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At least 271 records · Page 15

Strain-Modified Raman Responses in Monolayer MoS 2 Nanobubbles Resolved at 5 nm

The formation of nanoscale bubbles is an unavoidable consequence during the transfer of two-dimensional materials onto target substrates, driven by van der Waals interactions at the interface. While often viewed as imperfections, these nanoscale bubbles have garnered considerable scientific interest due to the substantial in-plane strain gradients they induce, which in turn give rise to a variety of intriguing optoelectronic effects, particularly in semiconducting transition metal dichalcogenides. Determining and analyzing the strain distribution within nanobubbles at the nanoscale is crucial for advancing our understanding of these underlying strain-induced effects. Here, we present a high-resolution scanning tunneling microscopy-based tip-enhanced Raman spectroscopic investigation of localized nanoscale strain distribution within the nanobubbles formed between monolayer MoS 2 and Au interface. By employing cryogenic temperature (78 K), we successfully differentiate the nanoscale Raman signatures between nanobubble edge and pristine MoS 2 . We verify a maximum tensile strain of ∽1.15–1.34% at the nanobubble edge, which gradually diminishes toward the center, yielding a cross-sectional strain profile consistent with a doughnut-shaped distribution. Furthermore, we report to achieve ∽5 nm spatial resolution in probing such edge-localized strain within the nanobubble. In addition, comparative average strain analysis of such MoS 2 nanobubbles is conducted via geometric mechanistic analysis such as membrane and nonlinear plate theories, providing key insight into the geometric nature near the bubble edge. Our work provide fundamental information about strain-induced nanoscale chemical understanding of 2D materials on the nanometer scale, paving the way for practical applications of nanobubbles in strain-engineered optoelectronic devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Atom Efficiency of Pd Sites for Methane Combustion: Single Atom Catalysts Versus Nanocatalysts

Methane combustion is an important reaction for energy production and methane removal from the atmosphere. This reaction highly relies on the use of noble metal Pd-based catalysts, which therefore drives the pursuit of catalysts with high atomic dispersion and activity. In this work, Pd/ceria catalysts dominated with Pd single atoms or nanosized Pd clusters (∼1 nm) are prepared and characterized by combining high-resolution high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), in situ diffuse reflectance infrared Fourier-transform spectroscopy (DRIFTS), and Raman and X-ray absorption spectroscopy (XAS) techniques. By comparing the turnover frequencies (TOF; per every Pd atom) of Pd/ceria single atom catalysts and nanocatalysts, it is found that the atom efficiency of Pd is increased by 10 ∼30 times from single atom catalysts to nanocatalysts. For Pd single atom catalysts, although their activity can be tuned by changing the local structures, the intrinsic activity and number of active sites need to be further improved by engineering the surfaces of supports. For nanosized Pd species, despite the high TOF, the Pd atoms in the bulk structure are not directly participating in the catalytic reaction. Furthermore, this work highlights the importance of increasing the intrinsic activity of individual noble atoms, as well as the homogeneity of their local structures. For Pd/ceria systems reported in this work, our results indicate that from the application point of view, at the current stage, it is not practical to replace Pd nanocatalysts with single atom catalysts for methane combustion.

Pd↗

Spontaneously formed phonon frequency combs in van der Waals solid CrGeTe 3 and CrSiTe 3

Optical phonon engineering through nonlinear effects has been utilized in ultrafast control of material properties. However, nonlinear optical phonons typically exhibit rapid decay due to strong mode-mode couplings, limiting their effectiveness in temperature or frequency sensitive applications. Here we report the observation of long-lived nonlinear optical phonons through the spontaneous formation of phonon frequency combs in the van der Waals material CrXTe 3 (X=Ge, Si) using high-resolution Raman scattering. Unlike conventional optical phonons, the highest A g mode in CrGeTe 3 splits into equidistant, sharp peaks forming a frequency comb that persists for hundreds of oscillations and survives up to 200K. These modes correspond to localized oscillations of Ge 2 Te 6 clusters, isolated from Cr hexagons, behaving as independent quantum oscillators. Introducing a cubic nonlinear term to the harmonic oscillator model, we simulate the phonon time evolution and successfully replicate the observed comb structure. Similar frequency comb behavior is observed in CrSiTe 3 , demonstrating the generalizability of this phenomenon. Our findings demonstrate that Raman scattering effectively probes high-frequency nonlinear phonon modes, offering insight into the generation of long-lived, tunable phonon frequency combs with potential applications in ultrafast material control and phonon-based technologies.

