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At least 19 records

Which Strategy for a Protein Crystallization Project?

The three-dimensional, atomic-resolution protein structures produced by X-ray crystallography over the past 50+ years have led to tremendous chemical understanding of fundamental biochemical processes. The pace of discovery in protein crystallography has increased greatly with advances in molecular biology, crystallization techniques, cryo-crystallography, area detectors, synchrotrons and computing. While the methods used to produce single, well-ordered crystals have also evolved over the years in response to increased understanding and advancing technology, crystallization strategies continue to be rooted in trial-and-error approaches. This review summarizes the current approaches in protein crystallization and surveys the first results to emerge from the structural genomics efforts.

Kundrot, Craig E.↗

Which strategy for a protein crystallization project?

The three-dimensional, atomic-resolution protein structures produced by X-ray crystallography over the past 50+ years have led to tremendous chemical understanding of fundamental biochemical processes. The pace of discovery in protein crystallography has increased greatly with advances in molecular biology, crystallization techniques, cryocrystallography, area detectors, synchrotrons and computing. While the methods used to produce single, well-ordered crystals have also evolved over the years in response to increased understanding and advancing technology, crystallization strategies continue to be rooted in trial-and-error approaches. This review summarizes the current approaches in protein crystallization and surveys the first results to emerge from the structural genomics efforts.

Review↗

Development of a large array of Silicon Drift Detectors for high-rate synchrotron fluorescence spectroscopy

An array of small-area Silicon Drift Detectors (SDD), named Hera, has been developed at Brookhaven National Laboratory (BNL) in the past few years. Its primary application is high-rate spectroscopy at synchrotrons. Each SDD pixel is a 1 mm × 1 mm square to match the footprint of the original diode-based pixel detector called Maia, which was developed for the same application. The replacement of the diode with an SDD allows for better energy resolution at short shaping times and an increased stability of the detector. 32, 96, and 384-channel arrays were designed and fabricated and achieved a Full Width Half Maximum (FWHM) as low as 176 eV at 5.9 keV with peaking time of 1 μs at -13°C. The sensor design, simulation, fabrication, its readout system, and its spectroscopic performance are reported.

47 OTHER INSTRUMENTATION↗

Considerations about future hard x-ray area detectors

X-ray sources continue to advance in both intensity and temporal domains, thereby opening new ways to analyze the structure and properties of matter, provided that the resultant x-ray images can be efficiently and quantitatively recorded. In this perspective we focus on specific limitations of pixel area x-ray detectors. Although pixel area x-ray detectors have also advanced in recent years, many experiments are still detector limited. Specifically, there is need for detectors that can acquire successive images at GHz rates; detectors that can accurately measure both single photon and millions of photons per pixel in the same image at frame rates of hundreds of kHz; and detectors that efficiently capture images of very hard x-rays (20 keV to several hundred keV). The data volumes and data rates of state-of-the-art detection exceeds most practical data storage options and readout bandwidths, thereby necessitating on-line processing of data prior to, or in lieu of full frame readouts.

36 MATERIALS SCIENCE↗

Synchrotron-based Characterization Techniques for Radiation Detection Materials and Devices: An Overview

High-performance room-temperature radiation detectors (high energy resolution for spectrometers, high spatial resolution for imaging devices, and low defect-density for high flux applications) are needed for photon energies (>20 keV) that are not well suited for silicon detectors. Applications for such radiation detectors include nonproliferation, synchrotron, medical, astrophysics, and homeland security. Material- and device- characterization to understand and solve the limiting factors of radiation detection materials and devices is a core element of a radiation detector development R&D program. This presentation will give an overview on the two main synchrotron-based characterization techniques that have been employed by the authors in the last ~20 years: (1) White Beam X-ray Diffraction Topography and (2) Micron-scale detector mapping. A perfect (one domain) crystal (radiation detection material) is a requirement to achieve a highperformance radiation detector. White Beam X-ray Diffraction Topography (WBXDT) allows the rapid screening of the crystallinity of the detector material. With WBXDT we can quickly screen CZT and other crystals to make sure they have only one domain, and to see the presence of extended defects and strain fields.

