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At least 55 records · Page 3

Investigation and simulation of metallic spherules from lunar soils

The microstructure and chemical composition of metallic spherules from the lunar soil were studied by optical, electron-probe, and scanning-electron-microscope techniques. Metallic spherules produced experimentally were compared to the lunar spherules with respect to structure, chemistry, and cooling rates. The structure of the lunar spherules indicates an origin by solidification of molten globules of metal. The spherules are probably produced from both lunar and meteoric sources, the major source being the metal phase present in lunar rocks and soil.

Blau, P. J.↗

Electron microscopy study of the iron meteorite Santa Catharina

A characterization of the microstructural features of Santa Catharina (SC) from the millimeter to submicron scale is presented. The same specimen was examined using an optical microscope, a scanning electron microscope, an electron probe microanalyzer, and an analytical electron microscope. Findings include the fact that SC metal nodules may have different bulk Ni values, leading to different microstructures upon cooling; that SC USNM 6293 is the less corroded sample, as tetrataenite exists as less than 10 nm ordered domains throughout the entire fcc matrix (it is noted that this structure is the same as that of the Twin City meteorite and identical to clear taenite II in the retained taenite regions of the octahedrites); that SC USNM 3043 has a more complicated microstructure due to corrosion; and that the low Ni phase of the cloudy zone was selectively corroded in some areas and formed the dark regions, indicating that the SC meteorite corrosion process was electrochemical in nature and may involve Cl-containing akaganeite.

Zhang, J.↗

Textural variations and impact history of the Millbillillie eucrite

We have investigated 10 new specimens of the Millbillillie eucrite to study its textures and mineral compositions by electron probe microanalyser and scanning electron microscope. Although originally described as having fine-grained texture, the new specimens show diversity of texture. The compositions (Mg/Fe ratios) of the host pigeonites and augite lamellae are homogeneous, respectively, in spite of the textural variation. In addition to their chemical homogeneity, pyroxenes in coarse and fine-grained clasts are partly inverted to orthopyroxene. Chemical zoning of plagioclase during crystal growth is preserved. This eucrite includes areas of granulitic breccias and impact melts. Large scale textures show a subparallel layering suggesting incomplete mixing and deposition of impact melt and lithic fragments. An Ar-39-Ar-40 age determination for a coarse-grained clast indicates a strong degassing event at 3.55 +/- 0.02 Ga. We conclude that Millbillillie is among the most equilibriated eucrites produced by thermal annealing after impact brecciation. According to the classificcation of impact breccias, Millbillillie can be classified as a mixture of granulitic breccias and impact melts. The last significant thermal event is characterized by network-like glassy veins that run through clasts and matrices. Consideration of textual observations and requirements for Ar-degassing suggests that the Ar-39-Ar-40 age could in principle date either the earlier brecciation and annealing event or the event which produced the veins.

Yamaguchi, Akira↗

Carbon Nanofibers Synthesized on Selective Substrates for Nonvolatile Memory and 3D Electronics

A plasma-enhanced chemical vapor deposition (PECVD) growth technique has been developed where the choice of starting substrate was found to influence the electrical characteristics of the resulting carbon nanofiber (CNF) tubes. It has been determined that, if the tubes are grown on refractory metallic nitride substrates, then the resulting tubes formed with dc PECVD are also electrically conducting. Individual CNFs were formed by first patterning Ni catalyst islands using ebeam evaporation and liftoff. The CNFs were then synthesized using dc PECVD with C2H2:NH3 = [1:4] at 5 Torr and 700 C, and approximately equal to 200-W plasma power. Tubes were grown directly on degenerately doped silicon <100> substrates with resistivity rho approximately equal to 1-5 meterohm-centimeter, as well as NbTiN. The approximately equal to 200-nanometer thick refractory NbTiN deposited using magnetron sputtering had rho approximately equal to 113 microohm-centimeter and was also chemically compatible with CNF synthesis. The sample was then mounted on a 45 beveled Al holder, and placed inside a SEM (scanning electron microscope). A nanomanipulator probe stage was placed inside the SEM equipped with an electrical feed-through, where tungsten probes were used to make two-terminal electrical measurements with an HP 4156C parameter analyzer. The positive terminal nanoprobe was mechanically manipulated to physically contact an individual CNF grown directly on NbTiN as shown by the SEM image in the inset of figure (a), while the negative terminal was grounded to the substrate. This revealed the tube was electrically conductive, although measureable currents could not be detected until approximately equal to 6 V, after which point current increased sharply until compliance (approximately equal to 50 nA) was reached at approximately equal to 9.5 V. A native oxide on the tungsten probe tips may contribute to a tunnel barrier, which could be the reason for the suppressed transport at low biases. Currents up to approximately 100 nA could be cycled, which are likely to propagate via the tube surface, or sidewalls, rather than the body, which is shown by the I-V in figure (a). Electrical conduction via the sidewalls is a necessity for dc NEMS (nanoelectromechanical system) applications, more so than for the field emission applications of such tubes. During the tests, high conductivity was expected, because both probes were shorted to the substrate, as shown by curve 1 in the I-V characteristic in figure (b). When a tube grown on NbTiN was probed, the response was similar to the approximately equal to 100 nA and is represented by curve 2 in figure (b), which could be cycled and propagated via the tube surface or the sidewalls. However, no measureable currents for the tube grown directly on Si were observed as shown by curve 3 in figure (b), even after testing over a range of samples. This could arise from a dielectric coating on the sidewalls for tubes on Si. As a result of the directional nature of ion bombardment during dc PECVD, Si from the substrate is likely re-sputtered and possibly coats the sidewalls.