36 MATERIALS SCIENCE↗

Using electron energy-loss spectroscopy to measure nanoscale electronic and vibrational dynamics in a TEM

Electron energy-loss spectroscopy (EELS) can measure similar information to x-ray, UV–Vis, and IR spectroscopies but with atomic resolution and increased scattering cross-sections. Recent advances in electron monochromators have expanded EELS capabilities from chemical identification to the realms of synchrotron-level core-loss measurements and to low-loss, 10–100 meV excitations, such as phonons, excitons, and valence structures. EELS measurements are easily correlated with electron diffraction and atomic-scale real-space imaging in a transmission electron microscope (TEM) to provide detailed local pictures of quasiparticle and bonding states. This perspective provides an overview of existing high-resolution EELS (HR-EELS) capabilities while also motivating the powerful next step in the field—ultrafast EELS in a TEM. Ultrafast EELS aims to combine atomic-level, element-specific, and correlated temporal measurements to better understand spatially specific excited-state phenomena. Ultrafast EELS measurements also add to the abilities of steady-state HR-EELS by being able to image the electromagnetic field and use electrons to excite photon-forbidden and momentum-specific transitions. We discuss the technical challenges ultrafast HR-EELS currently faces, as well as how integration with in situ and cryo measurements could expand the technique to new systems of interest, especially molecular and biological samples.

Chemistry↗

Optoelectronic and structural characterization of trapezoidal defects in 4H-SiC epilayers and the effect on MOSFET reliability

To this day, trapezoidal defects are found in clusters and high counts in wafers representing the industry standard in terms of material quality being produced. This study sheds light on the nature, origin, behavior, and impact of this defect on device yield and reliability. Trapezoidal defects in 4H-SiC epitaxial layers were investigated by photoluminescence (PL) imaging, scanning electron microscopy (SEM), cathodoluminescence spectrum imaging (CLSI), SEM electron beam induced current (EBIC) imaging, and by transmission electron microscopy (TEM) observation. The bar-shaped stacking faults were identified by the PL and CL measurements with a peak emission wavelength of 420 and 450 nm. An optoelectronic behavioral study based on the recombination enhanced dislocation glide mechanism revealed how expanding dislocations and stacking faults interact with each other. Combining the luminescence and microscopy results, the nature of the stacking faults was identified as being a combination of Shockley-type and Frank-type stacking faults. The TEM analysis showed that these defects originate from the substrate and the stacking sequences of some of the faults were determined as (…2, 4, 2…) and (…2, 3, 2…) in the Zhdanov's notation by high-resolution TEM. The origin of this defect is speculated based on our results and previous reports. The EBIC imaging showed that the high density of SFs in these towers is a strong site of carrier recombination, which presumably has an impact on the transfer characteristics of SiC devices. Furthermore, these defects have shown to impact metal oxide semiconductor field effect transistors electrical performance via an increase in the on-state resistance depending on the coverage percentage of the tower of defects in the active area of the device.

4H-SiC↗

Deep learning-driven super-resolution in Raman hyperspectral imaging: Efficient high-resolution reconstruction from low-resolution data

Deep learning (DL) has become an indispensable tool in hyperspectral data analysis, automatically extracting valuable features from complex, high-dimensional datasets. Super-resolution reconstruction, an essential aspect of hyperspectral data, involves enhancing spatial resolution, particularly relevant to low-resolution hyperspectral data. Yet, the pursuit of super-resolution in hyperspectral analysis is fraught with challenges, including acquiring ground truth high-resolution data for training, generalization, and scalability. The pressing issue of extended spectral acquisition times, notably for high-resolution scans, is a significant roadblock in hyperspectral imaging. Super-resolution methods offer a promising solution by providing higher spatial resolution data to expedite data collection and yield more efficient outcomes. This paper delves into a practical application of these concepts using Raman imaging, where spectral acquisition times can be prohibitively long. In this context, DL-based super-resolution models demonstrate their efficacy by predicting and reconstructing high-resolution Raman data from low-resolution input, eliminating the need for resource-intensive high-resolution scans. While previous work often relied on substantial high-resolution datasets, this study showcases the ability to achieve similar outcomes even with limited data, presenting a more practical and cost-effective approach. In conclusion, the results offer a glimpse into the transformative potential of this technology to streamline hyperspectral imaging applications by saving valuable time and resources through the successful generation of high-resolution data from low-resolution inputs.