Camarda, Giuseppe S.↗

High spatial resolution direct conversion amorphous selenium X-ray detectors with monolithically integrated CMOS readout

Recent progress in the field of micron-scale spatial resolution direct conversion X-ray detectors for high-energy synchrotron light sources serve applications ranging from nondestructive and noninvasive microscopy techniques which provide insight into the structure and morphology of crystals, to medical diagnostic measurement devices. Amorphous selenium ( a -Se) as a wide-bandgap thermally evaporated photoconductor exhibits ultra-low thermal generation rates for dark carriers and has been extensively used in X-ray medical imaging. Being an amorphous material, it can further be deposited over large areas at room temperatures and at substantially lower costs as compared to crystalline semiconductors. Here, to address the demands for a high-energy and high spatial resolution X-ray detector for synchrotron light source applications, we have thermally evaporated a -Se on a Mixed-Mode Pixel Array Detector (MM-PAD) Application Specific Integrated Circuit (ASIC). The ASIC format consists of 128 × 128 square pixels each 150 μm on a side. A 200 μm a -Se layer was directly deposited on the ASIC followed by a metal top electrode. The completed detector assembly was tested with 45 kV Ag and 23 kV Cu X-ray tube sources. The detector fabrication, performances, Modulation Transfer Function (MTF) measurements, and simulations are reported.

36 MATERIALS SCIENCE↗

Searching for the Best Protein Crystals: Synchrotron Based Measurements of Protein Crystal Quality

We are developing X-ray diffraction methods to quantitatively evaluate the quality of protein crystals. The ultimate use for these crystal quality will be to optimize crystal growth and freezing conditions to obtain the best diffraction data. We have combined super fine-phi slicing with highly monochromatic, low divergence synchrotron radiation and the ADSC Quantum 4 CCD detector at the Stanford Synchrotron Radiation laboratory beamline 1.5 to accurately measure crystal mosaicity. Comparisons of microgravity versus earth-grown insulin crystals using these methods will be presented.

Borgstahl, Gloria↗

High-resolution in-beam video rate imaging with the ClearXCam for synchrotron beamlines

The ClearXCam detector is a new video rate imaging in-beam monitor based on a diamond sensor. Imaging with 2304 effective pixels is achieved by sequentially biasing one of 48 metal stripes on one side of a diamond sensor, while reading out the current from 48 stripes on the other side of the sensor. This system was characterized for real-time X-ray beam diagnostics at synchrotron beam­line 17-BM at the National Synchrotron Light Source II. Significant results include: detection of in-beam structure via the imaging mode, beam focusing in one minute with real-time imaging feedback during a focusing event, linearity over five orders of magnitude, validation of a fast mode operating at 100 Hz, and sub-micron beam-positioning resolution. The system is now available commercially.

36 MATERIALS SCIENCE↗

Study of perovskite CsPbBr 3 detector polarization and its mitigation with ultrahigh x-ray flux

High-flux capable semiconductor x-ray detectors are essential in various applications, but the detrimental effects of detector polarization limit their use in many cases. Here, for this work, we studied the polarization of perovskite CsPbBr 3 semiconductor detectors using ultrahigh flux synchrotron x rays (10 6 –10 12 photons s –1 mm –2 at 58.61 keV). The CsPbBr 3 detectors did not show immediate polarization prominently until a flux higher than 10 10 photons s –1 mm –2 . Using the pump-and-probe technique, we visualized the spatial and temporal effects of polarization. The polarized region, represented by reduced photocurrent, extended beyond the area under direct irradiation, and the reduced photocurrent persisted after potential de-polarization treatments. We found that stronger applied electric fields and fewer carrier traps can mitigate polarization, represented by less photocurrent deficit. By examining the detectors’ current response under controlled ambient light, low, and high-flux x rays, we studied the trap filling and release behavior of CsPbBr 3 . We discovered that the polarization is caused by partial detector damage due to deep defects generated by ultrahigh flux x-ray irradiation. Our work provides insight into CsPbBr 3 polarization under extremely intense x-ray radiation and shows that reducing crystal defects and increasing detector bias voltage are effective solutions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Unfolding first and second order diffracted radiation when using synchrotron radiation sources - A technique

