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At least 343 records · Page 19

Size-Resolved Shape Evolution in Inorganic Nanocrystals Captured via High-Throughput Deep Learning-Driven Statistical Characterization

Precise size and shape control in nanocrystal synthesis is essential for utilizing nanocrystals in various industrial applications, such as catalysis, sensing, and energy conversion. However, traditional ensemble measurements often overlook the subtle size and shape distributions of individual nanocrystals, hindering the establishment of robust structure–property relationships. In this study, we uncover intricate shape evolutions and growth mechanisms in Co 3 O 4 nanocrystal synthesis at a subnanometer scale, enabled by deep-learning-assisted statistical characterization. By first controlling synthetic parameters such as cobalt precursor concentration and water amount then using high resolution electron microscopy imaging to identify the geometric features of individual nanocrystals, this study provides insights into the interplay between synthesis conditions and the sizedependent shape evolution in colloidal nanocrystals. Utilizing population-wide imaging data encompassing over 441,067 nanocrystals, we analyze their characteristics and elucidate previously unobserved size-resolved shape evolution. This high-throughput statistical analysis is essential for representing the entire population accurately and enables the study of the size dependency of growth regimes in shaping nanocrystals. Our findings provide experimental quantification of the growth regime transition based on the size of the crystals, specifically (i) for faceting and (ii) from thermodynamic to kinetic, as evidenced by transitions from convex to concave polyhedral crystals. Additionally, we introduce the concept of an “onset radius,” which describes the critical size thresholds at which these transitions occur. This discovery has implications beyond achieving nanocrystals with desired morphology; it enables finely tuned correlation between geometry and material properties, advancing the field of colloidal nanocrystal synthesis and its applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

High-resolution high-throughput spatiotemporal strain imaging reveals loss mechanisms in a surface acoustic wave device

Surface acoustic wave devices are key components for processing radio frequency signals in wireless communication because these devices offer simultaneously high performance, compact size and low cost. The optimization of the device structure requires a quantitative understanding of energy conversion and loss mechanisms. Here we use stroboscopic full-field diffraction x-ray microscopy to reveal an unanticipated acoustic loss in a prototypical one-port resonator device. A non-uniform acoustic excitation in the active area was responsible for the substantial end and side leakages observed at the design frequency. Quantitative analysis of the strain amplitude using a wave decomposition method allowed the determination of several key device parameters. This high-resolution high-throughput spatiotemporal strain imaging technique is more generally applicable to the study of dynamic strain modulation in nanoscale acoustic, electronic, optical and quantum devices. The high sensitivity allows precise measurement of the strain modulation with picometer-scale amplitude.

Zhou, Tao [ESRF - The European Synchrotron, Grenob↗

Molecular-resolution imaging of ice crystallized from liquid water by cryogenic liquid-cell TEM

Despite the ubiquity of ice, a molecular-resolution image of nanoscopic defects or microstructures in ice crystallized from liquid water has never been obtained. This is mainly due to the difficulties in preparing and preserving crystalline ice samples that can survive under high-resolution imaging conditions. Here, we report the stabilization and Å-resolution electron imaging of ice Ih crystallized from liquid water by developing cryogenic liquid-cell transmission electron microscopy (CRYOLIC-TEM). We combine lattice mapping with molecular dynamics simulations to reveal that ice formation is highly tolerant to nanoscale defects such as misoriented subdomains and trapped gas bubbles, which are stabilized by molecular-scale structural motifs. Importantly, bubble surfaces adopt low-energy nanofacets and create negligible strain fields in the surrounding crystal. These bubbles can dynamically nucleate, grow, migrate, dissolve, and coalesce under electron irradiation and be monitored in situ near a steady state. This work improves our understanding of water crystallization behaviors at a molecular spatial resolution.

