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At least 73 records · Page 4

Beam-driven ion cyclotron harmonic resonances in the terrestrial foreshock

A terrestrial upstream wave event which demonstrates multiple, ion cyclotron harmonic resonances between the interplanetary wave population and an observed proton beam is analyzed. The techniques and parameters employed in the data analysis are discussed, including the use of differential and band-pass filters. An upstream wave event demonstrating multiple harmonic waves is examined, and the instability analysis relevant to the ion beam observations thought to be responsible for that event is discussed. It is shown that an observed bi-Maxwellian ion beam is capable of generating right and left-hand polarized waves through ion cyclotron harmonic resonance.

Smith, C. W.↗

Ion Gun for In Situ Resource Identification

Identification of surface resources localized to landing sites is a critical need for future lunar exploration. Crews will need small, lightweight instrumentation that can be easily carried to identify potential resources in situ without extraction of samples for testing. This project aimed to conduct a proof-of-concept of using ion sputtering coupled with mass spectroscopy to provide in situ composition analysis of surface materials with no need to collect and/or return samples. Ion beam sputtering is a mature ground-based technique that ablates material surfaces for analysis.

ion sputtering↗

Segmented Ion Engine Plume Characteristics

Preliminary evaluation of the segmented ion thruster (SIT) ion beam characteristics was performed by measuring the two dimensional ion current density distribution at four axial locations downstream from the thruster. Current density profiles were measured with the concurrent operation of multiple ion sources. Preliminary assessments regarding symmetry of the plume, characterization of plume development as a function of axial position, and the interactions of multiple simultaneously operating ion sources were conducted. A numerical integration scheme was applied to the acquired data to determine the total beam current. A qualitative analysis of the downstream development of the ion beam was conducted. Most of the data acquired so far has been on somewhat of a trial basis and extensive testing is scheduled to resume in August 1994.

ion↗

Multi-scale structural analysis of swift heavy ion-irradiated ZrO 2 and HfO 2

The radiation-induced monoclinic-to-tetragonal phase transition in ZrO 2 and HfO 2 has been the subject of many investigations, but the transformation pathways and underlying structural mechanisms are still not well understood. In this study, microcrystalline powder samples of ZrO 2 and HfO 2 were irradiated with 946 MeV and 1470 MeV Au ions to a wide fluence range up to 3 × 10 13 ions/cm 2 . To characterize beam-induced structural modifications across all spatial length scales, complementary experimental techniques such as synchrotron X-ray diffraction and spallation neutron total scattering were used. The phase evolution of the tetragonal polymorph with increasing ion fluence is accurately described by a heterogeneous track-overlap model that incorporates both direct- and double-impact processes. These damage accumulation processes are an expression of a core-shell ion track morphology that depends on irradiation conditions and target material. Neutron pair distribution function analysis revealed that ion-beam-induced tetragonal ZrO 2 is merely a configurational average of short-range orthorhombic (Pbcn) domains stabilized by a dense network of domain walls. Furthermore, this knowledge is critical for a better understanding of how crystalline-to-crystalline phase transformations proceed at the atomic scale under extreme conditions.

Monoclinic-to-tetragonal phase transformation↗

Conjugate Multimode Heat Transfer Analysis of Cryogenic EXLO Manipulation

Abstract In this study, a conjugate radiation/conduction multimode heat transfer analysis of cryogenic focused ion beam (FIB) milling steps necessary for producing ex situ lift out specimens under cryogenic conditions (cryo-EXLO) is performed. Using finite volume for transient heat conduction and enclosure theory for radiation heat transfer, the analysis shows that as long as the specimen is attached or touching the FIB side wall trenches, the specimen will remain vitreous indefinitely, while actively cooled at liquid nitrogen (LN2) temperatures. To simulate the time needed to perform a transfer step to move the bulk sample containing the FIB-thinned specimen from the cryo-FIB to the cryo-EXLO cryostat, the LN2 temperature active cooling is turned off after steady-state conditions are reached and the specimen is monitored over time until the critical devitrification temperature is reached. Under these conditions, the sample will remain vitreous for >3 min, which is more than enough time needed to perform the cryo-transfer step from the FIB to the cryostat, which takes only ∼10 s. Cryo-transmission electron microscopy images of a manipulated cryo-EXLO yeast specimen prepared with cryo-FIB corroborates the heat transfer analysis.

Materials Science↗

Trochoidal analysis of scattered electrons in a merged electron-ion beam geometry

The method and apparatus of this invention provides a plurality of measurements indicative of the absolute cross section for excitation of an ion beam. The ion beam is merged for excitation by specific energies of electrons in an electron beam. Both beams are merged in an evacuated enclosure having a longitudinal magnetic field and a crossed uniform electric field. The ions and electrons interact over a known merged longitudinal length in a merged beam area. After collision, the electron and ion beams are demerged. Forward and backward-scattered electrons are collected and position-detected by a pair of microchannel plate arrays located at opposite ends of said longitudinal beam-merging area. A series of electron and ion primary current measurements are taken at full ion and electron beam strength. Measurements are also taken at greatly reduced beam strength to obtain a beam overlap profile.

