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Michele Conroy

Publications and source records attributed to Michele Conroy.

10 recordsLinked to original sources

Predictive drift compensation of multi-frame STEM via live scan modification

Scanning transmission electron microscopy (STEM) is widely used tool for materials characterisation. However, being a scanned technique, STEM is susceptible to sample, stage or beam drift, manifesting as distortions within images or movement in the field-of-view during multi-frame imaging. Often this is corrected post-acquisition using image registration of multiple frames, but drift reduces the usable area common to all frames. Here we present a method to mitigate sample drift by analysing past frames to predict the sampling-grid points for the immediately future frame. We present this correction across two time-scales and two lengthscales. By offsetting the scan-grid framewise we remove long-range drift, and offsetting pixelwise we minimise intra-image warping. Examples are presented for both atomic-resolution imaging and lower-magnification in-situ video capture. The framework is general to raster, serpentine, interlaced and other scan patterns, as well as sequential or scan-rotation series STEM.

physics.ins-det

Tailoring Ultrathin Magnetic Multilayers at Terraced Topologically Insulating Interfaces for Perpendicularly Magnetized Domains

Topological insulators and skyrmion-hosting, chiral magnetic multilayers are two well-explored areas of modern condensed matter physics, each offering unique advantages for spintronics applications. In this paper, we demonstrate the optimization process for the growth of a Bi$_2$Se$_3$/buffer/[Pt/CoB/Ru]$_{\times N}$ heterostructure that combines these two material classes: the Bi$_2$Se$_3$ epilayer was grown by molecular beam epitaxy before transfer under ultrahigh vacuum to a separate growth chamber where the polycrystalline metallic multilayer was sputter deposited. The structure of the samples was characterized by co-fitted X-ray and polarized neutron reflectometry measurements and scanning transmission electron microscopy. Polarized neutron models and standard magnetometry show that a buffer layer exceeding a critical thickness is required to obtain the desired uniform, perpendicular magnetic anisotropy in every magnetic layer in the multilayer. Samples with both Ta and Mo buffers were used requiring thicknesses of 1.5 and 0.9 nm respectively. In minimizing the Bi$_2$Se$_3$ terracing, buffered samples yield well-defined, out-of-plane, magnetic domains suitable for spin-orbit torque induced manipulation as determined by X-ray photoemission electron microscopy.

cond-mat.mtrl-sci

Look What You Made Me Glue: SEMGluTM Enabled Alternative Cryogenic Sample Preparation Process for Cryogenic Atom Probe Tomography Studies

Extensive efforts over the past number of years have been applied to develop workflows for sample preparation of specimens for atom probe tomography at cryogenic temperatures. This is primarily due to the difficulty involved in preparing site specific lift out samples at cryogenic temperatures without the assistance of the gas injection system (GIS) as using it under cryogenic conditions leads to nonuniform and difficult to control deposition. Building on the efforts of previously developed GIS free workflows utilising redeposition techniques, this work provides an alternative approach using SEMGluTM, which is an electron beam curing adhesive that remains usable at cryogenic temperatures, to both lift out cryogenically frozen samples, and mount these samples to Si microarray posts for subsequent redeposition welding. This approach is applicable for a full cryogenic workflow but is particularly useful for non-fully cryogenic workflows such as beam sensitive samples, samples that mill easily, and samples with challenging geometries. We demonstrate atom probe analysis of silicon samples in both laser pulsing and voltage mode prepared using this workflow, with comparable analytical performance to a pre-sharpened microtip coupon. An application-based example which directly benefits from this approach, correlative Liquid Cell Transmission Electron Microscopy and cryogenic Atom Probe Tomography sample preparation, is also shown.

