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At least 199 records · Page 11

Applying shot boundary detection for automated crystal growth analysis during in situ transmission electron microscope experiments

In-situ (scanning) transmission electron microscopy (S/TEM) is being developed for numerous applications in the study of nucleation and growth under electrochemical driving forces. For this type of experiment, one of the key parameters is to identify when nucleation initiates. Typically the process of identifying the moment that crystals begin to form is a manual process requiring the user to perform an observation and respond accordingly (adjust focus, magnification, translate the stage etc.). However, as the speed of the cameras being used to perform these observations increases, the ability of a user to “catch” the important initial stage of nucleation decreases (there is more information that is available in the first few milliseconds of the process). Here we show that video shot boundary detection (SBD) can automatically detect frames where a change in the image occurs. We show that this method can be applied to quickly and accurately identify points of change during crystal growth. This technique allows for automated segmentation of a digital stream for further analysis and the assignment of arbitrary time stamps for the initiation of processes that are independent of the user’s ability to observe and react.

36 MATERIALS SCIENCE↗

Analysis of runaway electron driven whistler wave instability experiments

Data acquired on the DIII-D tokamak were analyzed. The data are from experiments that were conducted to study an instability that is driven unstable by intense populations of electrons with MeV energies that are known as runaway electrons. The instability is a type of plasma wave called a whistler wave that occurs at frequencies above the ion cyclotron frequency but well below the electron cyclotron frequency. The waves were measured by magnetic fluctuation coils that are embedded in the DIII-D vacuum vessel wall. After upgrades to this diagnostic were completed, new experiments were conducted on July 13, 2020 in order to measure the toroidal mode number of the whistler waves and to extend the frequency of the detected waves. Through the use of mixers, instability between 600-700 MHz was detected. (The initial experiments only measured up to 200 MHz.) Analysis of the data was led by Hari Choudhury, a PhD student at Columbia University. Mr. Choudhury has submitted two papers for publication that include contributions by UC Irvine (UCI) Professor Heidbrink and his graduated PhD student Genevieve DeGrandchamp: “Detailed Characterization of Runaway Electron Driven Whistler Waves in Low-Density DIII-D Discharges” and “First Demonstration of Resonant Pitch-Angle Scattering of Relativistic Electrons by Externally-Launched Helicon Waves.” The first paper, which has been submitted to Physics of Plasmas, has significant contributions to both the data and the interpretation by UCI scientists. In contrast, UCI contributions to the second paper, which has been submitted to Physical Review Letters, are relatively minor.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Electromagnetic Analysis of ITER Electron Cyclotron Emission Model

The ITER electron cyclotron emission (ECE) diagnostic system is located at diagnostics shielding module 2 (DSM2), equatorial port 9 (EP9), to measure electron temperature profile and electron temperature fluctuations, and also assess nonthermal electron distributions via the oblique view. Therefore, ECE has both radial and oblique views with two hot sources for calibration and two couples of mirrors for two different optical views. It shall receive that the large electromagnetic (EM) loads up to 100-MN/m3 force density due to the eddy currents on the copper mirrors generated by the short transient plasma disruption. The simplified EM analysis model using magnetic field ( B ) data and flux variations (dB/dt) method based on the worst case of plasma disruption, MD_DW_EXP16MS_CATIII, has been developed to calculate the force and moments for each ECE component and support structure for EP9 DSM2 Bay2 and Bay3. The B and dB/dt methods use the constant B and dB/dt assumed for each local bay space, but the real B and dB/dt are basically varied along the radial direction of each bay. The complex global model with the local ECE components and support structure using Maxwell transient has been developed to do EM analysis to compare the results of the B and dB/dt models. The volumetric EM force density of the whole ECE components and support structure can be used for the subsequent structural analysis. In conclusion, combined with the thermal and nuclear loads and seismic and initial loads, the ECE integration analysis can be finalized for the operation case.