Kaul, Anupama B.↗

Quantitative Specifications to Avoid Degradation during E-Beam and Induced Current Microscopy of Halide Perovskite Devices

Degradation due to electron beam exposure has posed a challenge in the use of electron microscopy to probe halide perovskite materials and devices. Herein, the interaction between the electron beam and the perovskite across acceleration voltages and at low probe currents is investigated in a scanning electron microscope (SEM) by monitoring the electron-beaminduced current (EBIC) response in perovskite solar cells in a planview configuration. SEM probe conditions are identified where dozens of repeated scans over a single region of the perovskite solar cell induce minimal electronic degradation. Overall, the induced current response of the perovskite device is found to strongly depend upon the beam condition: rapid decay occurs at high beam powers, the current activates at the lowest beam powers, and a newfound quasi-steady response is revealed at intermediate beam conditions. A quantitative window for the successful conduction of e-beam studies with minimal electronic degradation is revealed by evaluating induced current response over a wide range of perovskite devices, which invites broader use of SEM-based characterization techniques, including EBIC, as powerful techniques for correlative microscopy investigations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Reconstruction and uncertainty quantification of lattice Hamiltonian model parameters from observations of microscopic degrees of freedom

The emergence of scanning probe and electron beam imaging techniques has allowed quantitative studies of atomic structure and minute details of electronic and vibrational structure on the level of individual atomic units. These microscopic descriptors, in turn, can be associated with local symmetry breaking phenomena, representing the stochastic manifestation of the underpinning generative physical model. In this work, we explore the reconstruction of exchange integrals in the Hamiltonian for a lattice model with two competing interactions from observations of microscopic degrees of freedom and establish the uncertainties and reliability of such analysis in a broad parameter-temperature space. In contrast to other approaches, we specifically specify a loss function inherent to thermodynamic systems and utilize it to estimate uncertainty in simulated realizations of different models. As an ancillary task, we develop a machine learning approach based on histogram clustering to predict phase diagrams efficiently using a reduced descriptor space. We further demonstrate that reconstruction is possible well above the phase transition and in the regions of parameter space when the macroscopic ground state of the system is poorly defined due to frustrated interactions. This suggests that this approach can be applied to the traditionally complex problems of condensed matter physics such as ferroelectric relaxors and morphotropic phase boundary systems, spin and cluster glasses, and quantum systems once the local descriptors linked to the relevant physical behaviors are known.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

SEM probe of IC radiation sensitivity

Scanning Electron Microscope (SEM) used to irradiate single integrated circuit (IC) subcomponent to test for radiation sensitivity can localize area of IC less than .03 by .03 mm for determination of exact location of radiation sensitive section.

Gauthier, M. K.↗

Sculpting the Plasmonic Responses of Nanoparticles by Directed Electron Beam Irradiation

Spatial confinement of matter in functional nanostructures has propelled these systems to the forefront of nanoscience, both as a playground for exotic physics and quantum phenomena and in multiple applications including plasmonics, optoelectronics, and sensing. In parallel, the emergence of monochromated electron energy loss spectroscopy (EELS) has enabled exploration of local nanoplasmonic functionalities within single nanoparticles and the collective response of nanoparticle assemblies, providing deep insight into associated mechanisms. However, modern synthesis processes for plasmonic nanostructures are often limited in the types of accessible geometry, and materials and are limited to spatial precisions on the order of tens of nm, precluding the direct exploration of critical aspects of the structure-property relationships. Here, the atomic-sized probe of the scanning transmission electron microscope is used to perform precise sculpting and design nanoparticle configurations. Using low-loss EELS, dynamic analyses of the evolution of the plasmonic response are provided. It is shown that within self-assembled systems of nanoparticles, individual nanoparticles can be selectively removed, reshaped, or patterned with nanometer-level resolution, effectively modifying the plasmonic response in both space and energy. This process significantly increases the scope for design possibilities and presents opportunities for unique structure development, which are ultimately the key for nanophotonic design.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Integrated material-surface analyzer