cond-mat.mtrl-sci

Spatially resolving superconductivity in type-II superconductors

Superconductivity is identified by the emergence of a macroscopic zero-resistance state, typically inferred from a vanishing four-probe voltage at finite current. That inference assumes spatially uniform conduction-e.g., at least one continuous superconducting path between the current leads and voltage electrodes that sample a finite potential gradient-and can fail if the drive current bypasses the electrodes or if narrow filaments short the current contacts. Here we introduce a methodology to test these assumptions in superconductors, by using spatially resolved measurements of local variations in dc using cryogenic conductive atomic-force microscopy (cAFM). Using Fe(Se,Te) as a model system, we find that despite bulk measurements consistent with a homogeneous superconducting state, the material exhibits a heterogeneous conducting landscape: micrometre-scale superconducting regions coexist with relatively insulating areas. We further show that cAFM resolves conductance fluctuations at 20 K (> TC) that vary between repeated scans, consistent with expectations for short-lived, pre-formed Cooper pairs in the BCS-BEC crossover regime. These results establish cAFM as a practical tool to validate assumptions underlying four-probe transport and underscore the need for direct spatial probes in materials whose macroscopic response can conceal nanoscale inhomogeneity. Accurate identification of macroscopic properties is critical for materials classes like superconductors that are defined by their macroscopic properties.

cond-mat.supr-con

Observation of Antiferroelectric Domain Walls in a Uniaxial Hyperferroelectric

Ferroelectric domain walls are a rich source of emergent electronic properties and unusual polar order. Recent studies showed that the configuration of ferroelectric walls can go well beyond the conventional Ising-type structure. Néel-, Bloch-, and vortex-like polar patterns have been observed, displaying strong similarities with the spin textures at magnetic domain walls. Here, we report the discovery of antiferroelectric domain walls in the uniaxial ferroelectric Pb$_{5}$Ge$_{3}$O$_{11}$. We resolve highly mobile domain walls with an alternating displacement of Pb atoms, resulting in a cyclic 180$^{\circ}$ flip of dipole direction within the wall. Density functional theory calculations reveal that Pb$_{5}$Ge$_{3}$O$_{11}$ is hyperferroelectric, allowing the system to overcome the depolarization fields that usually suppress antiparallel ordering of dipoles along the longitudinal direction. Interestingly, the antiferroelectric walls observed under the electron beam are energetically more costly than basic head-to-head or tail-to-tail walls. The results suggest a new type of excited domain-wall state, expanding previous studies on ferroelectric domain walls into the realm of antiferroic phenomena.

cond-mat.mtrl-sci

Atom probe analysis of BaTiO3 enabled by metallic shielding

Atom probe tomography has been raising in prominence as a microscopy and microanalysis technique to gain sub-nanoscale information from technologically-relevant materials. However, the analysis of some functional ceramics, particularly perovskites, has remained challenging with extremely low yield and success rate. This seems particularly problematic for materials with high piezoelectric activity, which may be difficult to express at the low temperatures necessary for satisfactory atom probe analysis. Here, we demonstrate the analysis of commercial BaTiO3 particles embedded in a metallic matrix. Density-functional theory shows that a metallic coating prevents charge penetration of the electrostatic field, and thereby suppresses the associated volume associated change linked to the piezoelectric effect.

cond-mat.mtrl-sci

In-situ sputtering from the micromanipulator to enable cryogenic preparation of specimens for atom probe tomography by focused-ion beam

Workflows have been developed in the past decade to enable atom probe tomography analysis at cryogenic temperatures. The inability to control the local deposition of the metallic precursor from the gas-injection system (GIS) at cryogenic temperature makes the preparation of site-specific specimens by using lift-out extremely challenging in the focused-ion beam. Schreiber et al. exploited redeposition to weld the lifted-out sample to a support. Here we build on their approach to attach the region-of-interest and additionally strengthen the interface with locally sputtered metal from the micromanipulator. Following standard focused-ion beam annular milling, we demonstrate atom probe analysis of Si in both laser pulsing and voltage mode, with comparable analytical performance as a pre-sharpened microtip coupon. Our welding approach is versatile, as various metals could be used for sputtering, and allows similar flexibility as the GIS in principle.