Fang, J. [Princeton Plasma Physics Laboratory (PPP↗

Inclusive and exclusive electron scattering data analysis from Jefferson Lab experiment E12-14-012

Since the first observations of neutrino oscillation, neutrino experiments have come a long way toward precise measurements of the neutrino oscillation parameters, but some obstacles still remain. The next generation of oscillation experiments, including the Deep Underground Neutrino Experiment (DUNE), will be using the Liquid Argon Time Projection Chambers (LArTPCs) with natural argon as the neutrino target material. A precise model of the neutrino cross section on argon does not exist, which is a source of significant uncertainty in such experiments. The E12-14-012 experiment at Jefferson Lab seeks to help remedy this via electron scattering measurements on argon and titanium targets. The experiment collected both inclusive (e,e') and exclusive (e,e'p) data at a wide range of kinematics with the intent to measure the electron-nucleus cross section and thus derive a spectral function for argon that can be used with neutrino experiments. The use of titanium in this experiment stems from the equivalent shell structure that its protons share with the neutrons in argon, which will be crucial in oscillation experiments but cannot be measured directly in electron scattering. This thesis collects several papers which present results from the E12-14-012 experiment. These results include the inclusive (e,e') cross sections for carbon, titanium, argon, and aluminum at a beam energy of 2.22 GeV and a scattering angle of 15.54 deg with uncertainty of less than 5%. Also included are the first results of the exclusive (e,e'p) cross section on argon and titanium.

Murphy, Matthew D.↗

In Situ Analysis of Electron-Induced Chemical Transformations in Vapor-Phase-Synthesized Al-Based Inorganic–Organic Hybrid Thin Films for EUV Resist Platform

The rapid advancement and stringent requirements of extreme ultraviolet (EUV) lithography technology necessitate the development of advanced photoresist systems for next-generation microelectronics. Recent studies have demonstrated that inorganic-based hybrid photoresists offer notable improvements in EUV sensitivity, etch resistance, and greater insusceptibility to pattern collapse compared to their purely organic counterparts. However, variations in the synthesis/coating approaches and chemistry of inorganic–organic photoresists can result in distinct exposure mechanisms. In this work, an Al-based hybrid thin film resist system synthesized via molecular (atomic) layer deposition (MLD or MALD) is explored, focusing on its electron-beam and EUV patterning mechanisms. The Al-based hybrid thin films are deposited using trimethylaluminum (TMA) and the organic precursor hydroquinone, exhibiting a saturated growth rate within the temperature range of 150–200°C. In diluted tetramethylammonium hydroxide (TMAH)-based developer solutions, the electron-irradiated Al-based hybrid thin film system behaves as a negative tone resist, achieving a sensitivity of 10.4 mC/cm 2 at 0.1 kV electron beam lithography (EBL). Chemical changes induced by electron exposure are also analyzed in this study using X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and a unique infrared spectroscopy setup, revealing the potential cross-linking pathways. To further correlate the electron-induced chemical transformations with those mediated by EUV irradiations, a combination of X-ray photoemission electron microscopy/low-energy electron microscopy (XPEEM/LEEM) system is also employed. In conclusion, this study provides critical insights into the mechanisms underlying solubility switching and contributes to the design of advanced resist materials for EUV lithography.

36 MATERIALS SCIENCE↗

An Electron Backscatter Diffraction Analysis of Grain Boundary Initiated Discontinuous Precipitation in U-10Mo

The effect of varied thermomechanical processing on discontinuous precipitation (DP) in U-10Mo was investigated, with specific emphasis on understanding the role of grain boundary misorientation in DP. Varied prior homogenization heat treatment and thermomechanical processing resulted in differences in both the fraction of DP and the colony width, and was attributed to variations in the grain boundary misorientation distribution. Regardless of the degree of DP-based transformation, extensive growth of DP colonies was dominant on 30°–45° misorientation boundaries. Interestingly, misorientation histograms of the deformed and annealed specimens suggest the processing steps involved may have inhibited DP colony growth along a small fraction of these high angle boundaries. Large-area electron backscatter diffraction montages coupled with high resolution mapping suggest symmetric {110}-type interfaces may be important considerations for mitigating extensive DP growth in this alloy system.

