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Results for “transition electron microscopy”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Inherent stochasticity during insulator–metal transition in VO 2

Vanadium dioxide (VO 2 ), which exhibits a near-room-temperature insulator–metal transition, has great potential in applications of neuromorphic computing devices. Although its volatile switching property, which could emulate neuron spiking, has been studied widely, nanoscale studies of the structural stochasticity across the phase transition are still lacking. In this study, using in situ transmission electron microscopy and ex situ resistive switching measurement, we successfully characterized the structural phase transition between monoclinic and rutile VO 2 at local areas in planar VO 2 /TiO 2 device configuration under external biasing. After each resistive switching, different VO 2 monoclinic crystal orientations are observed, forming different equilibrium states. We have evaluated a statistical cycle-to-cycle variation, demonstrated a stochastic nature of the volatile resistive switching, and presented an approach to study in-plane structural anisotropy. Furthermore, our microscopic studies move a big step forward toward understanding the volatile switching mechanisms and the related applications of VO 2 as the key material of neuromorphic computing.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Nematic transition and nanoscale suppression of superconductivity in Fe(Te,Se)

The interplay of different electronic phases underlies the physics of unconventional superconductors. One of the most intriguing examples is a high-temperature superconductor, FeTe 1 – x Se x . This superconductor undergoes both a topological transition, linked to the electronic band inversion, and an electronic nematic phase transition, associated with rotation symmetry breaking, around the same Se composition where the superconducting transition temperature peaks. In this regime, nematic fluctuations and symmetry-breaking strain could be important, but this is yet to be fully explored. Using spectroscopic-imaging scanning tunnelling microscopy, we study the electronic nematic transition in FeTe 1 – x Se x as a function of composition. Near the critical Se composition, we find electronic nematicity in nanoscale regions. The superconducting coherence peaks are suppressed in areas where static nematic order is the strongest. By analysing atomic displacement in scanning tunnelling microscopy topographs, we find that small anisotropic strain can give rise to these strongly nematic localized regions. Furthermore, our experiments reveal a tendency of FeTe 1 – x Se x , near x ≈ 0.45, to form puddles hosting static nematic order, suggestive of nematic fluctuations pinned by structural inhomogeneity, and demonstrate the effect of anisotropic strain on superconductivity in this regime.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1971

Electron microscopy and diffraction of layered, superconducting intercalation complexes.

Several layered, transition metal dichalcogenide intercalation complexes with unique superconducting properties have been examined by high-resolution electron microscopy and electron diffraction. Details of the crystalline lattice and of the lattice imperfections have been directly resolved. The results can be correlated with the available X-ray diffraction and chemical data, and they confirm and extend the postulated models.

Fernandez-Moran, H.↗
DOE OSTI2024

Voltage-induced magnetic domain evolution in a phase-change material

Applying voltage to metal–insulator transition (MIT) materials allows electrical actuation of the local electronic phase state. In MIT systems that have the electronic order coupled with the magnetic order, voltage switching of the electronic phase state can also enable the electrical manipulation of magnetic properties. In this work, we utilized x-ray magnetic circular dichroism photoemission electron microscopy (XMCD-PEEM) to investigate the control of magnetic domain configurations in ferromagnetic MIT electrical switches. For applied voltages above a threshold value, the XMCD-PEEM images show that the magnetic domains separate into two distinct regions: one with a high contrast (white/black), indicating well-defined micrometer-scale magnetic domains with a component of their magnetization aligned parallel/antiparallel to the x-ray helicity, and the other with different shades of intermediate contrast (gray). Significant changes in magnetic domain configurations upon voltage biasing were only observed in these gray regions. Furthermore, the voltage-induced magnetic domain separation was found to be bias polarity-dependent, with the gray regions expanding from the opposite sample edge when the applied voltage polarity was reversed. This polarity-dependent electrical control of magnetic domain configurations during the MIT switching opens alternative opportunities in memory applications for magnetic MIT switching materials.