These 10 surface-analysis tests can be run without breaking vacuum: secondary-ion mass spectroscopy, ion-scattering spectroscopy, electron-stimulated desorption, residual-gas analysis, auger electron spectroscopy, x-ray photoelectron spectroscopy, ultraviolet photoelectron spectroscopy, characteristic-electron energy-loss spectroscopy, scanning electron microscope, scanning low-energy electron probe. Quadruple mass spectrometer, used in first 4 tests, serves as electron transfer lens in last 6 tests.

Grunthaner, F. J.↗

A new Antarctic meteorite with chromite, orthopyroxene and metal with reference to a formation model of S asteroids

Mineralogy of a unique meteorite from Antarctica, EET84302 and the related primitive achondrites, was studied to gain better understanding on relationship between S asteroids and this meteorite group. EET84302 consists of metal-rich (M) region with metal filling interstices of silicate grains of orthopyroxene (Opx), olivine Fa8, plagioclase An24, and augite (Aug), chromite-rich (C) region with major chromite and Opx, and silicate-rich (S) region with mainly Opx. This is the first example of chromite-rich achondrite. Distribution of three areas (C, M, S) are in line with a proposed model of primitive achondrites and S asteroids. Since reflectance spectra of some members of primitive achondrites combined with those of iron meteorites, resemble those of the S asteroids, there is an expectation that S asteroids are modified products of chondrites. The trends of the variations in their mineral assemblages are in line with those of the S asteroids. Hiroi proposed a stony-iron model of S asteroids, which assumes that a few domains of various primitive achondrites are embedded in iron matrix. Polished thin sections (PTS) of EET84302,19 and ALH81187,16 were supplied from Meteorite Working Group (MWG). A previously studied PTS of EET84302 was similar in both texture and mineralogy to silicate inclusions in some iron meteorites. PTS EET84302,19 was studied by electron probe microanalyzer (EPMA) and scanning electron microscope (SEM). The reflectance spectra of EET84302 showed a weathering problem and was not used to match with those of S asteroids.

Takeda, Hiroshi↗

Tunneling magnetic force microscopy

We have developed a powerful new tool for studying the magnetic patterns on magnetic recording media. This was accomplished by modifying a conventional scanning tunneling microscope. The fine-wire probe that is used to image surface topography was replaced with a flexible magnetic probe. Images obtained with these probes reveal both the surface topography and the magnetic structure. We have made a thorough theoretical analysis of the interaction between the probe and the magnetic fields emanating from a typical recorded surface. Quantitative data about the constituent magnetic fields can then be obtained. We have employed these techniques in studies of two of the most important issues of magnetic record: data overwrite and maximizing data-density. These studies have shown: (1) overwritten data can be retrieved under certain conditions; and (2) improvements in data-density will require new magnetic materials. In the course of these studies we have developed new techniques to analyze magnetic fields of recorded media. These studies are both theoretical and experimental and combined with the use of our magnetic force scanning tunneling microscope should lead to further breakthroughs in the field of magnetic recording.

Burke, Edward R.↗

Resistivity of Surface Steps in Bulk-Insulating Topological Insulators

Electron transport in topological insulators usually involves both topologically protected surface states and trivial electronic states in the bulk material. The surface transport is particularly interesting; however, it is also susceptible to atomic defects on the surfaces, such as vacancies, impurities, and step edges. Experimental determination of scattering effects of these surface defects requires both nanoscale spatial resolution and the ability to decipher surface transport from bulk transport. Here we directly measure the resistivity of individual surface steps in the surface dominating transport process of topological insulator Bi 2 Te 2 Se. A variable probe-spacing transport spectroscopy with a multiprobe scanning tunneling microscope is used to differentiate the surface conductance from bulk conductance, allowing the identification of a surface dominant transport regime. The technique also reveals a deviation from ideal 2D transport at atomic steps. Then, a multi-probe scanning tunneling potentiometry is employed to visualize the electrochemical potentials across individual step edges. A quantitative analysis of the potential distributions enables us to acquire a resistivity of 0.530 mΩ · cm for the one quintuple-layer atomic step. The result indicates that atomic defects, despite preserving the time-reversal symmetry, can still significantly affect the transport in topological insulators.