Discontinuous Precipitation, Uranium, Electron Bac↗

Electromagnetic Analysis of ITER Electron Cyclotron Emission Components and Support Structures for the Preliminary Design Review

The ITER electron cyclotron emission (ECE) diagnostic system is located at Design Shield Module (DSM) 2, Equatorial Port (EP) 9 to measure electron temperature profile and electron temperature fluctuations and also to assess nonthermal electron distributions via the oblique view. Therefore, ECE has both radial and oblique views with two couples of mirrors for two different optical views. This ECE diagnostic system shall be exposed to significant power due to unabsorbed electron cyclotron heating power in the plasma. It shall also receive large electromagnetic (EM) loads up to 100 MN/m 3 force density due to the eddy currents generated by the short 16-ms transient plasma disruption. The global EM models of EP12 and EP11 with the worst case of plasma disruption Major Disruption Downward Exponential 16 ms Category III (MD_DW_EXP16MS_CATIII) have been provided by ITER. However, the support structure for these critical components, including four mirrors, is still under the design and development phase, especially during the period of preliminary design reviews (PDRs). For those small in-vessel components that are not modeled explicitly for the PDRs, we can extract the magnetic field (B) data and flux variations (dB/dt) at those locations from the global model and then use the B and dB/dt method to calculate the eddy currents, EM forces, and torques on those components in the local submodels. In conclusion, this paper will present the detailed PDR EM analysis results of the ECE components and support structures.

Electromagnetic↗

Acquisition of a High Resolution Field Emission Scanning Electron Microscope for the Analysis of Returned Samples

This grant furnished funds to purchase a state-of-the-art scanning electron microscope (SEM) to support our analytical facilities for extraterrestrial samples. After evaluating several instruments, we purchased a JEOL 6500F thermal field emission SEM with the following analytical accessories: EDAX energy-dispersive x-ray analysis system with fully automated control of instrument and sample stage; EDAX LEXS wavelength-dispersive x-ray spectrometer for high sensitivity light-element analysis; EDAX/TSL electron backscatter diffraction (EBSD) system with software for phase identification and crystal orientation mapping; Robinson backscatter electron detector; and an in situ micro-manipulator (Kleindiek). The total price was $550,000 (with $150,000 of the purchase supported by Carnegie institution matching funds). The microscope was delivered in October 2002, and most of the analytical accessories were installed by January 2003. With the exception of the wavelength spectrometer (which has been undergoing design changes) everything is working well and the SEM is in routine use in our laboratory.

Nittler, Larry R.↗

Electrode erosion in steady-state electric propulsion engines

The anode and cathode of a 30 kW class arcjet engine were sectioned and analyzed. This arcjet was operated for a total time of 573 hr at power levels between 25 and 30 kW with ammonia at flow rates of 0.25 and 0.27 gm/s. The accumulated run time was sufficient to clearly establish erosion patterns and their causes. The type of electron emission from various parts of the cathode surface was made clear by scanning electron microscope analysis. A scanning electron microscope was used to study recrystallization on the hot anode surface. These electrodes were made of 2 percent thoriated tungsten and the surface thorium content and gradient perpendicular to the surfaces was determined by quantitative microprobe analysis. The results of this material analysis on the electrodes and recommendations for improving electrode operational life time are presented.

Pivirotto, Thomas J.↗

Precision Oxygen Isotope Measurements of Two C-Rich Hydrated Interplanetary Dust Particles