42 ENGINEERING↗
DOE OSTI2022

Strength of tantalum to 276 GPa determined by two x-ray diffraction techniques using diamond anvil cells

Tantalum (Ta) is a metal that has useful properties that make it useful in extreme environments. It is therefore important to understand how Ta performs in such extreme conditions by accurately measuring its properties. In this work, the yield strength of tantalum has been measured at pressures up to 276 GPa using axial and radial x-ray diffraction (XRD) methods in diamond anvil cells (DAC). We measured strength using XRD in a radial DAC to 50 GPa, in an axial DAC to 60 GPa using diamonds with standard flat culets, and in a final experiment to 276 GPa using toroidal diamond anvils. The radial XRD data were refined using the Material Analysis Using Diffraction (MAUD) Rietveld software package to extract lattice strain and the yield strength. The axial data were refined using the General Structure Analysis System (GSAS) II and a linewidth method was used to calculate the yield strength. The yield strength measured near ambient pressure was found to be 0.5 GPa and increased with pressure up to 50 GPa, where the yield strength plateaued at a value of 2.4 GPa. At pressures above 60 GPa, the strength increased again to a maximum value of 9 GPa at the highest pressure of 276 GPa. Here, the data from the three experiments show good agreement between the methods and previously reported experimental data. This agreement illustrates the value of axial diffraction data for material strength determination and allows for measurements at multihundreds of GPa using toroidal DACs.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Resolving complex intralayer transition motifs in high-Ni-content layered cathode materials for lithium-ion batteries

High-Ni-content layered materials are promising cathodes for next-generation lithium-ion batteries. However, investigating the atomic configurations of the delithiation-induced complex phase boundaries and their transitions remains challenging. Here, in this study, by using deep-learning-aided super-resolution electron microscopy, we resolve the intralayer transition motifs at complex phase boundaries in high-Ni cathodes. We reveal that an O3 → O1 transformation driven by delithiation leads to the formation of two types of O1–O3 interface, the continuous- and abrupt-transition interfaces. The interfacial misfit is accommodated by a continuous shear-transition zone and an abrupt structural unit, respectively. Atomic-scale simulations show that uneven in-plane Li+ distribution contributes to the formation of both types of interface, and the abrupt transition is energetically more favourable in a delithiated state where O1 is dominant, or when there is an uneven in-plane Li + distribution in a delithiated O3 lattice. Moreover, a twin-like motif that introduces structural units analogous to the abrupt-type O1–O3 interface is also uncovered. The structural transition motifs resolved in this study provide further understanding of shear-induced phase transformations and phase boundaries in high-Ni layered cathodes.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2021

A strain-driven thermotropic phase boundary in BaTiO 3 at room temperature by cycling compression

In BaTiO 3 single crystals, we observed a strain-driven phase transition from the tetragonal phase to the tetragonal-orthorhombic phase boundary which can be introduced by slow cycling compressions (a loading of up to 0.5 GPa, strain rate of 10 -4 s -1 , and 100 cycles) at room temperature. Different from the well-known tetragonal to cubic phase transition under stress (~2 GPa), it only takes place locally around bent 90° domain walls. The inhomogeneous local stress and electrical fields as well as the mobile point defect pinning effect contribute to the phase re-entrance. Through comparison experiments by in situ synchrotron x-ray diffraction, Raman scattering, and (scanning) transmission electron microscopy, we explored the phase transition mechanism. Based on that, we developed a mechanical method to obtain well-stabilized high-density thermotropic phase boundary structures (with tetragonal, orthorhombic, and bridging monoclinic phases) in BaTiO 3 for potential applications.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructural and phase changes in alpha uranium investigated via in-situ studies and molecular dynamics

