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MacDowell, Alastair A.

Publications and source records attributed to MacDowell, Alastair A..

In situ X-ray and IR probes relevant to Earth science at the Advanced Light Source at Lawrence Berkeley Laboratory

Access to synchrotron X-ray facilities has become an important aspect for many disciplines in experimental Earth science. This is especially important for studies that rely on probing samples in situ under natural conditions different from the ones found at the surface of the Earth. The non-ambient condition Earth science program at the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory, offers a variety of tools utilizing the infra-red and hard X-ray spectrum that allow Earth scientists to probe Earth and environmental materials at variable conditions of pressure, stress, temperature, atmospheric composition, and humidity. These facilities are important tools for the user community in that they offer not only considerable capacity (non-ambient condition diffraction) but also complementary (IR spectroscopy, microtomography), and in some cases unique (Laue microdiffraction) instruments. The availability of the ALS’ in situ probes to the Earth science community grows especially critical during the ongoing dark time of the Advanced Photon Source in Chicago, which massively reduces available in situ synchrotron user time in North America.

58 GEOSCIENCES↗

The hard x-ray nanotomography microscope at the advanced light source

Beamline 11.3.1 at the Advanced Light Source is a tender/hard (6–17 keV) x-ray bend magnet beamline recently re-purposed with a new full-field, nanoscale transmission x-ray microscope. The microscope is designed to image composite and porous materials possessing a submicrometer structure and compositional heterogeneity that determine materials’ performance and geologic behavior. The theoretical and achieved resolutions are 55 and <100 nm, respectively. The microscope is used in tandem with a <25 nm eccentricity rotation stage for high-resolution volume imaging using nanoscale computed tomography. The system also features a novel bipolar illumination condenser for the illumination of an ~100 μm spot of interest on the sample, followed by a phase-type zone plate magnifying objective of ~52 µm field of view and a phase detection ring. The zone plate serves as the system objective and magnifies the sample with projection onto an indirect x-ray detection system, consisting of a polished single crystal CsI(Tl) scintillator and a range of high-quality Plan Fluorite visible light objectives. The objectives project the final visible light image onto a water-cooled CMOS 2048 × 2048-pixel 2 detector. Here, in this paper, we will discuss the salient features of this instrument and describe early results from imaging the internal three-dimensional microstructure and nanostructure of target materials, including fiber-reinforced composites and geomaterials.

47 OTHER INSTRUMENTATION↗

Revealing the ductility of nanoceramic MgAl 2 O 4

Ceramics are strong but brittle. As stated in classical theories, ceramics are brittle mainly because dislocations are suppressed by cracks. Here, the authors report the combined elastic and plastic deformation measurements of nanoceramics, in which dislocation-mediated stiff and ductile behaviors were detected at room temperature. In the synchrotron-based deformation experiments, a marked slope change is observed in the stress–strain relationship of MgAl 2 O 4 nanoceramics at high pressures, indicating that a deformation mechanism shift occurs in the compression and that the nanoceramics sample is elastically stiffer than its bulk counterpart. The bulk-sized MgAl 2 O 4 shows no texturing at pressures up to 37 GPa, which is compatible with the brittle behaviors of ceramics. Interestingly, substantial texturing is seen in nanoceramic MgAl 2 O 4 at pressures above 4 GPa. The observed stiffening and texturing indicate that dislocation-mediated mechanisms, usually suppressed in bulk-sized ceramics at low temperature, become operative in nanoceramics. This makes nanoceramics stiff and ductile.

36 MATERIALS SCIENCE↗

Implementation and application of the peak scaling method for temperature measurement in the laser heated diamond anvil cell

In this work, a new design for a double-sided high-pressure diamond anvil cell laser heating set-up is described. The prototype is deployed at beamline 12.2.2 of the Advanced Light Source at Lawrence Berkeley National Lab. Our compact design features shortened mechanical lever arms, which results in more stable imaging optics, and thus more user friendly and more reliable temperature measurements based on pyrometry. A modification of the peak scaling method was implemented for pyrometry, including an iterative method to determine the absolute peak temperature, thus allowing for quasi-real time temperature mapping of the actual hotspot within a laser-heated diamond anvil cell without any assumptions on shape, size, and symmetry of the hotspot and without any assumptions to the relationship between fitted temperature and peak temperature. This is important since we show that the relationship between peak temperature and temperature obtained by fitting the Planck function against the thermal emission spectrum averaged over the entire hotspot is not constant but depends on variable fitting parameters (in particular, the size and position of the fitting window). The accuracy of the method is confirmed through measuring melting points of metal wires at ambient pressure. Having absolute temperature maps in real time allows for more differentiated analyses of laser heating experiments. Finally, we present such an example of the pressure variations within a heated hotspot of AgI at a loaded base pressure of 3.8 GPa.

42 ENGINEERING↗

Soft x-ray spectroscopy of high pressure liquid

Here, we describe a new experimental technique that allows for soft x-ray spectroscopy studies (~100-1000 eV) of high pressure liquid (~100 bars). We achieve this through a liquid cell with a 100 nm-thick Si 3 N 4 membrane window, which is sandwiched by two identical O-rings for vacuum sealing. The thin Si 3 N 4 membrane allows soft x-rays to penetrate, while separating the high-pressure liquid under investigation from the vacuum required for soft x-ray transmission and detection. The burst pressure of the Si 3 N 4 membrane increases with decreasing size and more specifically is inversely proportional to the side length of the square window. It also increases proportionally with the membrane thickness. Pressures > 60 bars could be achieved for 100 nm-thick square Si 3 N 4 windows that are smaller than 65 μm. However, above a certain pressure, the failure of the Si wafer becomes the limiting factor. The failure pressure of the Si wafer is sensitive to the wafer thickness. Moreover, the deformation of the Si 3 N 4 membrane is quantified using vertical scanning interferometry. As an example of the performance of the high-pressure liquid cell optimized for total-fluorescence detected soft x-ray absorption spectroscopy (sXAS), the sXAS spectra at the Ca L edge (~350 eV) of a CaCl 2 aqueous solution are collected under different pressures up to 41 bars.