Materials science↗

Cryo2StructData: A Large Labeled Cryo-EM Density Map Dataset for AI-based Modeling of Protein Structures

The advent of single-particle cryo-electron microscopy (cryo-EM) has brought forth a new era of structural biology, enabling the routine determination of large biological molecules and their complexes at atomic resolution. The high-resolution structures of biological macromolecules and their complexes significantly expedite biomedical research and drug discovery. However, automatically and accurately building atomic models from high-resolution cryo-EM density maps is still time-consuming and challenging when template-based models are unavailable. Artificial intelligence (AI) methods such as deep learning trained on limited amount of labeled cryo-EM density maps generate inaccurate atomic models. To address this issue, we created a dataset called Cryo2StructData consisting of 7,600 preprocessed cryo-EM density maps whose voxels are labelled according to their corresponding known atomic structures for training and testing AI methods to build atomic models from cryo-EM density maps. Cryo2StructData is larger than existing, publicly available datasets for training AI methods to build atomic protein structures from cryo-EM density maps. We trained and tested deep learning models on Cryo2StructData to validate its quality showing that it is ready for being used to train and test AI methods for building atomic models.

59 BASIC BIOLOGICAL SCIENCES↗

Investigation of interfacial strength in nacre-mimicking tungsten heavy alloys for nuclear fusion applications

Abstract Tungsten heavy alloys have been proposed as plasma facing material components in nuclear fusion reactors and require experimental investigation in their confirmation. For this purpose, a 90W–7Ni–3Fe alloy has been selected and microstructurally manipulated to present a multiphase brick-and-mortar structure of W-phase ‘bricks’ surrounded by a ductile ‘mortar’. This work draws inspiration from nature to artificially imitate the extraordinary combination of strength and stiffness exhibited by mollusks and produce a nacre-mimicking metal matrix composite capable of withstanding the extremely hostile environment of the reactor interior and maintaining structural integrity. The underlying mechanisms behind this integrity have been probed through high-resolution structural and chemical characterization techniques and have revealed chemically diffuse phase boundaries exhibiting unexpected lattice coherency. These features have been attributed to an increase in the energy required for interfacial decohesion in these systems and the simultaneous expression of high strength and toughness in tungsten heavy alloys.

36 MATERIALS SCIENCE↗

Simultaneous bright- and dark-field X-ray microscopy at X-ray free electron lasers

Abstract The structures, strain fields, and defect distributions in solid materials underlie the mechanical and physical properties across numerous applications. Many modern microstructural microscopy tools characterize crystal grains, domains and defects required to map lattice distortions or deformation, but are limited to studies of the (near) surface. Generally speaking, such tools cannot probe the structural dynamics in a way that is representative of bulk behavior. Synchrotron X-ray diffraction based imaging has long mapped the deeply embedded structural elements, and with enhanced resolution, dark field X-ray microscopy (DFXM) can now map those features with the requisite nm-resolution. However, these techniques still suffer from the required integration times due to limitations from the source and optics. This work extends DFXM to X-ray free electron lasers, showing how the $$10^{12}$$ 10 12 photons per pulse available at these sources offer structural characterization down to 100 fs resolution (orders of magnitude faster than current synchrotron images). We introduce the XFEL DFXM setup with simultaneous bright field microscopy to probe density changes within the same volume. This work presents a comprehensive guide to the multi-modal ultrafast high-resolution X-ray microscope that we constructed and tested at two XFELs, and shows initial data demonstrating two timing strategies to study associated reversible or irreversible lattice dynamics.