36 MATERIALS SCIENCE↗

Consequences and Control of Multiscale Order/Disorder in Chiral Magnetic Textures

Transition metal intercalated transition metal dichalcogenides (TMDs) are promising platforms for next-generation spintronic devices based on their wide range of electronic and magnetic phases, which can be tuned by varying the host lattice or intercalant’s identity, stoichiometry, or spatial order. Some of these compounds host a chiral magnetic phase in which the helical winding of magnetic moments propagates along a high-symmetry crystalline axis. Previous studies have demonstrated that variation in intercalant concentrations can have a dramatic effect on the formation of chiral domains and ensemble magnetic properties. However, a systematic and comprehensive study of how atomic-scale order and disorder impact these chiral magnetic textures is so far lacking. Here, we leverage a combination of imaging modes in the (scanning) transmission electron microscope (S/TEM) to directly probe (dis)order across multiple length scales and show how subtle changes in the atomic lattice can tune the mesoscale spin textures and bulk magnetic response in Cr 1/3 NbS 2 , with direct implications for the fundamental understanding and technological implementation of such compounds.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Space-Time Quantum Information from the Entangled States of Magnetic Molecule (STI Product)

This collaborative project combines synthesis, measurement, and theory by three faculty members at the Eddleman Quantum Institute of UC Irvine to effectively investigate the quantum properties of molecules in the space, time, and frequency domains. Through synthetic chemistry, molecules are tailored for their magnetic and coherent properties. By combining femtosecond (fs) terahertz (THz) light and a continuous wave (cw) THz laser with a low temperature scanning tunneling microscope (STM), quantum phenomena are probed with simultaneous femtosecond temporal and atomic-scale spatial resolution. In particular, the invention of the quantum superposition microscope (QSM) advances quantum sensing for enhanced spectroscopy and imaging capabilities. Coupling theory to the experimental efforts offers a deeper understanding and predictive power for the molecular systems. The phenomena of superposition, entanglement, and coherence is central to quantum information science and can be realized in qubit states. Many systems can be modeled by a double-well potential in which two levels are formed in the two lowest energy states interacting with the environment and external radiation. In focusing on molecules as two-level systems, the underlying expectation is that their tunable composition and structure allows an effective parameter space to optimize their use as qubits for quantum sensing and computing. The THz radiation induces the superposition between the two states, appearing as temporal oscillations that damp in amplitude. Enhanced spectroscopy and imaging in the time and frequency domains is achieved through the extreme sensitivity of the frequency and damping of coherence of two-level systems to its environment. A single hydrogen molecule trapped in the STM tunneling gap experiences a double-well potential and absorption of THz femtosecond pulses of light creates the superposition of its two levels, appearing as damped oscillations in the light induced direct current (DC). The oscillation frequency depends sensitively on the electric field distribution of the copper nitride (Cu 2 N) surface, through the Stark effect, and associated with the different charge distributions at the copper and nitrogen sites and in between. This QSM can resolve variation in the surface electric field with 0.02 nanometer resolution. In addition, the single hydrogen molecule entaes with nearby hydrogen molecules as seen in the avoided level crossings of energy (oscillation frequency) versus the voltage across the tunneling gap. Thus, the first application of the QSM senses and images the surface electric field at the atomic scale. Results from this project advance fundamental understanding of quantum phenomena, develop novel synthesis, measurement, and theory, provide the knowledge foundation for molecule-based qubits and sensing that enable the development of the QSM and emergent technologies. This project trained researchers in quantum information science, extended knowledge in classrooms, and outreached to the community.

47 OTHER INSTRUMENTATION↗

Carbon Nanotube Scanning Probe for Surface Profiling of DUV and 193 nm Photoresist Pattern

The continual scaling down of semiconductors to 100 nm and below necessitates a characterization technique to resolve high aspect ratio features in the nanoscale regime. This paper reports the use of atomic force microscope coupled with high aspect ratio multi-walled carbon nanotube scanning probe tip for the purpose of imaging surface profile of photoresists. Multi-walled carbon nanotube tips used in this work are 5-10 nm in diameter and about a micron long. Their exceptional mechanical strength and ability to reversibly buckle enable to resolve steep, deep nanometer-scale features. Images of photoresist patterns generated by 257 nm interference lithography as well as 193 nm lithography are presented to demonstrate multi-walled carbon nanotube scanning probe tip for applications in metrology.