A technique is presented of using a single calibrated XUV detector for radiometric measurements of synchrotron radiation after the radiation passes through a monochromator that produces a mixture of first- and second-order diffracted radiation. Irradiance measurements are made with the synchrotron source operating at two different energies for the orbiting electrons. The known change in the spectral distribution produced by the electron energy change is used to calculate the flux in both first and second order. The dependence of the precision of these determinations on the two detected currents and on the detector calibration at both first- and second-order wavelengths is calculated. Experimental results using the National Bureau of Standards synchrotron (SURF-I) are presented, and anticipated results for the new NBS electron storage ring (SURF-II) are calculated.

Saloman, E. B.↗

The Simons Observatory: Design, Optimization, and Performance of Low-Frequency Detectors

The Simons Observatory (SO) is a cosmic microwave background (CMB) experiment located in the Atacama Desert in Chile that will make precise temperature and polarization measurements over six spectral bands ranging from 27 to 285 GHz. Three small aperture telescopes (SATs) and one large aperture telescope (LAT) will house ~60,000 detectors and cover angular scales between one arcminute and tens of degrees. We present the performance of the dichroic, low-frequency (LF) lenslet-coupled sinuous antenna transition-edge sensor (TES) bolometer arrays with bands centered at 27 and 39 GHz. The LF focal plane will primarily characterize Galactic synchrotron emission as a critical part of foreground subtraction from CMB data. We will discuss the design, optimization, and current testing status of these pixels.

79 ASTRONOMY AND ASTROPHYSICS↗

Determining the Quantum Detection Efficiency of A Soft X-Ray Micro-Channel Plate Detector for the Lunar Mission, LEXI

Micro-channel plate (MCP) detectors have long been a workhorse for space-based x-ray research and are advantageous over other imaging detectors because of their low size, weight and power. The Lunar Environment heliospheric x-ray Imager (LEXI), will utilize a MCP to image Earth’s magnetosphere in soft x-rays from the lunar surface. A critical element for interpreting on-orbit data is to understand the quantum detection efficiency (QDE) of the MCP. LEXI’s MCP is coated with potassium bromide (KBr) to increase the soft x-ray QDE. Historically, few measurements of QDE exist in the soft x-ray band for KBr detectors. This paper reviews the performance of LEXI’s detector, and the QDE experiment procedure conducted at and results from the Advanced Light Source synchrotron soft x-ray beam line (6.3.2) over the energy range 70eV-1300eV. A unique beam line setup was required to limit the photon flux as to not saturate the pores of the MCP or detector signal chain. The experimental results are similar to previous literature, with some caveats unique to this MCP and experimental setup.

X-ray imaging↗

Cadmium Magnesium Telluride for Next-Generation X-Ray Free Electron Laser, Synchrotron, and Many Other Applications

We developed a picosecond photodetector based on our Bridgman-grown and specially engineered cadmium magnesium telluride (Cd 1–x MgxTe) single crystal that is sensitive to both optical and X-ray pulses for coarse timing in free-electron laser applications. Cd 1–x MgxTe is a widebandgap semiconductor with potential applications, not only in optoelectronics, but also in particle physics as an intense pulse radiation detector for bremsstrahlung, X-ray/gamma-ray radiation, thermal neutrons, and medical imaging. For femtosecond optical and X-ray crosscorrelation, the material must have a very short lifetime, a condition that is opposite to that required for nuclear spectroscopy applications. At the same time, the material also needs to have a very low bulk leakage current, in the 10–90 nA range for voltages to even 1000 V. Hence, the ability to tailor or engineer the material is very crucial. Picosecond response and the crystal growth of this specially engineered Cd 1–x MgxTe material are presented. Furthermore, other characterization and transient measurements are discussed along with room-temperature semiconductor detector performance for other nuclear radiation detection applications.