47 OTHER INSTRUMENTATION↗

High-pressure phase transition in 3-D printed nanolamellar high-entropy alloy by imaging and simulation insights

Abstract We report on the high-resolution imaging and molecular dynamics simulations of a 3D-printed eutectic high-entropy alloy (EHEA) Ni 40 Co 20 Fe 10 Cr 10 Al 18 W 2 consisting of nanolamellar BCC and FCC phases. The direct lattice imaging of 3D-printed samples shows the Kurdjumov–Sachs (K–S) orientation relation {111} FCC parallel to {110} BCC planes in the dual-phase lamellae. Unlike traditional iron and steels, this alloy shows an irreversible BCC-to-FCC phase transformation under high pressures. The nanolamellar morphology is maintained after pressure cycling to 30 GPa, and nano-diffraction studies show both layers to be in the FCC phase. The chemical compositions of the dual-phase lamellae after pressure recovery remain unchanged, suggesting a diffusion-less BCC–FCC transformation in this EHEA. The lattice imaging of the pressure-recovered sample does not show any specific orientation relation between the two resulting FCC phases, indicating that many grain orientations are produced during the BCC–FCC phase transformation. Molecular dynamics simulations on phase transformation in a nanolamellar BCC/FCC in K–S orientation show that phase transformation from BCC to FCC is completed under high pressures, and the FCC phase is retained on decompression aided by the stable interfaces. Our work elucidates the irreversible phase transformation under static compression, providing an understanding of the orientation relationships in 3-D printed EHEA under high pressures.

3-D Printing↗

Ptychography at all wavelengths

Ptychography is a computational imaging technique that operates across multiple wavelength regimes, from electron (picometres) to X-ray (~0.1 nm), extreme ultraviolet (~10 nm) and visible light (micrometres). By reconstructing both amplitude and phase from diffraction patterns, ptychography enables high-resolution, quantitative imaging without conventional limitations imposed by lens-based optics. Ptychography has enabled advances across a range of scales: achieving deep-sub-angstrom resolution with electron microscopy, becoming an indispensable tool at X-ray synchrotron facilities worldwide and overcoming the trade-offs between resolution and field-of-view in optical imaging. This Primer provides a unified treatment of ptychography across these wavelength regimes. First, we discuss theoretical foundations, reconstruction algorithms, experimental considerations and wavelength-specific challenges. We then give examples of raw and processed data from various configurations and wavelengths. Next, we highlight key applications of ptychography in life sciences, materials science and industry. We also discuss data standards, open-source software implementations and best practices for ensuring reproducibility across different wavelength regimes. Finally, we consider limitations and future opportunities for ptychography. Together with accompanying datasets and code implementations, this Primer aims to serve newcomers and experienced practitioners in the field, facilitating broader adoption of ptychography across different disciplines.

47 OTHER INSTRUMENTATION↗

High-resolution planar electron beam induced current in bulk diodes using high-energy electrons

Understanding the impact of high-energy electron radiation on device characteristics remains critical for the expanding use of semiconductor electronics in space-borne applications and other radiation harsh environments. Here in this paper, we report on in situ measurements of high-energy electron radiation effects on the hole diffusion length in low threading dislocation density homoepitaxial bulk n-GaN Schottky diodes using electron beam induced current (EBIC) in high-voltage scanning electron microscopy mode. Despite the large interaction volume in this system, quantitative EBIC imaging is possible due to the sustained collimation of the incident electron beam. This approach enables direct measurement of electron radiation effects without having to thin the specimen. Using a combination of experimental EBIC measurements and Monte Carlo simulations of electron trajectories, we determine a hole diffusion length of 264 ± 11 nm for n-GaN. Irradiation with 200 kV electron beam with an accumulated dose of 24 × 10 16 electrons cm -2 led to an approximate 35% decrease in the minority carrier diffusion length.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Platinum nanoparticle compression: Combining in situ TEM and atomistic modeling