A deeper knowledge of thermally induced microstructural and phase evolution in nuclear metallic fuel can be obtained using novel in-situ microscopic analyses. Such studies can provide information on the dynamics of phase transitions which is not possible with conventional postmortem characterization (post-irradiation examination). In this work, the behavior of alpha uranium (α-U) was investigated via in-situ heating tests in a transmission electron microscope. Here, the main objective is to understand the microstructural and phase changes, such as defect annihilation and ß phase formation and retention, observed in reactor in-pile transient studies at the Transient Reactor Test facility. Indeed, defect migration and rearrangement were observed within the α phase starting at 673 K; α→ß phase transition was observed between 773 K and 1,073 K during the heating ramp (which is in the temperature window reported for α→ß transition temperatures). Recrystallization and formation of nano grains was observed at high temperatures (over 1,073 K). Such recrystallization was possibly related to the formation of the γ phase. Finally, it was indeed observed that the ß phase (but not γ phase) was retained at room temperature upon rapid cooling. Molecular dynamics studies support these experimental results and shows that the γ phase of pure uranium cannot be retained at room temperature if not stabilized with the addition of an alloying element.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Spatial Mapping of Electrostatic Fields in 2D Heterostructures

In situ electron microscopy is an effective tool for understanding the mechanisms driving novel phenomena in 2D structures. However, due to practical challenges, it is difficult to address these technologically relevant 2D heterostructures with electron microscopy. Here, we use the differential phase contrast (DPC) imaging technique to build a methodology for probing local electrostatic fields during electrical operation with nanoscale spatial resolution in such materials. We find that, by combining a traditional DPC setup with a high-pass filter, we can largely eliminate electric fluctuations emanating from short-range atomic potentials. Using a method based on this filtering algorithm, a priori electric field expectations can be directly compared with experimentally derived values to readily identify inhomogeneities and potentially problematic regions. Furthermore, we use this platform to analyze the electric field and charge density distribution across layers of hBN and MoS 2 .

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2023

In Situ Imaging of an Anisotropic Layer-by-Layer Phase Transition in Few-Layer MoTe 2

Understanding the phase transition mechanisms in two-dimensional (2D) materials is a key to precisely tailor their properties at the nanoscale. Molybdenum ditelluride (MoTe 2 ) exhibits multiple phases at room temperature, making it a promising candidate for phase-change applications. Here, we fabricate lateral 2H–T d interfaces with laser irradiation and probe their phase transitions from micro- to atomic scales with in situ heating in the transmission electron microscope (TEM). By encapsulating the MoTe 2 with graphene protection layers, we create an in situ reaction cell compatible with atomic resolution imaging. We find that the T d -to-2H phase transition initiates at phase boundaries at low temperatures (200–225 °C) and propagates anisotropically along the b-axis in a layer-by-layer fashion. We also demonstrate a fully reversible 2H-T d -2H phase transition cycle, which generates a coherent 2H lattice containing inversion domain boundaries. Furthermore, our results provide insights on fabricating 2D heterophase devices with atomically sharp and coherent interfaces.

2D materials↗
DOE OSTI2024

LaFeSi–LaFe 13-x Si x composites: Modulating magnetic and magnetocaloric properties through inherent stress manipulation

We examine structural and magnetic properties of a series of La–Fe–Si alloys in the region of concentrations where they naturally form two-phase LaFeSi–LaFe 13-x Si x composites with variable content and connectivity of LaFe 13-x Si x grains distributed within the LaFeSi matrix. Theoretical calculations confirm that the LaFeSi constituent is magnetically and structurally inert below room temperature and at pressures between -10 and 10 GPa. The LaFe 13-x Si x constituent, on the other hand, is magnetically and structurally active: it exhibits first-order magnetostructural transformations that, in addition to x Si , can be controlled with temperature, magnetic field, and pressure. In composites where the concentration of the inactive constituent is ~70 wt. % or greater, the standard, single-step, LaFe 13-x Si x first-order phase transformation proceeds in two steps separated by over 30 K in a zero magnetic field. Increasing the magnetic field recouples the two steps and restores the single-step phase transformation pathway. We analyze the roles of stresses caused by both thermal expansion mismatch and the first-order magnetic phase transition in LaFe 13-x Si x to rationalize the observed physical behaviors that emerge as the temperature or/and magnetic field vary.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Dynamic response of 17-4 stainless steel as a function of manufacturing method and heat treatment

