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Philipp, Hugh T.

Publications and source records attributed to Philipp, Hugh T..

15 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Characterization of a Small-Scale Prototype Detector With Wide Dynamic Range for Time-Resolved High-Energy X-Ray Applications

We present characterization measurements of a fast-framing, wide-dynamic-range x-ray area detector intended for high-energy applications (≥20 keV photons). The MM-PAD-2.1 combines an integrating pixel front-end with a charge-removal mechanism to extend the maximum measurable signal to > 107 20-keV ph/pixel/frame. The charge-removal mechanism is dead-time-less (i.e., incoming signal continues to be integrated by the front-end while charge removal is taking place) up to an incoming photon rate of > 109 20-keV ph/pix/s. A 16×16 pixel prototype was fabricated and characterized using both laboratory and synchrotron x-ray sources, allowing for measurements from single-photon to high-flux conditions. High-flux measurements show linear performance up to ~1010 ph/s in a spot spanning approximately 2×1.5 pixels (FWHM). The onset of temporary radiation damage in the detector was observed during these measurements, manifesting as failure of the digital readout from the detector. These effects were seen to reverse after annealing at 30° C for several hours.

47 OTHER INSTRUMENTATION↗
DOE OSTI2019

Characterization of a Fast-Framing X-Ray Camera With Wide Dynamic Range for High-Energy Imaging

We present first characterization results, with a focus on high-flux measurements, of a fast-framing, wide-dynamic-range x-ray camera intended for high-energy imaging. The MM-PAD-2.1 uses an integrating pixel front-end with a charge removal architecture and in-pixel counter to extend the pixel well depth while maintaining low read noise across the full dynamic range. The charge-removal mechanism is dead-time-less (i.e., incoming signal continues to be integrated by the front-end while charge removal is taking place). The purpose of the highflux characterization was to determine the maximum sustained incident flux that could be measured while still exhibiting linear behavior. To this end, a 16 x 16 pixel prototype was tested at the Advanced Photon Source at Argonne National Laboratory using 10 keV photons generated by an undulator source. The intensity of the incident beam was varied over 3 orders of magnitude using a series of attenuators, and the signal integrated by the MM-PAD-2.1 prototype was compared to that measured by a He-filled ion chamber directly upstream. Initial results indicate linear performance up to ca. 10(10) ph/s in a spot spanning approximately 2 x 1.5 pixels (FWHM). The onset of transient radiation damage was observed during these measurements, characterized primarily by failure of digital readout from the detector ASIC. These effects were observed to reverse after annealing at 30 degrees C for several hours, with full recovery of the detector readout.

Shanks, Katherine S.↗
DOE OSTI2018

Solving protein structure from sparse serial microcrystal diffraction data at a storage-ring synchrotron source

In recent years, the success of serial femtosecond crystallography and the paucity of beamtime at X-ray free-electron lasers have motivated the development of serial microcrystallography experiments at storage-ring synchrotron sources. However, especially at storage-ring sources, if a crystal is too small it will have suffered significant radiation damage before diffracting a sufficient number of X-rays into Bragg peaks for peak-indexing software to determine the crystal orientation. As a consequence, the data frames of small crystals often cannot be indexed and are discarded. Introduced here is a method based on the expand–maximize–compress (EMC) algorithm to solve protein structures, specifically from data frames for which indexing methods fail because too few X-rays are diffracted into Bragg peaks. The method is demonstrated on a real serial microcrystallography data set whose signals are too weak to be indexed by conventional methods. In spite of the daunting background scatter from the sample-delivery medium, it was still possible to solve the protein structure at 2.1 Å resolution. The ability of the EMC algorithm to analyze weak data frames will help to reduce sample consumption. Furthermore, it will also allow serial microcrystallography to be performed with crystals that are otherwise too small to be feasibly analyzed at storage-ring sources.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2017

Reconstructing three-dimensional protein crystal intensities from sparse unoriented two-axis X-ray diffraction patterns

Recently, there has been a growing interest in adapting serial microcrystallography (SMX) experiments to existing storage ring (SR) sources. For very small crystals, however, radiation damage occurs before sufficient numbers of photons are diffracted to determine the orientation of the crystal. The challenge is to merge data from a large number of such `sparse' frames in order to measure the full reciprocal space intensity. To simulate sparse frames, a dataset was collected from a large lysozyme crystal illuminated by a dim X-ray source. The crystal was continuously rotated about two orthogonal axes to sample a subset of the rotation space. With the EMC algorithm [expand–maximize–compress; Loh & Elser (2009). Phys. Rev. E , 80 , 026705], it is shown that the diffracted intensity of the crystal can still be reconstructed even without knowledge of the orientation of the crystal in any sparse frame. Moreover, parallel computation implementations were designed to considerably improve the time and memory scaling of the algorithm. The results show that EMC-based SMX experiments should be feasible at SR sources.