Introduction: Chondritic-smooth IDPs (Interplanetary Dust Particles) are low porosity objects whose mineralogy is dominated by aqueous alteration products such as Mg-rich phyllosilicates (smectite and serpentine group) and Mg-Fe carbonate minerals. Their hydrated mineralogy combined with low atmospheric entry velocities have been used to infer an origin largely from asteroidal sources. Spectroscopic studies show that the types and abundance of organic matter in CS IDPs is similar to that in CP IDPs. Although CS IDPs show broad similarities to primitive carbonaceous chondrites, only a few particles have been directly linked to specific meteorite groups such as CM and CI chondrites based on the presence of diagnostic minerals. Many CS IDPs however, have carbon contents that greatly exceed that of known meteorite groups suggesting that they either may derive from comets or represent samples of more primitive parent bodies than do meteorites. It is now recognized that many large, dark primitive asteroids in the outer main belt, as well as some trans-Neptunian objects, show spectroscopic evidence for aqueous alteration products on their surfaces. Some CS IDPs exhibit large bulk D enrichments similar to those observed in the cometary CP IDPs. While hydrated minerals in comets have not been unambiguously identified to date, the presence of the smectite group mineral nontronite has been inferred from infrared spectra obtained from the ejecta from comet 9P/Tempel 1 during the Deep Impact mission. Recent observations of low temperature sulfide minerals in Stardust mission samples suggest that limited aqueous activity occurred on comet Wild-2. All of these observations, taken together, suggest that the high-carbon hydrated IDPs are abundant and important samples of primitive solar system objects not represented in meteorite collections. Oxygen isotopic compositions of chondrites reflect mixing between a 16O-rich reservoir and a 17O,18O-rich reservoir produced via mass-independent fractionation. The composition of the 16O-rich reservoir is well constrained but material representing the 17O,18O-rich end-member is rare. Self-shielding models predict that cometary water, presumed to represent this reservoir, should be enriched in 17O and 18O by greater than 200 per mille. The high-carbon hydrated IDPs may be among the best materials available to search for preserved "cometary" H2O signatures. In order to better understand the origin and evolution of these particles, we have obtained 10 hydrated interplanetary dust particles for coordinated mineralogical, isotopic and organic analyses. We have previously reported the results of mineralogical and O isotopic measurements of two hydrated IDPs; here we present results of O isotopic measurements of three additional IDPs. Samples and Methods: Three interplanetary dust particles (L2079C35, L2083D46 and L2083E46) were embedded in S and partially ultramicrotomed into approximately 70 nanometer sections for analysis via transmission electron microscopy (TEM). The remainders of the unsliced particles were removed from S and pressed into high purity Au foil that was cleaned with HF acid and annealed at 800 degrees Centigrade. The pressed IDPs were analyzed via electron microprobe analysis (EPMA) for quantitative bulk chemical analysis. After EPMA analysis, the IDPs were subjected to precision O isotope analysis with the UCLA Cameca IMS-1270 ion probe. A 20 kiloelectronvolt, 0.5 nanoangstrom Cs+ primary beam of approximately 15 micrometers diameter was used for each measurement. Small particles of San Carlos olivine and Burma spinel were pressed into the Au foil for use as standards to correct for instrumental mass fractionation. The detection system was configured for multicollection, with 16O measured on a Faraday cup, and 17O and 18O measured on electron multipliers (EMs). Individual analyses consisted of 15 cycles of 10 seconds per cycle. Additionally, two microtome thin sections were measured for H isotopic compositions with the JSC NanoSIMS 50L ion probe. An 8 picoangstrom, 16 kiloelectronvolt Cs plus primary beam was used. Measurements consisted of H, C, 12C, 16O, and 18O collected with EMs in multicollection. Terrestrial biotite and kerogen were used for isotopic standards. A significant challenge in O isotope measurement of hydrated minerals is the interference from 16OH at mass 17O. We ensured that the 17O and 16OH peaks were fully resolved by using a mass resolution of greater than 7000 and by careful analyses of San Carlos olivine, Burma spinel and chlorite hydrated mineral standards. The hydride was further suppressed with a cold finger attached to an LN2 dewar to trap volatiles in the sample chamber. All sputtered ions were counted (i.e. presputtering was not used); after applying background, yield and deadtime corrections, we performed a change-point analysis on our data via R in order to determine when the sample reached sputtering equilibrium; data points collected prior to the change point were excluded. Change-point analysis was also used to determine whether the IDP had completely sputtered. Results: Mineralogy. IDPs C35 and E46 exhibited hydrated mineralogies, Fe-Ni sulfide grains, nanoglobules and occasional enstatite grains distributed throughout a fine-grained Mg-Fe saponite matrix. C35 also contained breunnerite (Mg,Fe)CO3; solar flare tracks were observed in enstatite, indicating minimal atmospheric entry heating. The mineralogy of D46 is dominated by a large FeS grain with a minor component of adhering silicate material. D46 was strongly heated during atmorpheric entry as evidenced by a well-developed magnetite rim. EPMA analyses show that both C35 and E46 have high carbon contents of 20 weight percentage (approximately 6X CI). D46 contains approximately 6 wt.weight percentage C. A significant amount of the carbon is present as carbon nanoglobules. Results: Hydrogen isotopes: Although the bulk delta D values of both sections of L2079C35 were within error of SMOW (minus 33 plus or minus 19 per mille, 1 plus or minus 14 per mille 1 sigma), several delta D-rich hotspots were also identified, reaching 2000 per mille. As shown in Fig. 1, these hotspots are clearly associated with discrete carbonaceous inclusions that are akin to nanoglobules found in many meteorites and other IDPs. Oxygen Isotopes. Results of the oxygen isotope measurements are shown in Figure 1. The oxygen isotope composition for L2079C35 was delta 18O equals plus11.6 plus or minus 1.9per mille, delta 17O equals plus 7.9 plus or minus 1.9per mille (2 standard errors). The oxygen isotope composition for L2083D46 was delta 18O equals minus 8.1 plus or minus 1.9 per mille, delta 17O equals minus 6.4 plus or minus 3.1 per mille (2 standard errors). The oxygen isotope composition for L2083E46 was delta 18O equals plus 12.0 plus or minus 1.9 per mille, delta 17O equals plus 9.2 plus or minus 2.0 per mille (2 standard errors). Discussion: Despite mineralogical similarities to highly aqueously altered carbonaceous chondrites, the hydrated IDPs we analyzed have oxygen isotopic compositions that are distinct from matrix materials in the CI, CM, and CR chondrites. The IDPs plot along the Young-Russell line, with delta 17O values for C35 and E46 suggestive of interaction with a 16O-poor reservoir. However, we have thus far not observed evidence of extreme 16O-poor reservoirs expected from self-shielding models and observed in Acfer 094 simplectite. The high carbon contents of the IDPs also set them apart from known meteoritic samples. The lack of atmospheric entry heating effects are consistent with low encounter velocities and suggest either an asteroidal source, or a low inclination, low eccentricity cometary origin. Conclusions: The unusual oxygen isotopic compositions, high carbon contents, and the abundance of Drich nanoglobules, together, suggest that the high-carbon, hydrated IDPs are derived from a primitive source that is not yet represented in meteorite collections.