42 ENGINEERING↗

Reward based optimization of resonance-enhanced piezoresponse spectroscopy

Dynamic spectroscopies in scanning probe microscopy (SPM) are critical for probing material properties, such as force interactions, mechanical properties, polarization switching, electrochemical reactions, and ionic dynamics. However, the practical implementation of these measurements is constrained by the need to balance imaging time and data quality. Signal to noise requirements favor long acquisition times and high frequencies to improve signal fidelity. However, these are limited on the low end by contact resonant frequency and photodiode sensitivity and on the high end by the time needed to acquire high-resolution spectra or the propensity for sample degradation under high field excitation over long times. The interdependence of key parameters such as instrument settings, acquisition times, and sampling rates makes manual tuning labor-intensive and highly dependent on user expertise, often yielding operator-dependent results. These limitations are prominent in techniques like dual amplitude resonance tracking in piezoresponse force microscopy that utilize multiple concurrent feedback loops for topography and resonance frequency tracking. Here, a reward-driven workflow is proposed that automates the tuning process, adapting experimental conditions in real time to optimize data quality. Furthermore, this approach significantly reduces the complexity and time required for manual adjustments and can be extended to other SPM spectroscopic methods, enhancing overall efficiency and reproducibility.

47 OTHER INSTRUMENTATION↗

Formation of distinctive nanostructured metastable polymorphs mediated by kinetic transition pathways in germanium

High-pressure β -Sn germanium may transform into diverse metastable allotropes with distinctive nanostructures and unique physical properties via multiple pathways under decompression. However, the mechanism and transition kinetics remain poorly understood. Here, we investigate the formation of metastable phases and nanostructures in germanium via controllable transition pathways of β -Sn Ge under rapid decompression at different rates. High-resolution transmission electron microscopy reveals three distinct metastable phases with the distinctive nanostructures: an almost perfect st12 Ge crystal, nanosized bc8/r8 structures with amorphous boundaries, and amorphous Ge with nanosized clusters (0.8–2.5 nm). Fast in situ x-ray diffraction and x-ray absorption measurements indicate that these nanostructured products form in certain pressure regions via distinct kinetic pathways and are strongly correlated with nucleation rates and electronic transitions mediated by compression rate, temperature, and stress. This work provides deep insight into the controllable synthesis of metastable materials with unique crystal symmetries and nanostructures for potential applications.

36 MATERIALS SCIENCE↗

Deuterium supersaturated surface layer in tungsten: ion energy dependence

Abstract Properties of deuterium (D) supersaturated surface layers (DSSLs) formed in tungsten (W), such as thickness, internal microstructures, and D retention, are experimentally investigated as a function of the incident ion energy, E i . W samples were exposed to D plasmas in the PISCES-A linear plasma device in a range of E i ∼ 45–175 eV, while other plasma exposure parameters were fixed: sample temperature, T s , ∼423 K, ion flux, Γ i , ∼1.2 × 10 21 m −2 s −1 , and fluence, Φ i , ∼3.0 × 10 24 m −2 . High-resolution, cross-sectional, transmission electron microscopy observations confirm that (1) a DSSL forms even at the lowest E i ∼ 45 eV, (2) the DSSL thickness, Δ t DSSL , is found to decrease with decreasing E i from ∼11–12 nm at E i ∼ 175 eV to ∼5–6 nm at ∼45 eV, and to agree with approximately the maximum implantation depth calculated using SDTrimSP, and (3) high-density D nanobubbles with a diameter of ∼1 nm or less exist inside the DSSL, which is deemed to validate a theory-predicted vacancy stabilization process due to trapping of a solute D atom(s). Utilizing a D areal density of ∼4.2 × 10 19 m −2 in the first 14 nm from the surface at E i ∼ 75 eV from nuclear reaction analysis and the measured E i dependence of Δ t DSSL , our previous laser-induced breakdown spectroscopy data is updated: both dynamic and static D retention increase with decreasing E i , and the D/W atomic fraction during plasma exposure reaches ∼0.3 at E i ∼ 45 eV. A possible DSSL formation mechanism is proposed.

