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The use of fast pixelated detectors and direct electron detection technology is revolutionising many aspects of scanning transmission electron microscopy (STEM). The widespread adoption of these new technologies is impeded by the technical challenges associated with them. These include issues related to hardware control, and the acquisition, real-time processing and visualisation, and storage of data from such detectors. We discuss these problems and present software solutions for them, with a view to making the benefits of new detectors in the context of STEM more accessible. Throughout, we provide examples of the application of the technologies presented, using data from a Medipix3 direct electron detector. Most of our software is available under an open source licence, permitting transparency of the implemented algorithms, and allowing the community to freely use and further improve upon them., 16 pages, 7 figures, post revision

Magnetic skyrmions are topological magnetic spin structures exhibiting particle-like behaviour. They are of strong interest from a fundamental viewpoint and for application, where they have potential to act as information carriers in future low-power computing technologies. Importantly, skyrmions have high physical stability because of topological protection. However, they have potential to deform according to their local energy environment. Here we demonstrate that, in regions of high exchange energy density, skyrmions may exhibit such extreme deformation that spontaneous merging with nearest neighbours or spawning new skyrmions is favoured to attain a lower energy state. Using transmission electron microscopy and a high-speed imaging detector, we observe dynamics involving distinct configurational states, in which transitions are accompanied by spontaneous creation or annihilation of skyrmions. These observations raise important questions regarding the limits of skyrmion stability and topological charge conservation, while also suggesting a means of control of skyrmion creation and annihilation., 19 pages total. 4 figures at the end of the main text, supplementary material follows

The growth of cobalt nanopatterns (NPs) using focused electron-beam induced deposition (FEBID) for localised magnetic studies is presented. The initial FEBID products are shown to be polycrystalline and form hetero-structured core-shell NPs through surface oxidation. Off-axis electron holography is performed to reconstruct their morphology, thickness profile and image their individual magnetic vortex domain states. In situ annealing to 400°C promoted migration of the Co-overspray to grow the Co NPs and improved their crystallinity through coarsening, as well as induced diffusion of embedded carbon out of their surface. It is found that the change in their morphology and chemical instability under heating restricts their suitability for examining thermally induced magnetic variations. LAY DESCRIPTION: In this paper, electron microscopy is used to deposit magnetic cobalt nanopatterns and characterise the effect of in-situ heating on their chemistry, structure and magnetic properties. The electron beam of the secondary electron microscope is used to dissociate an injected precursor gas near the SiN membrane substrate of in-situ transmission electron microscopy (TEM) chips and locally deposit the elemental Co in circular patterns ∼ 90 nm in diameter. TEM reveals formation of a Co-oxide shell and embedding of carbon from the precursor gas during growth. The technique of electron holography is used to image the magnetism of the core-shell Co / Co-oxide nanopatterns, which are shown to exhibit magnetic vortex states. In-situ annealing results in migration of the Co overspray to increase their height and carbon diffusion from their surface, as well as change in their original magnetic state through change of orientation. It is found that the change in the morphology and chemistry of Co nanopatterns under heating limits their use for studying the effect of temperature on their magnetism in isolation.

It is shown that higher order Laue zone (HOLZ) rings in high energy electron diffraction are specific to individual columns of atoms, and show different strengths, structure and radii for different atom columns along the same projection in a structure. An atomic resolution 4-dimensional STEM dataset is recorded from a direction in a perovskite trilayer, where only the central LaFeO3 layer should show a period doubling that gives rise to an extra HOLZ ring. Careful comparison between experiment and multislice simulations is used to understand the origins of all features in the patterns. A strong HOLZ ring is seen for the La-O columns, indicating strong La position modulation along this direction, whereas a weaker ring is seen along the O columns, and a very weak ring is seen along the Fe columns. This demonstrates that atomic resolution HOLZ-STEM is a feasible method for investigating the 3D periodicity of crystalline materials with atomic resolution.