The mechanical behavior of nanoparticles governs their performance and stability in many applications. However, the small sizes of technologically relevant nanoparticles, with diameters in the range of 10 nm or less, significantly complicate experimental examination. These small nanoparticles are difficult to manipulate onto commercial test platforms and deform at loads that are below the typical noise floor of the testing instruments. Here, we synthesized small platinum nanoparticles directly onto a mechanical tester and used a modified nanomanipulator to enhance load resolution to the nanonewton scale. We demonstrated the in situ compression of an 11.5-nm platinum nanoparticle with simultaneous high-resolution measurements of load and particle morphology. Molecular dynamics simulations were performed on similarly sized particles to achieve complementary measurements of load and morphology, along with atomic resolution of dislocations. The experimental and simulation results revealed comparable values for the critical resolved shear stress for failure, 1.28 and 1.15 GPa, respectively. Altogether, this investigation demonstrated the promise of, and some initial results from, the combination of atomistic simulations and in situ experiments with an unprecedented combination of high spatial resolution and high load resolution to understand the behavior of metal nanoparticles under compression.

42 ENGINEERING↗

NiGa 2 O 4 interfacial layers in NiO/Ga 2 O 3 heterojunction diodes at high temperature

NiO/Ga 2 O 3 heterojunction diodes have attracted attention for high-power applications, but their high temperature performance and reliability remain underexplored. Here, we report the time evolution of the electrical properties in the widely studied p-NiO/n-Ga 2 O 3 heterojunction diodes and formation of NiGa 2 O 4 interfacial layers at high temperatures. Results of our thermal cycling experiment show an initial leakage current increase which stabilizes after sustained thermal load, due to reactions at the NiO–Ga 2 O 3 interface. High-resolution TEM microstructure analysis of the devices after thermal cycling indicates that the NiO–Ga 2 O 3 interface forms a ternary compound at high temperatures, and thermodynamic calculations suggest the formation of the spinel NiGa 2 O 4 layer between NiO and Ga 2 O 3 . First-principles defect calculations find that NiGa 2 O 4 shows low p-type intrinsic doping and hence can serve to limit electric field crowding at the interface. Vertical NiO/ Ga 2 O 3 diodes with intentionally grown 5 nm thin spinel-type NiGa 2 O 4 interfacial layers show an excellent device ON/OFF ratio of >10 10 (± 3 V), V ON of ~1.9 V, and increased breakdown voltage of ~1.2 kV for an initial unoptimized 300 lm diameter device. These p–n heterojunction diodes are promising for high-voltage, high temperature applications.

30 DIRECT ENERGY CONVERSION↗

Epitaxial growth of monolayer PdTe 2 and patterned PtTe 2 by direct tellurization of Pd and Pt surfaces

Two-dimensional (2D) palladium ditelluride (PdTe 2 ) and platinum ditelluride (PtTe 2 ) are two Dirac semimetals, which have fascinating quantum properties such as superconductivity, magnetism and topological order and show the promising applications in future nanoelectronics and optoelectronics. However, the synthesis of PdTe 2 and PtTe 2 monolayers (MLs) is hindered by a strong interlayer coupling and orbital hybridization. Here, in this study, we demonstrate an efficient synthesis of PdTe 2 and PtTe 2 MLs Large-area and high quality MLs of PdTe 2 and patterned PtTe 2 were epitaxially grown on the Pd(111) and Pt(111) surfaces by direct telurization in ultra-high vacuum. This was confirmed by x-ray photoelectron spectroscopy, low energy electron diffraction and scanning tunnelling microscopy. PdTe 2 ML demonstrated high thermal stability showing no decomposition sign after annealing at 470 °C. A well-ordered (2 × 2) PtTe 2 structure with Kagome lattice was observed on Te/Pt(111) surface following annealing at 200 °C in UHV, where the (2 × 2) pattern was formed by Te atom vacancies. PtTe 2 multilayer film was prepared as well, and it demonstrated the excitation of the Dirac plasmons as measured by high-resolution electron energy loss spectroscopy. The direct tellurization offers the simple and reliable protocol for the preparation of the ML of PdTe 2 and patterned PtTe 2 , and this opens new opportunities for quantum phenomena research and for practical optoelectronics applications.

