ∼80% coverage. The high dynamic range is achieved with three distinct gain settings (low, medium, high) as well as two auto-ranging modes (high-to-low and medium-to-low). Here the three fixed gain modes are evaluated. The resulting dynamic range (from single photon counting to 10000 photons pixel−1 pulse−1 at 8 keV) makes it suitable for a large number of different XFEL experiments. The ePix10k replaces the large CSPAD in operation since 2011. The dimensions of the two detectors are similar, making the upgrade from CSPAD to ePix10k straightforward for most setups, with the ePix10k improving on experimental performance. The SLAC-developed ePix cameras all utilize a similar platform, are tailored to target different experimental conditions and are designed to provide an upgrade path for future high-repetition-rate XFELs. Here the first measurements on this new ePix10k detector are presented and the performance under typical XFEL conditions evaluated during an LCLS X-ray diffuse scattering experiment measuring the 9.5 keV X-ray photons scattered from a thin liquid jet.


2016 ◽  
Vol 72 (2) ◽  
pp. 236-242 ◽  
Author(s):  
E. van Genderen ◽  
M. T. B. Clabbers ◽  
P. P. Das ◽  
A. Stewart ◽  
I. Nederlof ◽  
...  

Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enablingab initiophasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼0.013 e− Å−2 s−1) were collected at room temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS,SHELX) and for electron crystallography (ADT3D/PETS,SIR2014).


2007 ◽  
Vol 98 (1) ◽  
pp. 502-512 ◽  
Author(s):  
Michael T. Lippert ◽  
Kentaroh Takagaki ◽  
Weifeng Xu ◽  
Xiaoying Huang ◽  
Jian-Young Wu

We describe methods to achieve high sensitivity in voltage-sensitive dye (VSD) imaging from rat barrel and visual cortices in vivo with the use of a blue dye RH1691 and a high dynamic range imaging device (photodiode array). With an improved staining protocol and an off-line procedure to remove pulsation artifact, the sensitivity of VSD recording is comparable with that of local field potential recording from the same location. With this sensitivity, one can record from ∼500 individual detectors, each covering an area of cortical tissue 160 μm in diameter (total imaging field ∼4 mm in diameter) and a temporal resolution of 1,600 frames/s, without multiple-trial averaging. We can record 80–100 trials of intermittent 10-s trials from each imaging field before the VSD signal reduces to one half of its initial amplitude because of bleaching and wash-out. Taken together, the methods described in this report provide a useful tool for visualizing evoked and spontaneous waves from rodent cortex.


2002 ◽  
Vol 35 (2) ◽  
pp. 207-211 ◽  
Author(s):  
Diego Pontoni ◽  
T. Narayanan ◽  
Adrian R. Rennie

Data with a wide dynamic range of intensity can be collected with a pinhole high-brilliance small-angle X-ray scattering (SAXS) camera using an image-intensified charge-coupled device (CCD) detector. The point spread function (PSF) of this detector has a narrow peak with a broad low tail such that a high level of scattered intensity at small angles can cause a significant background in the detector elements at higher angles. A correction scheme for the long tail of the PSF of the detector is needed when this integrating area detector is used for measuring intensity that spans a dynamic range of four to five orders of magnitude. A procedure is described for measuring the PSF contribution by masking a small part of the detector from the scattered radiation with an absorbing material. In order to measure the PSF, it is necessary to use a high-intensity spot, which is readily achieved by using a sample that scatters strongly at small angles. Although this intensity is spread over many pixels, the sharp features in the scattering from the silica sample chosen for this study permit one to obtain simultaneously both the narrow and the broad parts of the PSF. The data are compared with the actual scattering function, which has been measured exactly with a point-geometry Bonse–Hart camera. The advantages of this procedure are discussed.


1993 ◽  
Vol 37 ◽  
pp. 145-151
Author(s):  
N. Loxley ◽  
S. Cockerton ◽  
B. K. Tanner

AbstractWe show that a very low noise, high dynamic range scintillation detector has major advantages over conventional detectors for characterization of pseudomorphic HEMT structures by high resolution X-ray diffraction. We show that the reduced background enables a second modulation period to be detected, enabling the thickness and composition to be determined independently. Using a conventional X-ray generator and diffractometer we demonstrate that, in a single scan taking only 10 seconds, we are able to obtain sufficiently good data to provide quality assurance.


2014 ◽  
Vol 70 (a1) ◽  
pp. C694-C694
Author(s):  
Stephan Stern ◽  
Leonard Chavas ◽  
Henry Chapman ◽  
Adrian Mancuso ◽  
Andrew Aquila ◽  
...  