Physics↗

Cyclotron radiation emission spectroscopy of electrons from tritium $β$ decay and 83m Kr internal conversion

Project 8 has developed a novel technique, cyclotron radiation emission spectroscopy (CRES), for direct neutrino mass measurements. A CRES-based experiment on the beta spectrum of tritium has been carried out in a small-volume apparatus. Here, we provide a detailed account of the experiment, focusing on systematic effects and analysis techniques. In a Bayesian (frequentist) analysis, we measure the tritium endpoint as ${18}$ ${553}_{—19}^{+18}$ (${18}$ ${548}_{—19}^{+19}$) eV and set upper limits of 155 (152) eV (90% C.L.) on the neutrino mass. No background events are observed beyond the endpoint in 82 days of running. We also demonstrate an energy resolution of 1.66 ± 0.19 eV in a resolution-optimized magnetic trap configuration by measuring 83m Kr 17.8-keV internal-conversion electrons. These measurements establish CRES as a low-background, high-resolution technique with the potential to advance neutrino mass sensitivity

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Filterscope Techniques for Parasitic Signal Screening

Here, the filterscope diagnostic uses bandpass filters and photomultiplier tubes (PMTs) to detect specific spectral emission lines. A filterscope was used to measure the W I 400.88 nm line emission as a function of ion energy on the Radio Frequency Plasma Interaction Experiment (RF PIE) for the purpose of assessing W erosion on plasma-facing components (PFCs). Different filter techniques are being explored and compared in order to effectively screen out nearby impurity lines, like the Ar II 401.39 nm line. The effectiveness of these techniques is determined by comparing the measurements to a high-resolution 1.0 m Czerny–Turner spectrometer with 0.012 nm spectral resolution. The ability to filter out nearby impurity emissions is useful when imaging PFCs in fusion devices including divertor and antenna guard limiters. Initial results with a helium plasma show little difference between the two techniques at higher bias voltages. In a helium plasma at lower dc bias voltages, a two-filter technique with filters at two separate wavelengths was shown to be more effective at screening out background signals. Data collected with an argon plasma however show the technique with overlapping filters on the line of interest is a closer match to spectrometer data at lower dc bias voltages.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Resolve instrument onboard XRISM: design, integration, and instrument test results

The Resolve instrument onboard the X-Ray Imaging and Spectroscopy Mission (XRISM) consists of an array of 6 × 6 silicon-thermistor microcalorimeters cooled down to 50 mK and a high-throughput X-ray mirror assembly (XMA) with a focal length of 5.6 m. XRISM is a recovery mission of ASTRO-H/Hitomi, and the Resolve instrument is a rebuild of the ASTRO-H Soft X-ray spectrometer (SXS) and the Soft X-ray Telescope (SXT) that achieved energy resolution of ∼ 5 eV FWHM on orbit, with several important changes based on lessons learned from ASTRO-H. The flight models of the Dewar and the electronics boxes were fabricated, and the instrument test and calibration were conducted in 2021. By tuning the cryocooler frequencies, energy resolution better than 4.9 eV FWHM at 6 keV was demonstrated for all 36 pixels and high-resolution grade events, as well as energy-scale accuracy better than 2 eV up to 30 keV. The immunity of the detectors to microvibration, electrical conduction, and radiation was evaluated. The instrument was delivered to the spacecraft system in April 2022. The XMA was tested and calibrated separately. Its angular resolution is 1.27′, and the effective area of the mirror itself is 570 cm 2 at 1 keV and 424 cm 2 at 6 keV. We report the design and the major changes from the ASTRO-H SXS, the integration, and the results of the instrument test.