Nguyen, Cattien V.↗

Advanced Characterization of Fuel-cladding Chemical Interaction between U-10Zr Fuel and HT9 Cladding Tested in Fast Flux Test Facility

Fuel cladding chemical interaction (FCCI) can greatly accelerate the cladding failure. However, due to the limited space in a fuel cladding assembly, it is historically challenging to gain an mechanistical understanding of the formation mechanism of FCCI and its influence on fuel and cladding performance. With the imminent need to qualify U-10Zr based metallic fuel cladded by HT-9 for advanced reactors demonstration project, it is of vital importance to use advanced characterization method to study FCCI in a unprecedent detailed manner and gain better mechanism understanding of FCCI. Mechanistic Fuel Failure (MFF) series of prototypic fuel elements irradiated in FFTF [1, 2] provides the best samples to study FCCI since the MFF-series assemblies had an axial fuel height the same as proposed length by industry partners. Jason et al. [3] has performed preliminary post-irradiation examination on a MFF fuel pin sample, which was extracted from the HT9 cladded U-10at.%Zr MFF-3 pin MFF-3 pin (#193045) at an axial location of X/L = 0.98. This sample has a peak burnup of 5.7 at.% and peak inner cladding temperature (PICT) of around 615 °C during in-core testing. Scanning electron microscope examination has identified visible FCCI region on more than half of the HT9 circumference [3]. The most striking feature are grain boundary attacking by apparently lanthanides (Lns) rich phase. However, SEM cannot provide accurate assessment of phase and concentration of grain boundary phases and prevented a better understanding of the formation mechanism of such attach. This study, by pairing transmission electron microscope (TEM) characterization and atom probe tomography (APT) techniques with in-situ micro-tensile testing in scanning electron microscope (SEM), aims at gaining in-depth understanding on the formed FCCI region. The identified FCCI region roughly consists of multilayers as illustrated in Figure 1 (c). The main findings are: (1) layer-B shows observable lanthanides (Lns) infiltration along grain boundaries and mechanical softening due to FCCI- and irradiation-induced microstructural and microchemistry changes, particularly the recovery of martensitic lath structure and dissolution of pre-existing M23C6 together with the formation of coarsened Laves phases, (Fe, Cr)2(Mo, W); (2) layer-C is Fe depleted but Lns significantly enriched, becoming very brittle; (3) layer-D is mainly composed of UFe2 and Lns; (4) three FCCI-induced intermetallic U-Fe-Zr phases, ? (Fe0.5Zr0.32U0.18), e (Fe0.3Zr0.4U0.3), ? (Fe0.06Zr0.23U0.71), were identified near layer-E; (5) the ? (Fe0.5Zr0.32U0.18) phase was characterized to be a face centered cubic (FCC) crystal structure. These results will help to better understanding the governing mechanism of FCCI and facilitating the development of theoretical model for assessing the performance of metallic fuel and cladding integrity.

36 MATERIALS SCIENCE↗

Automated Weld Characterization Using the Thermoelectric Method

The effective assessment of the integrity of welds is a complicated NDE problem that continues to be a challenge. To be able to completely characterize a weld, detailed knowledge of its tensile strength, ductility, hardness, microstructure, macrostructure, and chemical composition is needed. NDE techniques which can provide information on any of these features are extremely important. In this paper, we examine a seldom used approach based on the thermoelectric (TE) effect for characterizing welds and their associated heat affected zone (HAZ). The thermoelectric method monitors the thermoelectric power which is sensitive to small changes in the kinetics of the conduction electrons near the Fermi surface that can be caused by changes in the local microstructure. The technique has been applied to metal sorting, quality testing, flaw detection, thickness gauging of layers, and microscopic structural analysis. To demonstrate the effectiveness of the technique for characterizing welds, a series of tungsten-inert-gas welded Inconel-718 samples were scanned with a computer controlled TE probe. The samples were then analyzed using a scanning electron microscope and Rockwell hardness tests to characterize the weld and the associated HAZ. We then correlated the results with the TE measurements to provide quantitative information on the size of the HAZ and the degree of hardness of the material in the weld region. This provides potentially valuable information on the strength and fatigue life of the weld. We begin the paper by providing a brief review of the TE technique and then highlight some of the factors that can effect the measurements. Next, we provide an overview of the experimental procedure and discuss the results. Finally, we summarize our findings and consider areas for future research.

Fulton, J. P.↗