36 MATERIALS SCIENCE↗

Specimen-displacement correction for powder X-ray diffraction in Debye–Scherrer geometry with a flat area detector

The effect of small changes in the specimen-to-detector distance on the unit-cell parameters is examined for synchrotron powder diffraction in Debye–Scherrer (transmission) geometry with a flat area detector. An analytical correction equation is proposed to fix the shift in 2θ values due to specimen capillary displacement. This equation does not require the use of an internal reference material, is applied during the Rietveld refinement step, and is analogous to the specimen-displacement correction equations for Bragg–Brentano and curved-detector Debye–Scherrer geometry experiments, but has a different functional form. The 2θ correction equation is compared with another specimen-displacement correction based on the use of an internal reference material in which new integration and calibration parameters of area-detector images are determined. Example data sets showing the effect of a 3.3 mm specimen displacement on the unit-cell parameters for 25°C CeO 2 , including both types of displacement correction, are described. These experiments were performed at powder X-ray diffraction beamlines at the National Synchrotron Light Source II at Brookhaven National Laboratory and the Advanced Photon Source at Argonne National Laboratory.

36 MATERIALS SCIENCE↗

Design Improvements and X-Ray Performance of a Time Projection Chamber Polarimeter for Persistent Astronomical Sources

The design of the Time-Projection Chamber (TPC) Polarimeter for the Gravity and Extreme Magnetism Small Explorer (GEMS) was demonstrated to Technology Readiness Level 6 (TRL-6)3 and the flight detectors fabricated, assembled and performance tested. A single flight detector was characterized at the Brookhaven National Laboratory Synchrotron Light Source with polarized X-rays at 10 energies from 2.3-8.0 keV at five detector positions. The detector met all of the GEMS performance requirements. Lifetime measurements have shown that the existing flight design has 23 years of lifetime4, opening up the possibility of relaxing material requirements, in particular the consideration of the use of epoxy, to reduce risk elsewhere. We report on design improvements to the GEMS detector to enable a narrower transfer gap that, when operated with a lower transfer field, reduces asymmetries in the detector response. In addition, the new design reduces cost and risk by simplifying the assembly and reducing production time. Finally, we report on the performance of the narrow-gap detector in response to polarized and unpolarized X-rays.

GEMS↗

XUV radiometric standards at NBS

The far-UV and XUV detector calibration services at NBS, the properties of the detectors, and the spectrometer calibration facilities at the Synchrotron Ultraviolet Radiation Facility (SURF II) at NBS are described. The method used to calibrate the quantum efficiency of windowless photodiode detectors in the ionization chamber, and the facilities for calibrating photodiodes at various wavelengths are discussed. The cathode and anode of the windowless photodiodes and their operation are examined. Consideration is given to the calculation of spectral irradiance from SURF II; the two stations of the spectrometer facility; the large spectrometer calibration chamber; and sources of error in flux determinations for SURF II.

Ott, W. R.↗

tomoCAM : fast model-based iterative reconstruction via GPU acceleration and non-uniform fast Fourier transforms

X-ray-based computed tomography is a well established technique for determining the three-dimensional structure of an object from its two-dimensional projections. In the past few decades, there have been significant advancements in the brightness and detector technology of tomography instruments at synchrotron sources. These advancements have led to the emergence of new observations and discoveries, with improved capabilities such as faster frame rates, larger fields of view, higher resolution and higher dimensionality. These advancements have enabled the material science community to expand the scope of tomographic measurements towards increasingly in situ and in operando measurements. In these new experiments, samples can be rapidly evolving, have complex geometries and restrictions on the field of view, limiting the number of projections that can be collected. In such cases, standard filtered back-projection often results in poor quality reconstructions. Iterative reconstruction algorithms, such as model-based iterative reconstructions (MBIR), have demonstrated considerable success in producing high-quality reconstructions under such restrictions, but typically require high-performance computing resources with hundreds of compute nodes to solve the problem in a reasonable time. Here, tomoCAM , is introduced, a new GPU-accelerated implementation of model-based iterative reconstruction that leverages non-uniform fast Fourier transforms to efficiently compute Radon and back-projection operators and asynchronous memory transfers to maximize the throughput to the GPU memory. The resulting code is significantly faster than traditional MBIR codes and delivers the reconstructive improvement offered by MBIR with affordable computing time and resources. tomoCAM has a Python front-end, allowing access from Jupyter -based frameworks, providing straightforward integration into existing workflows at synchrotron facilities.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