X-ray↗

Full Rod Length Gamma Spectroscopy Measurements of LWR Used Fuel Rods

Twenty-five high-burnup pressurized water reactor used fuel rods were scanned in the Irradiated Fuels Examination Laboratory at Oak Ridge National Laboratory with a high-resolution gamma spectrometer. A planar high-purity germanium detector was used across an energy range from 60 keV to 3 MeV. Gamma spectra of individual fuel rods were collected in 4.5 mm steps along the entire length of each rod. Additional spectra were collected on select rods in rotational increments of 30 degrees to provide data on the distribution of fission products along the rod perimeter.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Quantitative Nonlinear Optical Polarimetry with High Spatial Resolution

Nonlinear optical microscopy such as in the optical second-harmonic generation (SHG) modality has become a popular tool today for probing materials in the physical and biological sciences. While imaging and spectroscopy are widely used in the microscopy mode, nonlinear polarimetry, which can shed light on materials’ symmetry and microstructure, is relatively underdeveloped. This is partly because quantitative analytical modeling of the optical SHG response for anisotropic crystals and films largely assumes low-numerical aperture (NA) focusing of light, where the plane-wave approximation is sufficient. Tight focusing provides unique benefits in revealing out-of-plane polarization responses, which cannot be detected by near-plane-wave illumination at normal incidence. Here, we outline a method for quantitatively analyzing SHG polarimetry measurements obtained under high-NA focusing within a microscope geometry. Experiments and simulations of a variety of standard samples, from single crystals to thin films, are in good agreement, including measured and simulated spatial SHG maps of ferroelectric domains. A solution to the inverse problem is demonstrated, where the spatial distribution of an SHG tensor with unknown tensor coefficient magnitudes is determined by experimentally measured polarimetry. The ability to extract the out-of-plane component of the nonlinear polarization in normal incidence is demonstrated, which can be valuable for high-resolution polarimetry of 2D materials, thin films, heterostructures, and uniaxial crystals with a strong out-of-plane response.

36 MATERIALS SCIENCE↗

Closed-loop electron-beam-induced spectroscopy and nanofabrication around individual quantum emitters

Color centers in diamond play a central role in the development of quantum photonic technologies, and their importance is only expected to grow in the near future. For many quantum applications, high collection efficiency from individual emitters is required, but the refractive index mismatch between diamond and air limits the optimal collection efficiency with conventional diamond device geometries. While different out-coupling methods with near-unity efficiency exist, many have yet to be realized due to current limitations in nanofabrication methods, especially for mechanically hard materials like diamond. Here, we leverage electron-beam-induced etching to modify Sn-implanted diamond quantum microchiplets containing integrated waveguides with a width and thickness of 280 nm and 200 nm, respectively. This approach allows for simultaneous high-resolution imaging and modification of the host matrix with an open geometry and direct writing. When coupled with the cathodoluminescence signal generated from the electron–emitter interactions, we can monitor the enhancement of the quantum emitters in real-time with nanoscale spatial resolution. The operando cathodoluminescence measurement and fabrication around single photon emitters demonstrated here provide a new foundation for the potential control of emitter–cavity interactions in integrated quantum photonics.

36 MATERIALS SCIENCE↗

Nanotomography for Quantitative 3D Particle Reconstruction

Particulates are ubiquitous across fuel cycle operations and carry critical information about particle formation, processing, and potential proliferation-related activities. Traditional analytical techniques, including micro-Raman spectroscopy and standard electron microscopy, are often limited in spatial resolution or dimensionality, particularly when used to examine metallic or submicron-scale features. Understanding particle morphology, phase distribution, and internal porosity is essential for constraining formation conditions, thermodynamic environments, and material transport behavior. In this report, we demonstrate the application of plasma focused ion beam nanotomography to reconstruct micron-scale particulates at nanoscale resolution. Using high-resolution backscattered electron imaging and Avizo software, we obtained 3D reconstructions that enabled quantitative analysis of particle morphology, phase composition, and internal voids. Representative examples include a Ta particle with a large central void and a composite particle with embedded tetrahedral crystalline structures. These reconstructions reveal structural and compositional details that are inaccessible through conventional 2D imaging. The results demonstrate that nanotomography provides both qualitative and quantitative insights into particle formation and behavior. Using nanotomography, porosity and phase distributions can be quantified to inform models of particle density, transport, and solidification conditions. Beyond technical insights, the workflow developed here establishes a transferable capability for analyzing heterogeneous particles and has potential applications in bulk materials studies via x-ray computed tomography or other volumetric imaging modalities. Ongoing efforts are focused on optimizing the workflow to process multiple particles simultaneously, increasing throughput and statistical robustness. Overall, this work illustrates the power of nanotomography as a tool for connecting particulate morphology to formation mechanisms, composition, and transport, thereby strengthening analytical capabilities for nuclear forensics, fuel cycle analysis, and related scientific investigations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Hubble Space Telescope Observations within the Sphere of Influence of the Powerful Supermassive Black Hole in PKS 0745-191