We present a series of plate-impact experiments on 17-4 stainless steel to study the effect of manufacturing method and heat treatment on the Hugoniot elastic limit (HEL), Hugoniot, phase transformation stress, and spallation strength. Two traditional manufacturing methods were considered, wrought processing and casting, as well as two additive manufacturing methods, laser powder-bed fusion (LPBF) and wire-fed electron beam (EBAM). For both LPBF and EBAM 17-4 stainless steel variants, two billets were printed, enabling the application of two unique heat treatments. The HEL stress depended heavily on the thermal history, with the HEL increasing after the formation of Cu-rich precipitates via heat treatment. The Hugoniot response both below and above the phase transition was unaffected by the manufacturing method or heat treatment. The phase transition stress depended heavily on the thermal history, with its variation being attributed to the presence of various microstructural features. This is supported by a marked increase in the phase transition stress after precipitation hardening. These results suggest that the notion of the phase transition stress being dictated by bulk composition is an oversimplification and the stress fields generated by the meso-scale structure are a dominant force. The spallation strength was lower in the cast material compared to all other 17-4 stainless steel variants due to the presence of brittle δ-ferrite inclusions. Additionally, a drop in the tensile strain-rate was observed in the spallation response above the phase transition stress, which was hypothesized to stem from the kinetics of the reversion to the low-pressure phase during spall.

Compressive stress↗
DOE OSTI2026

Dynamic compression and spallation behavior of NbTaTiVZr high-entropy alloy

High-entropy alloys are a new class of materials with promising properties for aerospace and defense applications. The unique behavior of these materials is driven by the complex interactions between dissimilar atoms in a crystal and requires combined theoretical and experimental efforts to unlock their full potential. Here, we evaluate the relationship between the microstructure and the dynamic response of the equiatomic NbTaTiVZr alloy. Specifically, the shock Hugoniot, or equation of state, was measured up to a particle velocity of 0.5 mm μs −1 using gas gun plate impacts. Shock wave profile and incipient spallation experiments were used to characterize wave propagation and damage formation with post-mortem recovery experiments. Molecular dynamics simulations confirm the experimental findings and extend them up to 2.1 mm μs −1 particle velocity. Computational thermodynamic calculation of phase diagram simulations explain details of the material microstructure, which explains the measured strength and experimental damage patterns. Overall, this work provides detailed high-strain-rate characterization of a refractory high-entropy alloy, and more importantly, a framework and demonstration of the utility and necessity of a combined theoretical and experimental approach, outlining the importance of considering processing and manufacturing conditions when evaluating the performance of new materials.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Time-resolved cryogenic electron tomography for the study of transient cellular processes

Cryogenic electron tomography (cryo-ET) is the highest resolution imaging technique applicable to the life sciences, enabling sub-nanometer visualization of specimens preserved in their near native states. The rapid plunge freezing process used to prepare samples lends itself to time-resolved studies, which researchers have pursued for in vitro samples for decades. Here, we focus on developing a freezing apparatus for time-resolved studies in situ. The device mixes cellular samples with solution-phase stimulants before spraying them directly onto an electron microscopy grid that is transiting into cryogenic liquid ethane. By varying the flow rates of cell and stimulant solutions within the device, we can control the reaction time from tens of milliseconds to over a second prior to freezing. In a proof-of-principle demonstration, the freezing method is applied to a model bacterium, Caulobacter crescentus, mixed with an acidic buffer. Through cryo-ET we resolved structural changes throughout the cell, including surface-layer protein dissolution, outer membrane deformation, and cytosolic rearrangement, all within 1.5 seconds of reaction time. This new approach, Time-Resolved cryo-ET (TR-cryo-ET), enhances the capabilities of cryo-ET by incorporating a sub-second temporal axis and enables the visualization of induced structural changes at the molecular, organelle, or cellular level.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2020

Direct Observations of Field-Intensity-Dependent Dielectric Breakdown Mechanisms in TiO 2 Single Nanocrystals