The European X-ray Free-Electron Laser (XFEL.EU) [1] will provide ultra-short, highly-intense, coherent x-ray pulses at an unprecedented repetition rate, transforming experiments in many scientific areas, including serial femtosecond crystallography (SFX). For the purpose of SFX experiments at the XFEL.EU, a dedicated endstation is being developed to be installed within the Single Particles, Clusters and Biomolecules (SPB) instrument [2]. The setup will refocus the beam spent by SPB into a second interaction region, thereby enabling two parallel experiments. In order to overcome various challenges in XFEL crystallography, and to optimize the output for SFX experiments at XFEL.EU, the Adaptive Gain Integrating Pixel Detector (AGIPD) [3] is currently under development and is to be implemented in the SPB instrument, including a 4 Megapixel version for the SFX apparatus. The AGIPD is a hybrid-pixel detector with pixels of 200 x 200 micron^2 each. The gain of each single pixel dynamically and independently adapts to the incoming signal. Thus, diffraction patterns of high dynamic range can be recorded, with the measured signal within a single data frame ranging from single photons and up to 1e+4 photons at 12 keV. Moreover, the AGIPD is designed to store over 350 data frames from successive pulses prior to digitization and read-out, thereby enabling operation at the European XFEL with its challenging repetition rate with 10 Hz pulse trains and a 4.5 MHz intra-train repetition rate. Furthermore, the incorporation of a veto system in AGIPD will allow one to potentially store only the frames that contain diffraction data from actual crystal hits, which ultimately increases the efficiency of the detector and DAQ systems dramatically. In the present work, we will review the design of the 4Mpix AGIPD for the SFX apparatus and discuss simulations and tests of its expected performance under the conditions foreseen for SFX experiments at the XFEL.EU.


2017 ◽  
Vol 12 (12) ◽  
pp. P12003-P12003 ◽  
Author(s):  
M.C. Veale ◽  
P. Adkin ◽  
P. Booker ◽  
J. Coughlan ◽  
M.J. French ◽  
...  

Author(s):  
Emmanuel Wenger ◽  
Slimane Dahaoui ◽  
Paul Alle ◽  
Pascal Parois ◽  
Cyril Palin ◽  
...  

The new generation of X-ray detectors, the hybrid pixel area detectors or `pixel detectors', is based on direct detection and single-photon counting processes. A large linearity range, high dynamic and extremely low noise leading to an unprecedented high signal-to-noise ratio, fast readout time (high frame rates) and an electronic shutter are among their intrinsic characteristics which render them very attractive. First used on synchrotron beamlines, these detectors are also promising in the laboratory, in particular for pump-probe or quasi-static experiments and accurate electron density measurements, as explained in this paper. An original laboratory diffractometer made from a Nonius Mach3 goniometer equipped with an Incoatec Mo microsource and an XPAD pixel area detector has been developed at the CRM2 laboratory. MoKα accurate charge density quality data up to 1.21 Å−1resolution have been collected on a sodium nitroprusside crystal using this home-made diffractometer. Data quality for charge density analysis based on multipolar modelling are discussed in this paper. Deformation electron densities are compared to those already published (based on data collected with CCD APEXII and CAD4 diffractometers).


Author(s):  
Nicolas Casaretto ◽  
Dominik Schaniel ◽  
Paul Alle ◽  
Emmanuel Wenger ◽  
Pascal Parois ◽  
...  

With the remarkable progress of accelerator-based X-ray sources in terms of intensity and brightness, the investigation of structural dynamics from time-resolved X-ray diffraction methods is becoming widespread in chemistry, biochemistry and materials science applications. Diffraction patterns can now be measured down to the femtosecond time-scale using X-ray free electron lasers or table-top laser plasma X-ray sources. On the other hand, the recent developments in photon counting X-ray area detectors offer new opportunities for time-resolved crystallography. Taking advantage of the fast read-out, the internal stacking of recorded images, and the gating possibilities (electronic shutter) of the XPAD hybrid pixel detector, we implemented a laboratory X-ray diffractometer for time-resolved single-crystal X-ray diffraction after pulsed laser excitation, combined with transient optical absorption measurement. The experimental method and instrumental setup are described in detail, and validated using the photoinduced nitrosyl linkage isomerism of sodium nitroprusside, Na2[Fe(CN)5NO]·2H2O, as proof of principle. Light-induced Bragg intensity relative variations ΔI(hkl)/I(hkl) of the order of 1%, due to the photoswitching of the NO ligand, could be detected with a 6 ms acquisition window. The capabilities of such a laboratory time-resolved experiment are critically evaluated.


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