Snead, C. J.↗

Structure of Rhizobium sp. 4-9 histamine dehydrogenase and analysis of the electron transfer pathway to an abiological electron acceptor

Histamine dehydrogenase from the gram-negative bacterium Rhizobium sp. 4-9 (HaDHR) is a member of a small family of dehydrogenases containing a covalently attached FMN, and the only member so far identified to date that does not exhibit substrate inhibition. Here, in this study, we present the 2.1 Å resolution crystal structure of HaDHR. This new structure allowed for the identification of the internal electron transfer pathway to abiological ferrocene-based mediators. Alanine 437 was identified as the exit point of electrons from the Fe 4 S 4 cluster. The enzyme was modified with a Ser436Cys mutation to facilitate covalent attachment of a ferrocene moiety. When modified with Fc-maleimide, this new construct demonstrated direct electron transfer from the enzyme to a gold electrode in a histamine concentration-dependent manner without the need for any additional electron mediators.

59 BASIC BIOLOGICAL SCIENCES↗

Optical design and synthetic analysis of the electron cyclotron emission imaging diagnostic of HL-2M tokamak

The electron cyclotron emission imaging (ECEI) diagnostic is a powerful tool to study the MHD and turbulent transport in magnetically confined fusion plasmas. In this work, the optical system including the local oscillator (LO) coupling and radio frequency (RF) receiving optics, has been designed and analyzed for the HL-2M ECEI diagnostic. The LO optics can illuminate the antenna array and drive the mixer diode to work efficiently, with more than 36% of the beam intensity for the channels which probe the plasma edge relative to those of channels which probe the plasma core. The RF optics aims at guiding the plasma emission signal to the antenna array. To meet different physical requirements, three types of field of view have been achieved for the plasma imaging, with zoom factors of around 1, 1.5 and 2, respectively. The focal surfaces are almost flat, with a maximum off-mapping (defined as the radial distance between the beam waists of the lower-/uppermost antennas and electron cyclotron emission layer) less than 2.5 cm, which can match the electron cyclotron emission layer quite well and suppress the image distortion in the plasma edge region. Furthermore, the impact of possible vibrations and installation error on the focal plane has been evaluated. In addition, the predefined MHD and turbulence perturbations are well reproduced by combining the optical simulation results and synthetic ECEI modeling, which further verifies the good performance of the RF optics.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Phase transformations and phase equilibria in the Co–Sn–Ti system in the crystallization interval

