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MacDowell, Alastair

Publications and source records attributed to MacDowell, Alastair.

11 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Compression–tension cell with sample manipulator for in situ X‐ray nanotomography experiments

In situ X-ray nanotomography experiments where tensile or compressive force is applied on the sample require specialized equipment. A compression-tension device with fluid flow-through capability has been designed for X-ray nanotomography beamlines. The compression-tension cell is equipped with a triaxial stage for sample alignment and a high sensitivity loadcell for measurement of applied force. To handle the <100 µm samples used for X-ray nanotomography imaging and for loading samples on the compression-tension cell a sample manipulator has been built. The sample manipulator is capable of selecting a single <100 µm particle for nanotomography scanning while viewing multiple samples under an optical microscope. To test the functionality of these two devices an initial compression experiment involving two glass beads was performed. To demonstrate instrument stability two spherical glass beads were compressed from a no load condition until one of the beads fractured. Nanotomography data were collected at each step of increasing compressive force. The experimentally observed contact area of the spherical glass beads was compared with the theoretical estimate using the Hertz analysis. To demonstrate the fluid flow capability, two calcite grains were compressed against each other under a calcite saturated solution. Surface topological changes were observed for the stressed grain contact area.

X-ray tomography↗
DOE OSTI2024

Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source

Geological samples are inherently multi-scale. Understanding their bulk physical and chemical properties requires characterization down to the nano-scale. A powerful technique to study the three-dimensional microstructure is X-ray tomography, but it lacks information about the chemistry of samples. To develop a methodology for measuring the multi-scale 3D microstructure of geological samples, correlative X-ray micro- and nanotomography were performed on two rocks followed by scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS) analysis. The study was performed in five steps: (i) micro X-ray tomography was performed on rock sample cores, (ii) samples for nanotomography were prepared using laser milling, (iii) nanotomography was performed on the milled sub-samples, (iv) samples were mounted and polished for SEM analysis and (v) SEM imaging and compositional mapping was performed on micro and nanotomography samples for complimentary information. Correlative study performed on samples of serpentine and basalt revealed multiscale 3D structures involving both solid mineral phases and pore networks. Significant differences in the volume fraction of pores and mineral phases were also observed dependent on the imaging spatial resolution employed. This highlights the necessity for the application of such a multiscale approach for the characterization of complex aggregates such as rocks. Information acquired from the chemical mapping of different phases was also helpful in segmentation of phases that did not exhibit significant contrast in X-ray imaging. Adoption of the protocol used in this study can be broadly applied to 3D imaging studies being performed at the Advanced Light Source and other user facilities.

58 GEOSCIENCES↗
DOE OSTI2018

Liebermannite, KAlSi3 O8 , a new shock-metamorphic, high-pressure mineral from the Zagami Martian meteorite

© The Meteoritical Society, 2017. In this paper, we discuss the occurrence of liebermannite (IMA 2013-128), KAlSi3O8, a new, shock-generated, high-pressure tetragonal hollandite-type structure silicate mineral, in the Zagami basaltic shergottite meteorite. Liebermannite crystallizes in space group I4/m with Z = 2, cell dimensions of a = 9.15 ± 0.14 (1σ) Å, c = 2.74 ± 0.13 Å, and a cell volume of 229 ± 19 Å3 (for the type material), as revealed by synchrotron diffraction. In Zagami, liebermannite likely formed via solid-state transformation of primary igneous K-feldspar during an impact event that achieved pressures of ~20 GPa or more. The mineral name is in honor of Robert C. Liebermann, a high-pressure mineral physicist at Stony Brook University, New York, USA.