Ara Chutjian↗

Reactive Carbide‐Based Synthesis and Microstructure of NASICON Sodium Metal All Solid‐State Electrolyte

Reactive carbide precursor-based synthesis of NASICON-type NZSP (Na 1+x Zr 2 Si x P 3-x O 12 ) solid-state electrolyte (SSE) is demonstrated, in contrast to the established oxide-based approach. Exothermic decomposition of ZrC and SiC in air homogenizes microstructure, yielding 98% compact density after conventional sintering at 1200 °C. Quantitative stereology demonstrates that significant microstructural differences are present. Compacts of carbide-derived Carb-NZSP are 98% dense with a secondary zirconium oxide (ZrO 2 ) volume fraction of 0.2% ± 0.3%, versus 93% dense and 3% ± 1% for oxide-derived baseline. For Carb-NZSP, the secondary glassy phosphate phase is agglomerated, while for baseline, it is dispersed and percolated. Electrochemical testing combined with post-mortem analysis demonstrates how microstructural control of secondary phases is critical for dendrite suppression: Carb-NZSP critical current density (CCD) is 3.1 ± 0.8 mA cm −2 at 0.1 mAh cm −2 , versus 1.0 ± 0.7 mA cm −2 at 0.1 mAh cm −2 . Cryogenic focused ion beam (cryo-FIB) analysis demonstrates that in both materials, the porous 2D sheet-like sodium metal dendrites propagate around and subsume NZSP grains, likely following a path enriched with glassy phase and with porosity. Dendrites also flow around isolated zirconia particles. Phase field simulation reveals deflection of dendrites by mechanically tough zirconia, while brittle glassy phase accelerates dendrite growth, especially when finely distributed.

36 MATERIALS SCIENCE↗

Beam characterization at NSRL for radiobiological experiments—phase 1

An experimental campaign was carried out at the NASA Space Radiation Laboratory to perform an additional, independent dosimetric characterization of the beams of protons, helium and carbon ions for radiobiological experiments. The campaign was undertaken by the request and with the support from the National Cancer Institute, U.S. In this initial phase, the goals were to obtain a first assessment of the dosimetric reproducibility of the beam control system, including analysis of spatial homogeneity and evaluation of ion beam contamination. They should facilitate the design of further experimental campaigns for beam characterization for radiobiological experiments. Measurements included reference dosimetry with comparison of in-house and external ionization chambers and electrometers, lateral-dose profile measurements in air, depth-dose profile in a water tank, evaluation of water equivalent thickness of a HDPE binary range shifter and estimation of impurities of the investigated helium-ion beam. The experiments and results are presented.

43 PARTICLE ACCELERATORS↗

Wet-chemical etching of FIB lift-out TEM lamellae for damage-free analysis of 3-D nanostructures

Reducing ion beam damage from the focused ion beam (FIB) during fabrication of cross sections is a well-known challenge for materials characterization, especially cross sectional characterization of nanostructures. To address this, a new method has been developed for cross section fabrication enabling high resolution transmission electron microscopy (TEM) analysis of 3-D nanostructures free of surrounding material and free of damage detectable by TEM analysis. Before FIB processing, nanopillars are encapsulated in a sacrificial oxide which acts as a protective layer during FIB milling. Furthermore, the cross sectional TEM lamella containing the nanopillars is then mounted and thinned with some modifications to conventional FIB sample preparation that provide stability for the lamella during the following wet-chemical dip etch. The wet-chemical etch of the TEM lamella removes the sacrificial oxide layer, freeing the nanopillars from any material that would obscure TEM imaging. Both high resolution TEM and aberration corrected scanning TEM images of Si/SiGe pillars with diameters down to 30 nm demonstrate the successful application of this approach.