We present Space Telescope Imaging Spectrograph observations from the Hubble Space Telescope of the supermassive black hole (SMBH) at the center of PKS 0745-191, a brightest cluster galaxy (BCG) undergoing powerful radio-mode active galactic nucleus (AGN) feedback (P cav ~ 5 × 10 45 erg s -1 ). These high-resolution data offer the first spatially resolved map of gas dynamics within an SMBH's sphere of influence under such powerful feedback. Our results reveal the presence of highly chaotic, nondrotational ionized gas flows on subkiloparsec scales, in contrast to the more coherent flows observed on larger scales. While radio-mode feedback effectively thermalizes hot gas in galaxy clusters on kiloparsec scales, within the core, the hot gas flow may decouple, leading to a reduction in angular momentum and supplying ionized gas through cooling, which could enhance accretion onto the SMBH. This process could, in turn, lead to a self-regulating feedback loop. Compared to other BCGs with weaker radio-mode feedback, where rotation is more stable, intense feedback may lead to more chaotic flows, indicating a stronger coupling between jet activity and gas dynamics. Additionally, we observe a sharp increase in velocity dispersion near the nucleus, consistent with a very massive M BH ~ 1.5 × 10 10 M ⊙ SMBH. The density profile of the ionized gas is also notably flat, paralleling the profiles observed in X-ray gas around galaxies where the Bondi radius is resolved. These results provide valuable insights into the complex mechanisms driving galaxy evolution, highlighting the intricate relationship between SMBH fueling and AGN feedback within the host galaxy.

79 ASTRONOMY AND ASTROPHYSICS↗

The DECam MAGIC Survey: Spectroscopic Follow-up of the Most Metal-poor Stars in the Distant Milky Way Halo *

In this work, we present high-resolution spectroscopic observations for six metal-poor stars with [Fe/H] < –3 (including one with [Fe/H] < –4), selected using narrowband Ca ii HK photometry from the DECam MAGIC Survey. The spectroscopic data confirm the accuracy of the photometric metallicities and allow for the determination of chemical abundances for 16 elements, from carbon to barium. The program stars have chemical abundances consistent with the [Fe/H] < –3 range. A kinematic/dynamical analysis suggests that all program stars belong to the distant Milky Way halo population (heliocentric distances 35 < d helio /kpc ≲ 55), including three with high-energy orbits that might have been associated with the Magellanic system and one, J0026−5445, having parameters consistent with being a member of the Sagittarius stream. The remaining two stars show kinematics consistent with the Gaia-Sausage/Enceladus dwarf galaxy merger. J0433−5548, with [Fe/H] = –4.12, is a carbon-enhanced ultra metal-poor star, with [C/Fe] = +1.73. This star is believed to be a bona fide second-generation star, and its chemical abundance pattern was compared with yields from metal-free supernova models. Results suggest that J0433−5548 could have been formed from a gas cloud enriched by a single supernova explosion from an ∼11 M ⊙ star in the early Universe. The successful identification of such objects demonstrates the reliability of photometric metallicity estimates, which can be used for target selection and statistical studies of faint targets in the Milky Way and its satellite population. These discoveries illustrate the power of measuring chemical abundances of metal-poor Milky Way halo stars to learn more about early galaxy formation and evolution.

CEMP stars↗