Ma, Chi↗
DOE OSTI2016

In-situ characterization of highly reversible phase transformation by synchrotron X-ray Laue microdiffraction

The alloy Cu{sub 25}Au{sub 30}Zn{sub 45} undergoes a huge first-order phase transformation (6% strain) and shows a high reversibility under thermal cycling and an unusual martensitc microstructure in sharp contrast to its nearby compositions. This alloy was discovered by systematically tuning the composition so that its lattice parameters satisfy the cofactor conditions (i.e., the kinematic conditions of compatibility between phases). It was conjectured that satisfaction of these conditions is responsible for the enhanced reversibility as well as the observed unusual fluid-like microstructure during transformation, but so far, there has been no direct evidence confirming that these observed microstructures are those predicted by the cofactor conditions. To verify this hypothesis, we use synchrotron X-ray Laue microdiffraction to measure the orientations and structural parameters of variants and phases near the austenite/martensite interface. The areas consisting of both austenite and multi-variants of martensite are scanned by microLaue diffraction. The cofactor conditions have been examined from the kinematic relation of lattice vectors across the interface. The continuity condition of the interface is precisely verified from the correspondent lattice vectors between two phases.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Coded Aperture Imaging for Fluorescent X-rays-Biomedical Applications

Employing a coded aperture pattern in front of a charge couple device pixilated detector (CCD) allows for imaging of fluorescent x-rays (6-25KeV) being emitted from samples irradiated with x-rays. Coded apertures encode the angular direction of x-rays and allow for a large Numerical Aperture x- ray imaging system. The algorithm to develop the self-supported coded aperture pattern of the Non Two Holes Touching (NTHT) pattern was developed. The algorithms to reconstruct the x-ray image from the encoded pattern recorded were developed by means of modeling and confirmed by experiments. Samples were irradiated by monochromatic synchrotron x-ray radiation, and fluorescent x-rays from several different test metal samples were imaged through the newly developed coded aperture imaging system. By choice of the exciting energy the different metals were speciated.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2013

Combined resistive and laser heating technique for in situ radial X-ray diffraction in the diamond anvil cell at high pressure and temperature

To extend the range of high-temperature, high-pressure studies within the diamond anvil cell, a Liermann-type diamond anvil cell with radial diffraction geometry (rDAC) was redesigned and developed for synchrotron X-ray diffraction experiments at beamline 12.2.2 of the Advanced Light Source. The rDAC, equipped with graphite heating arrays, allows simultaneous resistive and laser heating while the material is subjected to high pressure. The goals are both to extend the temperature range of external (resistive) heating and to produce environments with lower temperature gradients in a simultaneously resistive- and laser-heated rDAC. Three different geomaterials were used as pilot samples to calibrate and optimize conditions for combined resistive and laser heating. For example, in Run1, FeO was loaded in a boron-mica gasket and compressed to 11 GPa then gradually resistively heated to 1007 K (1073 K at the diamond side). The laser heating was further applied to FeO to raise temperature to 2273 K. In Run2, Fe-Ni alloy was compressed to 18 GPa and resistively heated to 1785 K (1973 K at the diamond side). The combined resistive and laser heating was successfully performed again on (Mg{sub 0.9}Fe{sub 0.1})O in Run3. In this instance, the sample was loaded in a boron-kapton gasket, compressed to 29 GPa, resistive-heated up to 1007 K (1073 K at the diamond side), and further simultaneously laser-heated to achieve a temperature in excess of 2273 K at the sample position. Diffraction patterns obtained from the experiments were deconvoluted using the Rietveld method and quantified for lattice preferred orientation of each material under extreme conditions and during phase transformation.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Compressive Phase Contrast Tomography

When x-rays penetrate soft matter, their phase changes more rapidly than their amplitude. Interference effects visible with high brightness sources creates higher contrast, edge enhanced images. When the object is piecewise smooth (made of big blocks of a few components), such higher contrast datasets have a sparse solution. We apply basis pursuit solvers to improve SNR, remove ring artifacts, reduce the number of views and radiation dose from phase contrast datasets collected at the Hard X-Ray Micro Tomography Beamline at the Advanced Light Source. We report a GPU code for the most computationally intensive task, the gridding and inverse gridding algorithm (non uniform sampled Fourier transform).

47 OTHER INSTRUMENTATION↗