36 MATERIALS SCIENCE↗

X-ray Micro-Tomography of Ablative Heat Shield Materials

X-ray micro-tomography is a non-destructive characterization technique that allows imaging of materials structures with voxel sizes in the micrometer range. This level of resolution makes the technique very attractive for imaging porous ablators used in hypersonic entry systems. Besides providing a high fidelity description of the material architecture, micro-tomography enables computations of bulk material properties and simulations of micro-scale phenomena. This presentation provides an overview of a collaborative effort between NASA Ames Research Center and Lawrence Berkeley National Laboratory, aimed at developing micro-tomography experiments and simulations for porous ablative materials. Measurements are carried using x-rays from the Advanced Light Source at Berkeley Lab on different classes of ablative materials used in NASA entry systems. Challenges, strengths and limitations of the technique for imaging materials such as lightweight carbon-phenolic systems and woven textiles are discussed. Computational tools developed to perform numerical simulations based on micro-tomography are described. These enable computations of material properties such as permeability, thermal and radiative conductivity, tortuosity and other parameters that are used in ablator response models. Finally, we present the design of environmental cells that enable imaging materials under simulated operational conditions, such as high temperature, mechanical loads and oxidizing atmospheres.Keywords: Micro-tomography, Porous media, Ablation

tomography↗

Real-time data-intensive computing

Today users visit synchrotrons as sources of understanding and discovery—not as sources of just light, and not as sources of data. To achieve this, the synchrotron facilities frequently provide not just light but often the entire end station and increasingly, advanced computational facilities that can reduce terabytes of data into a form that can reveal a new key insight. The Advanced Light Source (ALS) has partnered with high performance computing, fast networking, and applied mathematics groups to create a “super-facility”, giving users simultaneous access to the experimental, computational, and algorithmic resources to make this possible. This combination forms an efficient closed loop, where data—despite its high rate and volume—is transferred and processed immediately and automatically on appropriate computing resources, and results are extracted, visualized, and presented to users or to the experimental control system, both to provide immediate insight and to guide decisions about subsequent experiments during beamtime. We will describe our work at the ALS ptychography, scattering, micro-diffraction, and micro-tomography beamlines.

43 PARTICLE ACCELERATORS↗

Making Advanced Scientific Algorithms and Big Scientific Data Management More Accessible

Synchrotrons such as the Advanced Light Source (ALS) at Lawrence Berkeley National Laboratory are known as user facilities. They are sources of extremely bright X-ray beams, and scientists come from all over the world to perform experiments that require these beams. As the complexity of experiments has increased, and the size and rates of data sets has exploded, managing, analyzing and presenting the data collected at synchrotrons has been an increasing challenge. The ALS has partnered with high performance computing, fast networking, and applied mathematics groups to create a"super-facility", giving users simultaneous access to the experimental, computational, and algorithmic resources to overcome this challenge. This combination forms an efficient closed loop, where data despite its high rate and volume is transferred and processed, in many cases immediately and automatically, on appropriate compute resources, and results are extracted, visualized, and presented to users or to the experimental control system, both to provide immediate insight and to guide decisions about subsequent experiments during beam-time. In this paper, We will present work done on advanced tomographic reconstruction algorithms to support users of the 3D micron-scale imaging instrument (Beamline 8.3.2, hard X-ray micro-tomography).

97 MATHEMATICS AND COMPUTING↗

High-temperature strain cell for tomographic imaging

This disclosure provides systems, methods, and apparatus related to the high temperature mechanical testing of materials. In one aspect, a method includes providing an apparatus. The apparatus may include a chamber. The chamber may comprise a top portion and a bottom portion, with the top portion and the bottom portion each joined to a window material. A first cooled fixture and a second cooled fixture may be mounted to the chamber and configured to hold the sample in the chamber. A plurality of heating lamps may be mounted to the chamber and positioned to heat the sample. The sample may be placed in the first and the second cooled fixtures. The sample may be heated to a specific temperature using the heating lamps. Radiation may be directed though the window material, the radiation thereafter interacting with the sample and exiting the chamber through the window material.

42 ENGINEERING↗

Tensile testing of materials at high temperatures above 1700 °C with in situ synchrotron X-ray micro-tomography

A compact ultrahigh temperature tensile testing instrument has been designed and fabricated for in situ x-ray micro-tomography using synchrotron radiation at the Advanced Light Source, Lawrence Berkeley National Laboratory. It allows for real time x-ray micro-tomographic imaging of test materials under mechanical load at temperatures up to 2300 °C in controlled environments (vacuum or controlled gas flow). Sample heating is by six infrared halogen lamps with ellipsoidal reflectors arranged in a confocal configuration, which generates an approximately spherical zone of high heat flux approximately 5 mm in diameter. Samples are held between grips connected to a motorized stage that loads the samples in tension or compression with forces up to 2.2 kN. The heating chamber and loading system are water-cooled for thermal stability. The entire instrument is mounted on a rotation stage that allows stepwise recording of radiographs over an angular range of 180°. A thin circumferential (360°) aluminum window in the wall of the heating chamber allows the x-rays to pass through the chamber and the sample over the full angular range. The performance of the instrument has been demonstrated by characterizing the evolution of 3D damage mechanisms in ceramic composite materials under tensile loading at 1750 °C.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