2D materials↗

Growth of Mesoscale Ordered Two-Dimensional Hydrogen-Bond Organic Framework with the Observation of Flat Band

Flat bands (FBs), presenting a strongly interacting quantum system, have drawn increasing interest recently. However, experimental growth and synthesis of FB materials have been challenging and have remained elusive for the ideal form of monolayer materials where the FB arises from destructive quantum interference as predicted in 2D lattice models. Here, we report surface growth of a self-assembled monolayer of 2D hydrogen-bond (H-bond) organic frameworks (HOFs) of 1,3,5-tris(4-hydroxyphenyl)benzene (THPB) on Au(111) substrate and the observation of FB. High-resolution scanning tunneling microscopy or spectroscopy shows mesoscale, highly ordered, and uniform THPB HOF domains, while angle-resolved photoemission spectroscopy highlights a FB over the whole Brillouin zone. Density-functional-theory calculations and analyses reveal that the observed topological FB arises from a hidden electronic breathing-kagome lattice without atomically breathing bonds. In conclusion, our findings demonstrate that self-assembly of HOFs provides a viable approach for synthesis of 2D organic topological materials, paving the way to explore many-body quantum states of topological FBs.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Exploring the $A$-V-Sb landscape beyond $A$$\mathrm{V_3}$ $\mathrm{Sb_5}$: A case study on the $\mathrm{KV_6}$ $\mathrm{Sb_6}$ Kagome compound

Kagome compounds have garnered attention in the past few years for their intriguing magnetic properties arising from spin frustration dictated by the geometry of the Kagome sublattice. In this paper, we highlight the success of the unconventional hydride route for the fast and easy synthesis of the Kagome compound $\mathrm{KV_6}$ $\mathrm{Sb_6}$. Here, high-temperature in situ powder x-ray diffraction (PXRD) studies proved to be useful in hinting at the existence of $\mathrm{KV_6}$ $\mathrm{Sb_6}$, identifying its synthesis conditions, and understanding the reaction mechanism. The crystal structure for $\mathrm{KV_6}$ $\mathrm{Sb_6}$ was determined from high-resolution PXRD data. The compound has a layered structure [$R\overline{3}m, a = 5.5318$ (9) Å, $c = 34.23$ (3)Å 3 $Z = 3$] at room temperature] and features a Kagome bilayer of V atoms. $\mathrm{KV_6}$ $\mathrm{Sb_6}$ is isostructural to the previously reported $\mathrm{RbV_6}$ $\mathrm{Sb_6}$ and $\mathrm{CsV_6}$ $\mathrm{Sb_6}$ compounds. $\mathrm{KV_6}$ $\mathrm{Sb_6}$ is thermally stable in vacuum up to 1173 K, as evident from the high-temperature in situ PXRD and differential scanning calorimetric analysis. Investigation of magnetic properties for $\mathrm{KV_6}$ $\mathrm{Sb_6}$ between 2 and 300 K reveals temperature-independent paramagnetism and an absence of superconductivity, like the Rb and Cs analogs. Furthermore, we compare the magnetic properties of K V 3 Sb 5 , another ternary Kagome compound, synthesized via two different methods: the hydride route and the traditional route from elements. Low-temperature transport property measurements of $\mathrm{KV_6}$ $\mathrm{Sb_6}$ indicate metallic behavior and an intrinsically low thermal conductivity of $\mathrm{1.0 W K^-1}$ $\mathrm{m^-1}$ at 300 K. The layered structure of $\mathrm{KV_6}$ $\mathrm{Sb_6}$ makes it an attractive candidate for deintercalation and doping studies to tune both magnetic and transport properties, laying a foundation for further studies.