Chemistry↗
DOE OSTI2016

The high dynamic range pixel array detector (HDR-PAD): Concept and design

Experiments at storage ring light sources as well as at next-generation light sources increasingly require detectors capable of high dynamic range operation, combining low-noise detection of single photons with large pixel well depth. XFEL sources in particular provide pulse intensities sufficiently high that a purely photon-counting approach is impractical. The High Dynamic Range Pixel Array Detector (HDR-PAD) project aims to provide a dynamic range extending from single-photon sensitivity to 10{sup 6} photons/pixel in a single XFEL pulse while maintaining the ability to tolerate a sustained flux of 10{sup 11} ph/s/pixel at a storage ring source. Achieving these goals involves the development of fast pixel front-end electronics as well as, in the XFEL case, leveraging the delayed charge collection due to plasma effects in the sensor. A first prototype of essential electronic components of the HDR-PAD readout ASIC, exploring different options for the pixel front-end, has been fabricated. Here, the HDR-PAD concept and preliminary design will be described.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2016

High-speed imaging at high x-ray energy: CdTe sensors coupled to charge-integrating pixel array detectors

Pixel Array Detectors (PADs) consist of an x-ray sensor layer bonded pixel-by-pixel to an underlying readout chip. This approach allows both the sensor and the custom pixel electronics to be tailored independently to best match the x-ray imaging requirements. Here we describe the hybridization of CdTe sensors to two different charge-integrating readout chips, the Keck PAD and the Mixed-Mode PAD (MM-PAD), both developed previously in our laboratory. The charge-integrating architecture of each of these PADs extends the instantaneous counting rate by many orders of magnitude beyond that obtainable with photon counting architectures. The Keck PAD chip consists of rapid, 8-frame, in-pixel storage elements with framing periods <150 ns. The second detector, the MM-PAD, has an extended dynamic range by utilizing an in-pixel overflow counter coupled with charge removal circuitry activated at each overflow. This allows the recording of signals from the single-photon level to tens of millions of x-rays/pixel/frame while framing at 1 kHz. Both detector chips consist of a 128×128 pixel array with (150 µm){sup 2} pixels.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2016

Potential beneficial effects of electron-hole plasmas created in silicon sensors by XFEL-like high intensity pulses for detector development

There is a compelling need for a high frame rate imaging detector with a wide dynamic range, from single x-rays/pixel/pulse to >10{sup 6} x-rays/pixel/pulse, that is capable of operating at both x-ray free electron laser (XFEL) and 3rd generation sources with sustained fluxes of > 10{sup 11} x-rays/pixel/s [1, 2, 3]. We propose to meet these requirements with the High Dynamic Range Pixel Array Detector (HDR-PAD) by (a) increasing the speed of charge removal strategies [4], (b) increasing integrator range by implementing adaptive gain [5], and (c) exploiting the extended charge collection times of electron-hole pair plasma clouds that form when a sufficiently large number of x-rays are absorbed in a detector sensor in a short period of time [6]. We have developed a measurement platform similar to the one used in [6] to study the effects of high electron-hole densities in silicon sensors using optical lasers to emulate the conditions found at XFELs. Characterizations of the employed tunable wavelength laser with picosecond pulse duration have shown Gaussian focal spots sizes of 6 ± 1 µm rms over the relevant spectrum and 2 to 3 orders of magnitude increase in available intensity compared to previous measurements presented in [6]. Results from measurements on a typical pixelated silicon diode intended for use with the HDR-PAD (150 µm pixel size, 500 µm thick sensor) are presented.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

High-speed X-ray imaging pixel array detector for synchrotron bunch isolation

A wide-dynamic-range imaging X-ray detector designed for recording successive frames at rates up to 10 MHz is described. X-ray imaging with frame rates of up to 6.5 MHz have been experimentally verified. The pixel design allows for up to 8–12 frames to be stored internally at high speed before readout, which occurs at a 1 kHz frame rate. An additional mode of operation allows the integration capacitors to be re-addressed repeatedly before readout which can enhance the signal-to-noise ratio of cyclical processes. This detector, along with modern storage ring sources which provide short (10–100 ps) and intense X-ray pulses at megahertz rates, opens new avenues for the study of rapid structural changes in materials. The detector consists of hybridized modules, each of which is comprised of a 500 µm-thick silicon X-ray sensor solder bump-bonded, pixel by pixel, to an application-specific integrated circuit. The format of each module is 128 × 128 pixels with a pixel pitch of 150 µm. In the prototype detector described here, the three-side buttable modules are tiled in a 3 × 2 array with a full format of 256 × 384 pixels. Lastly, we detail the characteristics, operation, testing and application of the detector.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2016