3-d nanostructure analysis↗

Alumina – Stabilized SEI and CEI in Potassium Metal Batteries

Aluminum oxide (Al 2 O 3 ) nanopowder is spin-coated onto both sides of commercial polypropene separator to create artificial solid-electrolyte interphase (SEI) and artificial cathode electrolyte interface (CEI) in potassium metal batteries (KMBs). Here, this significantly enhances the stability, including of KMBs with Prussian Blue (PB) cathodes. For example, symmetric cells are stable after 1,000 cycles at 0.5 mA/cm 2 –0.5 mAh/cm 2 and 3.0 mA/cm 2 –0.5 mAh/cm 2 . Alumina modified separators promote electrolyte wetting and increase ionic conductivity (0.59 vs. 0.2 mS/cm) and transference number (0.81 vs. 0.23). Cryo-stage focused ion beam (cryo-FIB) analysis of cycled modified anode demonstrates dense and planar electrodeposits, versus unmodified baseline consisting of metal filaments (dendrites) interspersed with pores and SEI. Alumina-modified CEI also suppresses elemental Fe crossover and reduces cathode cracking. Mesoscale modeling of metal – SEI interactions captures crucial role of intrinsic heterogeneities, illustrating how artificial SEI affects reaction current distribution, conductivity and morphological stability.

25 ENERGY STORAGE↗

Controlling superconductivity of CeIrIn 5 microstructures by substrate selection

Superconductor/metal interfaces are usually fabricated in heterostructures that join these dissimilar materials. A conceptually different approach has recently exploited the strain sensitivity of heavy-fermion superconductors, selectively transforming regions of the crystal into the metallic state by strain gradients. The strain is generated by differential thermal contraction between the sample and the substrate. Here, we present an improved finite-element model that reliably predicts the superconducting transition temperature in CeIrIn 5 even in complex structures. Different substrates are employed to tailor the strain field into the desired shapes. Using this approach, both highly complex and strained as well as strain-free microstructures are fabricated to validate the model. This enables a high degree of control over the microscopic strain fields and forms the basis for more advanced structuring of superconductors as in Josephson junctions yet also finds natural use cases in any material class in which a modulation of the physical properties on a chip is desirable.

36 MATERIALS SCIENCE↗

Control of wetting and uniformity via ZrSi x formation in ceramic-to-metal joints fabricated using Ag-Zr brazes

The deposition of a 2.0 µm SiO 2 film on the alumina surface in Kovar TM /94% alumina joints enables the formation of a silicide reaction layer on the alumina during brazing with 97Ag2Zr1Cu. Additionally, the average and standard deviation of joint thickness decrease from 50 to 15 and 29 to 4 µm, respectively compared to joints without added SiO 2 . Finally, the average failure stress of these braze joints was 45 MPa, while that of similar joints without added SiO 2 was 90 MPa. Sessile drop experiments of 98Ag2Zr on SiO 2 and 99.6% Al 2 O 3 substrates show that the braze wets and spreads to 3x its original area on SiO 2 with a wetting angle near 0°, but remains the same area on 99.6% Al 2 O 3 with a wetting angle of 106.6°. Focused-ion-beam scanning electron microscopy analysis of a cross-section of the 98Ag2Zr sessile drop on the SiO 2 substrate has shown that Zr reacts with SiO 2 to form Zr oxide and silicide layers. Scanning transmission electron microscopy diffraction and energy dispersive X-ray spectroscopy analysis indicate this silicide layer contains tetragonal Zr 5 Si 4 . In conclusion, analysis shows the silicide layer enhances wetting and joint uniformity while unreacted SiO 2 embrittles the joint and degrades strength.

alumina↗

Capturing Carbonation: Understanding Kinetic Complexities through a New Era of Electron Microscopy

Cryogenic plasma focused ion beam (PFIB) electron microscopy analysis is applied to visualizing ex situ (surface industrial) and in situ (subsurface geologic) carbonation products, to advance understanding of carbonation kinetics. Ex situ carbonation is investigated using NIST fly ash standard #2689 exposed to aqueous sodium bicarbonate solutions for brief periods of time. In situ carbonation pathways are investigated using volcanic flood basalt samples from Schaef et al. (2010) exposed to aqueous CO 2 solutions by them. The fly ash reaction products at room temperature show small amounts of incipient carbonation, with calcite apparently forming via surface nucleation. Reaction products at 75° C show beginning stages of an iron carbonate phase, e.g., siderite or ankerite, common phases in subsurface carbon sequestration environments. This may suggest an alternative to calcite in carbonation low calcium-bearing fly ashes. Flood basalt carbonation reactions show distinct zonation with high calcium and calcium-magnesium bearing zones alternating with high iron-bearing zones. The calcium-magnesium zones are notable with occurrence of localized pore space. Oscillatory zoning in carbonate minerals is distinctly associated with far-from-equilibrium conditions where local chemical environments fluctuate via a coupling of reaction with transport. The high porosity zones may reflect a precursor phase (e.g., aragonite) with higher molar volume that then “ripens” to the high-Mg calcite phase-plus-porosity. These observations reveal that carbonation can proceed with evolving local chemical environments, formation and disappearance of metastable phases, and evolving reactive surface areas. Together this work shows that future application of cryo-PFIB in carbonation studies would provide advanced understanding of kinetic mechanisms for optimizing industrial-scale and commercial-scale applications.