One of the main challenges for next-generation electric power systems and electronics is to avoid premature dielectric breakdown in insulators and capacitors and to ensure reliable operations at higher electric fields and higher efficiencies. However, dielectric breakdown is a complex phenomenon and often involves many different processes simultaneously. Here we show distinctly different defect-related and intrinsic breakdown processes by studying individual, single crystalline TiO 2 nanoparticles using in-situ transmission electron microscopy (TEM). As the applied electric field intensity rises, rutile-to-anatase phase transition, local amorphization/melting, or ablation are identified as the corresponding breakdown processes, the field intensity thresholds of which are found to be related to the position of the intensified field and the duration of the applied bias relative to the time of charged defects accumulation. Our observations reveal an intensity-dependent dielectric response of crystalline oxides at breakdown and suggest possible routes to suppress the iniation of premature dielectric breakdown. Hence, they will aid the design and development of next generation robust and efficient solid dielectrics.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Machine learning for automated experimentation in scanning transmission electron microscopy

Abstract Machine learning (ML) has become critical for post-acquisition data analysis in (scanning) transmission electron microscopy, (S)TEM, imaging and spectroscopy. An emerging trend is the transition to real-time analysis and closed-loop microscope operation. The effective use of ML in electron microscopy now requires the development of strategies for microscopy-centric experiment workflow design and optimization. Here, we discuss the associated challenges with the transition to active ML, including sequential data analysis and out-of-distribution drift effects, the requirements for edge operation, local and cloud data storage, and theory in the loop operations. Specifically, we discuss the relative contributions of human scientists and ML agents in the ideation, orchestration, and execution of experimental workflows, as well as the need to develop universal hyper languages that can apply across multiple platforms. These considerations will collectively inform the operationalization of ML in next-generation experimentation.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Nanoscale phase transition in impact indented Mo/Cu thin films

The study reveals a size effect in deformation mechanisms via unique structural transitions in sputter deposited fcc/bcc nanolayers under high strain rate impact nanoindentation as layer thickness is reduced from around 100-200 nm to around 5 nm. Here, the indented 5 nm Cu/5 nm Mo multilayer films characterized via cross-sectional scanning/transmission electron microscopy have revealed a phase transition in the 5 nm thick Mo layers from BCC to a coherent metastable FCC structure and fine deformation twins in the 5 nm Cu layers inside a shear band that is approximately 500 nm long and inclined to the layer interfaces. In contrast, thicker layers, 80 nm Cu/180 nm Mo, show different deformation behavior with uneven layer thickness reduction, shearing of Cu layers, and bending of the columnar Mo grains beneath the indentation without any sign of shear band and localized phase transformation.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Thermoresponsive polymer assemblies via variable temperature liquid-phase transmission electron microscopy and small angle X-ray scattering

Abstract Herein, phase transitions of a class of thermally-responsive polymers, namely a homopolymer, diblock, and triblock copolymer, were studied to gain mechanistic insight into nanoscale assembly dynamics via variable temperature liquid-cell transmission electron microscopy (VT-LCTEM) correlated with variable temperature small angle X-ray scattering (VT-SAXS). We study thermoresponsive poly(diethylene glycol methyl ether methacrylate) (PDEGMA)-based block copolymers and mitigate sample damage by screening electron flux and solvent conditions during LCTEM and by evaluating polymer survival via post-mortem matrix-assisted laser desorption/ionization imaging mass spectrometry (MALDI-IMS). Our multimodal approach, utilizing VT-LCTEM with MS validation and VT-SAXS, is generalizable across polymeric systems and can be used to directly image solvated nanoscale structures and thermally-induced transitions. Our strategy of correlating VT-SAXS with VT-LCTEM provided direct insight into transient nanoscale intermediates formed during the thermally-triggered morphological transformation of a PDEGMA-based triblock. Notably, we observed the temperature-triggered formation and slow relaxation of core-shell particles with complex microphase separation in the core by both VT-SAXS and VT-LCTEM.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