cond-mat.mtrl-sci

Ultra-High Carrier Mobilities in Ferroelectric Domain Wall Corbino Cones at Room Temperature

Recently, electrically conducting heterointerfaces between dissimilar band-insulators (such as lanthanum aluminate and strontium titanate) have attracted considerable research interest. Charge transport has been thoroughly explored and fundamental aspects of conduction firmly established. Perhaps surprisingly, similar insights into conceptually much simpler conducting homointerfaces, such as the domain walls that separate regions of different orientations of electrical polarisation within the same ferroelectric band-insulator, are not nearly so well-developed. Addressing this disparity, we herein report magnetoresistance in approximately conical 180o charged domain walls, which occur in partially switched ferroelectric thin film single crystal lithium niobate. This system is ideal for such measurements: firstly, the conductivity difference between domains and domain walls is extremely and unusually large (a factor of at least 1013) and hence currents driven through the thin film, between planar top and bottom electrodes, are overwhelmingly channelled along the walls; secondly, when electrical contact is made to the top and bottom of the domain walls and a magnetic field is applied along their cone axes (perpendicular to the thin film surface), then the test geometry mirrors that of a Corbino disc, which is a textbook arrangement for geometric magnetoresistance measurement. Our data imply carriers at the domain walls with extremely high room temperature Hall mobilities of up to ~ 3,700cm2V-1s-1. This is an unparalleled value for oxide interfaces (and for bulk oxides too) and is most comparable to mobilities in other systems typically seen at cryogenic, rather than at room, temperature.

cond-mat.mtrl-sci

Atom probe analysis of battery materials: challenges and ways forward

The worldwide developments of electric vehicles, as well as large-scale or grid-scale energy storage to compensate the intermittent nature of renewable energy generation has generated a surge of interest in battery technology. Understanding the factors controlling battery capacity and, critically, their degradation mechanisms to ensure long-term, sustainable and safe operation requires detailed knowledge of their microstructure and chemistry, and their evolution under operating conditions, on the nanoscale. Atom probe tomography (APT) provides compositional mapping of materials in three-dimensions with sub-nanometre resolution, and is poised to play a key role in battery research. However, APT is underpinned by an intense electric-field that can drive lithium migration, and many battery materials are reactive oxides, requiring careful handling and sample transfer. Here, we report on the analysis of both anode and cathode materials, and show that electric-field driven migration can be suppressed by using shielding by embedding powder particles in a metallic matrix or by using a thin conducting surface layer. We demonstrate that for a typical cathode material, cryogenic specimen preparation and transport under ultra-high vacuum leads to major delithiation of the specimen during the analysis. In contrast, transport of specimens through air enables analysis of the material. Finally, we discuss the possible physical underpinnings and discuss ways forward to enable shield of the electric field, which helps address the challenges inherent to the APT analysis of battery materials.

cond-mat.mtrl-sci

TopoTEM: A Python Package for Quantifying and Visualising Scanning Transmission Electron Microscopy Data of Polar Topologies

The exotic internal structure of polar topologies in multi-ferroic materials offers a rich landscape for materials science research. As the spatial scale of these entities are often sub-atomic in nature, aberration corrected transmission electron microscopy (TEM) is the ideal characterisation technique. Software to quantify and visualise the slight shifts in atomic placement within unit cells is of paramount importance due to the now routine acquisition of images at such resolution. In the previous ~decade since the commercialisation of aberration corrected TEM, many research groups have written their own code to visualise these polar entities. More recently, open access Python packages have been developed for the purpose of TEM atomic position quantification. Building on these packages, we introduce the TEMUL Toolkit: a Python package for analysis and visualisation of atomic resolution images. Here, we focus specifically on the TopoTEM module of the toolkit where we show an easy to follow, streamlined version of calculating the atomic displacements relative to the surrounding lattice and thus polarisation plotting. We hope this toolkit will benefit the rapidly expanding field of topology based nano-electronic and quantum materials research, and we invite the electron microscopy community to contribute to this open access project.

cond-mat.mtrl-sci