The Co–Sn–Ti system was studied in the crystallization interval (below ~50 at% Sn) by the methods of Scanning Electron Microscopy, microprobe analysis, Differential Thermal Analysis, X-ray diffraction. The liquidus and solidus projections and the melting diagram were constructed. Only Co{sub 2}TiSn(τ1) ternary compound (Heusler phase-L1{sub 2}) was found in equilibria with the liquid in the concentration interval studied. Taking into account our recent data, the liquidus projection is characterized by the fields of primary crystallization of (βTi), (Co), binary-based phases Ti{sub 3}Sn, Ti{sub 2}Sn, Ti{sub 5}Sn{sub 3}, Ti{sub 6}Sn{sub 5}, Ti{sub 2}Co, TiCo, TiCo{sub 2} (c), TiCo{sub 2} (h), TiCo{sub 3}, βCo{sub 3}Sn{sub 2}, CoSn and ternary τ1. The solidus projection is characterized by thirteen three-phase fields, which result from invariant four-phase equilibria, five are of eutectic type (E) and eight of transition type (U) and the existence of one more region Ti{sub 2}Sn{sub 3}+βCoSn{sub 3}+(Sn) in the solidus projection is discussed. - Graphical abstract: Liquidus projection of the Ti–Ð ÐŽÐ Ñ• –Sn system. Fields of crystallization, isotherms and monovariant lines. - Highlights: • The Ti–Co–Sn system is first studied in the composition range up to 50% of Sn. • Liquidus and solidus projections, melting diagram and reaction scheme are constructed. • One ternary compound form in the studied temperature interval: (Co{sub 2}TiSn(τ1)).

36 MATERIALS SCIENCE↗

Analysis of synthetic electron cyclotron emission from the high field side of HL-2M tokamak plasmas

A synthetic electron cyclotron emission (ECE) diagnostic is used to interpret ECE signals from preset plasma equilibrium profiles, including magnetic field, electron density, and electron temperature. According to the simulation results, the electron temperature (T e ) profile covering the harmonic overlap region can be obtained by receiving ECE signals at the high field side (HFS) of the HL-2M plasma. The third harmonic ECE at the low field side (LFS) cannot pass through the second harmonic resonance layer at the HFS unless the optical thickness (τ) of the second harmonic becomes gray (τ ≤ 2). In addition, the impact of the relativistic frequency down-shift has been evaluated and corrected. The measurable range of the HFS ECE has been calculated by scanning different parameters (electron density, temperature, and magnetic field). Higher plasma parameters allow a wider radial range of electron temperature measurements. The minimum inner measurable position can reach R = 120 cm (r/a = -0.89) when the product of core temperature (T e0 ) and density (n e0 ) is greater than 35 × 10 19 keV m -3 , which is extended by more than 30 cm inward compared with that of the LFS measurement. The HFS ECE will greatly improve the diagnostic ability of ECE systems on the HL-2M tokamak.

47 OTHER INSTRUMENTATION↗

Decomposition of L a 2 – x S r x Cu O 4 into several L a 2 O 3 phases at elevated temperatures in ultrahigh vacuum inside a transmission electron microscope

Here, we report the decomposition of La 2–x Sr x CuO 4 into La 2 O 3 and Cu nanoparticles in ultrahigh vacuum, observed by in situ heating experiments in a transmission electron microscope. The analysis of electron diffraction data reveals that the phase decomposition process starts at about 150°C and is considerably expedited in the temperature range of 350°C–450°C. Two major resultant solid phases are identified as metallic Cu and La 2 O 3 by electron diffraction, simulation, and electron energy-loss spectroscopy (EELS) analyses. With the aid of calculations, La 2 O 3 phases are further identified to be derivatives of a fluorite structure—fluorite, pyrochlore, and (distorted) bixbyite—characterized by different oxygen-vacancy order. Additionally, the bulk plasmon energy and the fine structures of the O K and LaM 4,5 EELS edges are reported for these structures, along with simulated O K x-ray absorption near-edge structure. The resultant Cu nanoparticles and La 2 O 3 phases remain unchanged after cooling to room temperature.

36 MATERIALS SCIENCE↗