Protein crystal structure from non-oriented, single-axis sparse X-ray data

X-ray free-electron lasers (XFELs) have inspired the development of serial femtosecond crystallography (SFX) as a method to solve the structure of proteins. SFX datasets are collected from a sequence of protein microcrystals injected across ultrashort X-ray pulses. The idea behind SFX is that diffraction from the intense, ultrashort X-ray pulses leaves the crystal before the crystal is obliterated by the effects of the X-ray pulse. The success of SFX at XFELs has catalyzed interest in analogous experiments at synchrotron-radiation (SR) sources, where data are collected from many small crystals and the ultrashort pulses are replaced by exposure times that are kept short enough to avoid significant crystal damage. The diffraction signal from each short exposure is so `sparse' in recorded photons that the process of recording the crystal intensity is itself a reconstruction problem. Using the EMC algorithm, a successful reconstruction is demonstrated here in a sparsity regime where there are no Bragg peaks that conventionally would serve to determine the orientation of the crystal in each exposure. In this proof-of-principle experiment, a hen egg-white lysozyme (HEWL) crystal rotating about a single axis was illuminated by an X-ray beam from an X-ray generator to simulate the diffraction patterns of microcrystals from synchrotron radiation. Millions of these sparse frames, typically containing only ~200 photons per frame, were recorded using a fast-framing detector. It is shown that reconstruction of three-dimensional diffraction intensity is possible using the EMC algorithm, even with these extremely sparse frames and without knowledge of the rotation angle. Further, the reconstructed intensity can be phased and refined to solve the protein structure using traditional crystallographic software. In conclusion, this suggests that synchrotron-based serial crystallography of micrometre-sized crystals can be practical with the aid of the EMC algorithm even in cases where the data are sparse.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2015

Determination of crystallographic intensities from sparse data

X-ray serial microcrystallography involves the collection and merging of frames of diffraction data from randomly oriented protein microcrystals. The number of diffracted X-rays in each frame is limited by radiation damage, and this number decreases with crystal size. The data in the frame are said to be sparse if too few X-rays are collected to determine the orientation of the microcrystal. It is commonly assumed that sparse crystal diffraction frames cannot be merged, thereby setting a lower limit to the size of microcrystals that may be merged with a given source fluence. The EMC algorithm [Loh & Elser (2009), Phys. Rev. E , 80 , 026705] has previously been applied to reconstruct structures from sparse noncrystalline data of objects with unknown orientations [Philipp et al. (2012), Opt. Express , 20 , 13129–13137; Ayyer et al. (2014), Opt. Express , 22 , 2403–2413]. Here, it is shown that sparse data which cannot be oriented on a per-frame basis can be used effectively as crystallographic data. As a proof-of-principle, reconstruction of the three-dimensional diffraction intensity using sparse data frames from a 1.35 kDa molecule crystal is demonstrated. The results suggest that serial microcrystallography is, in principle, not limited by the fluence of the X-ray source, and collection of complete data sets should be feasible at, for instance, storage-ring X-ray sources.

Chemistry↗
DOE OSTI2014

High-dynamic-range coherent diffractive imaging: ptychography using the mixed-mode pixel array detector

Coherent (X-ray) diffractive imaging (CDI) is an increasingly popular form of X-ray microscopy, mainly due to its potential to produce high-resolution images and the lack of an objective lens between the sample and its corresponding imaging detector. One challenge, however, is that very high dynamic range diffraction data must be collected to produce both quantitative and high-resolution images. In this work, hard X-ray ptychographic coherent diffractive imaging has been performed at the P10 beamline of the PETRA III synchrotron to demonstrate the potential of a very wide dynamic range imaging X-ray detector (the Mixed-Mode Pixel Array Detector, or MM-PAD). The detector is capable of single photon detection, detecting fluxes exceeding 1 × 10 8 8-keV photons pixel -1 s -1 , and framing at 1 kHz. A ptychographic reconstruction was performed using a peak focal intensity on the order of 1 × 10 10 photons µm -2 s -1 within an area of approximately 325 nm × 603 nm. This was done without need of a beam stop and with a very modest attenuation, while `still' images of the empty beam far-field intensity were recorded without any attenuation. The treatment of the detector frames and CDI methodology for reconstruction of non-sensitive detector regions, partially also extending the active detector area, are described.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2012

Solving structure with sparse, randomly-oriented x-ray data

Single-particle imaging experiments of biomolecules at x-ray free-electron lasers (XFELs) require processing hundreds of thousands of images that contain very few x-rays. Each low-fluence image of the diffraction pattern is produced by a single, randomly oriented particle, such as a protein. We demonstrate the feasibility of recovering structural information at these extremes using low-fluence images of a randomly oriented 2D x-ray mask. Successful reconstruction is obtained with images averaging only 2.5 photons per frame, where it seems doubtful there could be information about the state of rotation, let alone the image contrast. This is accomplished with an expectation maximization algorithm that processes the low-fluence data in aggregate, and without any prior knowledge of the object or its orientation. The versatility of the method promises, more generally, to redefine what measurement scenarios can provide useful signal.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