36 MATERIALS SCIENCE↗

High-resolution chemical patterns from negative tone resists for the integration of extreme ultraviolet patterns of metal-oxide resists with directed self-assembly of block copolymers

Extreme ultraviolet (EUV) lithography faces significant challenges in designing suitable resist materials that can provide adequate precision, while maintaining economically viable throughput. These challenges in resist materials have led to printing failures and high roughness in EUV patterns, compromising the performance of semiconductor devices. Integrating directed self-assembly (DSA) of block copolymers (BCPs) with EUV lithography offers a promising solution because, while the BCPs register to the EUV-defined chemical guiding pattern, the thermodynamically determined structures of the BCPs automatically rectify defects and roughness in the EUV pattern. Despite the superior resolution of metal-oxide EUV resists (MORs), their application to DSA is limited by the difficulty in converting them into chemical patterns that allow effective transfer of the rectified patterns of DSA films into inorganic materials. To address this challenge, this study introduces a novel strategy for fabricating chemical patterns using hydrogen silsesquioxane (HSQ), a high-resolution negative tone inorganic resist, as a model system for MORs. Initially, a sacrificial Cr pattern is generated from HSQ patterns via reactive ion etching. The sacrificial Cr pattern is converted into a chemical pattern by first grafting a water-soluble polyethylene oxide brush onto the substrate, then wet etching the Cr, and finally grafting nonpolar polystyrene brushes. Assembling polystyrene-block-poly(methyl methacrylate) on these patterns results in structures oriented and registered with the underlying pattern, achieving 24 nm full-pitch resolutions. In conclusion, this approach has the potential to integrate MOR patterns into the DSA process, thereby enabling the generation of high-quality sub-10 nm patterns with high-χ BCPs.

Atomic force microscopy↗

High-resolution magnetic microscopy applications using nitrogen-vacancy centers in diamond

Magnetic microscopy with high spatial resolution helps to solve a variety of technical problems in condensed-matter physics, electrical engineering, biomagnetism, and geomagnetism. In this work we used quantum diamond magnetic microscope (QDMM) setups, which use a dense uniform layer of magnetically-sensitive nitrogen-vacancy (NV) centers in diamond to image an external magnetic field using a fluorescence microscope. We used this technique for imaging few-micron ferromagnetic needles used as a physically unclonable function (PUF) and to passively interrogate electric current paths in a commercial 555 timer integrated circuit (IC). As part of the QDMM development, we also found a way to calculate ion implantation recipes to create diamond samples with dense uniform NV layers at the surface. This work opens the possibility for follow-up experiments with 2D magnetic materials, ion implantation, and electronics characterization and troubleshooting.

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↗

Quantitative Modeling of High-Energy Electron Scattering in Thick Samples Using Monte Carlo Techniques

Cryo-electron microscopy (cryo-EM) is a powerful tool for imaging biological samples but is typically limited by sample thickness, which is restricted to a few hundred nanometers depending on the electron energy. However, there is a growing need for imaging techniques capable of studying biological samples up to 10 µm in thickness while maintaining nanoscale resolution. This need motivates the use of mega-electron-volt scanning transmission electron microscopy (MeV-STEM), which leverages the high penetration power of MeV electrons to generate high-resolution images of thicker samples. In this study, we employ Monte Carlo simulations to model electron–sample interactions and explore the signal decay of imaging electrons through thick specimens. By incorporating material properties, interaction cross-sections for energy loss, and experimental parameters, we investigate the relationship between the incident and transmitted beam intensities. Key factors such as detector collection angle, convergence semi-angle, and the material properties of samples were analyzed. Our results demonstrate that the relationship between incident and transmitted beam intensities follows the Beer–Lambert law over thicknesses ranging from a few microns to several tens of microns, depending on material composition, electron energy, and collection angles. The linear depth of silicon dioxide reaches 3.9 µm at 3 MeV, about 6 times higher than that at 300 keV. Meanwhile, the linear depth of amorphous ice reaches 17.9 µm at 3 MeV, approximately 11.5 times higher than that at 300 keV. These findings are crucial for advancing the study of thick biological and semiconductor samples using MeV-STEM.

36 MATERIALS SCIENCE↗