36 MATERIALS SCIENCE↗

Higher Order Multipole Analysis of Beam Crabbing Mode at 197 MHz for Electron-Ion Collider

In the local crabbing scheme for Electron Ion Collider interaction region, beam rotation is initiated by one set of crab cavities at a high beta region with near 90 deg phase advance to the interaction point (IP), and ceased by an identical set of cavities on the symmetrically opposite side. The fundamental mode of all crab cavities is designed to apply a momentum kick to the particle bunches to complete this half cycle of rotation in the horizontal plane, meanwhile the electromagnetic (EM) field can be expanded into a series of harmonics. Despite the lowest dipole mode, higher harmonics cause instabilities during beam operation and loss of particles. We used SimTrack, which is the 6-d symplectic element-by-element tracking code developed at Brookhaven National Laboratory in 2015, to study the threshold of each higher-order harmonic multipolar mode with the criteria of maintaining a dynamic aperture of 6 σ or greater for the Hadron Storage Ring (HSR). In this paper, we showed the threshold for each higher harmonic multipole and their comparison with the multipole strength for the current crab cavity design.

43 PARTICLE ACCELERATORS↗

The source of electrostatic fluctuations in the solar-wind

Solar wind electron and ion distribution functions measured simultaneously with or close to times of intense electrostatic fluctuations are subjected to a linear Vlasov stability analysis. Although all distributions tested were found to be stable, the analysis suggests that the ion beam instability is the most likely source of the fluctuations.

Lemons, D. S.↗

A reliable workflow for improving nanoscale X-ray fluorescence tomographic analysis on nanoparticle-treated HeLa cells

Abstract Scanning X-ray fluorescence (XRF) tomography provides powerful characterization capabilities in evaluating elemental distribution and differentiating their inter- and intra-cellular interactions in a three-dimensional (3D) space. Scanning XRF tomography encounters practical challenges from the sample itself, where the range of rotation angles is limited by geometric constraints, involving sample substrates or nearby features either blocking or converging into the field of view. This study aims to develop a reliable and efficient workflow that can (1) expand the experimental window for nanoscale tomographic analysis of local areas of interest within a laterally extended specimen, and (2) bridge 3D analysis at micrometer and nanoscales on the same specimen. We demonstrate the workflow using a specimen of HeLa cells exposed to iron oxide core and titanium dioxide shell (Fe3O4/TiO2) nanocomposites. The workflow utilizes iterative and multiscale XRF data collection with intermediate sample processing by focused ion beam (FIB) sample preparation between measurements at different length scales. Initial assessment combined with precise sample manipulation via FIB allows direct removal of sample regions that are obstacles to both incident X-ray beam and outgoing XRF signals, which considerably improves the subsequent nanoscale tomography analysis. This multiscale analysis workflow has advanced bio-nanotechnology studies by providing deep insights into the interaction between nanocomposites and single cells at a subcellular level as well as statistical assessments from measuring a population of cells.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Allochthonous Addition of Meteoritic Organics to the Lunar Regolith

Preparation of lunar samples 74220,861 was discussed in detail in [3, 4]. Our analysis sequence was as follows: optical microscopy, UV fluorescence imaging, -Raman, FESEM-EDX imaging and mapping, FETEMEDX imaging and mapping of a Focused Ion Beam (FIB) extracted section, and NanoSIMs analysis. We observed fluffytextured C-rich regions of interest (ROI) on three different volcanic glass beads. Each ROI was several m2 in size and fluoresced when exposed to UV. Using FESEM/EDX, the largest ROI measured ~36 m and was located on an edge of a plateau located on the uppermost surface of the bead. The ROI was covered on one edge by a siliceous filament emanating from the plateau surface indicating it was attached to the bead while on the Moon. EDX mapping of the ROI shows it is composed primarily of heterogeneously distributed C. Embedded with the carbonaceous phase are localized concentrations of Si, Fe, Al and Ti indicating the presence of glass and/or minerals grains. -Raman showed strong D- and G-bands and their associated second order bands; intensity and location of these bands indicates the carbonaceous matter is structurally disorganized. A TEM thin section was extracted from the surface of a glass bead using FIB microscopy. High resolution TEM imaging and selected area electron diffraction demonstrate the carbonaceous layer to be amorphous; it lacked any long or short range order characteristic of micro- or nanocrystalline graphite. Additionally TEM imaging also revealed the presence of submicron mineral grains, typically < 50 nm in size, dispersed within the carbonaceous layer. NanoSIMs data will be presented and discussed at the meeting. Given the noted similarities between the carbonaceous matter present on 74220 glass beads and meteoritic kerogen, we suggest the allochthonous addition of meteoritic organics as the most probable source for the C-rich ROIs.

Thomas-Keprta, K. L.↗