Equiatomic FeRh alloys undergo a fascinating first-order metamagnetic phase transition (FOMPT) just above room temperature, which has attracted reinvigorated interest for applications in spintronics. Until now, all attempts to grow nanothin FeRh alloy films have consistently shown that FeRh layers tend to grow in the Volmer-Weber growth mode. Here we show that sputter-grown sub-15-nm-thick FeRh alloy films deposited at low sputter-gas pressure, typically ∼0.1 Pa, onto (001)-oriented MgO substrates, grow in a peening-induced Frank-van der Merwe growth mode for FeRh film thicknesses above 5 nm, circumventing this major drawback. The bombardment of high-energy sputtered atoms, the atom-peening effect, induces a rebalancing between adsorbate-surface and adsorbate-adsorbate interactions, leading to the formation of a smooth continuous nanothin FeRh film. Chemical order in the films increases with the FeRh thickness, tFeRh, and varies monotonically from 0.75 up to 0.9. Specular x-ray diffraction scans around Bragg peaks show Pendellösung fringes for films with tFeRh≥5.2 nm, which reflects in smooth well-ordered densified single-crystal FeRh layers. The nanothin film's roughness varies from 0.6 down to about 0.1 nm as tFeRh increases, and scales linearly with the integral breadth of the rocking curve, proving its microstructured origin. Magnetometry shows that the FOMPT in the nanothin films is qualitatively similar to that of the bulk alloy, except for the thinnest film of 3.7 nm.

A scanning precession electron diffraction system has been integrated with a direct electron detector to allow the collection of improved quality diffraction patterns. This has been used on a two-phase α–β titanium alloy (Timetal® 575) for phase and orientation mapping using an existing pattern-matching algorithm and has been compared to the commonly used detector system, which consisted of a high-speed video-camera imaging the small phosphor focusing screen. Noise is appreciably lower with the direct electron detector, and this is especially noticeable further from the diffraction pattern center where the real electron scattering is reduced and both diffraction spots and inelastic scattering between spots are weaker. The results for orientation mapping are a significant improvement in phase and orientation indexing reliability, especially of fine nanoscale laths of α-Ti, where the weak diffracted signal is rather lost in the noise for the optically coupled camera. This was done at a dose of ~19 e−/Å2, and there is clearly a prospect for reducing the current further while still producing indexable patterns. This opens the way for precession diffraction phase and orientation mapping of radiation-sensitive crystalline materials.

Fast pixelated detectors incorporating direct electron detection (DED) technology are increasingly being regarded as universal detectors for scanning transmission electron microscopy (STEM), capable of imaging under multiple modes of operation. However, several issues remain around the post acquisition processing and visualisation of the often very large multidimensional STEM datasets produced by them. We discuss these issues and present open source software libraries to enable efficient processing and visualisation of such datasets. Throughout, we provide examples of the analysis methodologies presented, utilising data from a 256$\times$256 pixel Medipix3 hybrid DED detector, with a particular focus on the STEM characterisation of the structural properties of materials. These include the techniques of virtual detector imaging; higher order Laue zone analysis; nanobeam electron diffraction; and scanning precession electron diffraction. In the latter, we demonstrate nanoscale lattice parameter mapping with a fractional precision $\le 6\times10^{-4}$ (0.06%)., 23 pages, 12 figures, add open data zenodo doi and revise precision discussion

Detector developments are currently enabling new capabilities in the field of transmission electron microscopy (TEM). We have investigated the limits of a hybrid pixel detector, Medipix3, to record dynamic, time varying, electron signals. Operating with an energy of 60keV, we have utilised electrostatic deflection to oscillate electron beam position on the detector. Adopting a pump-probe imaging strategy we have demonstrated that temporal resolutions three orders of magnitude smaller than are available for typically used TEM imaging detectors are possible. Our experiments have shown that energy deposition of the primary electrons in the hybrid pixel detector limits the overall temporal resolution. Through adjustment of user specifiable thresholds or the use of charge summing mode, we have obtained images composed from summing 10,000s frames containing single electron events to achieve temporal resolution less than 100ns. We propose that this capability can be directly applied to studying repeatable material dynamic processes but also to implement low-dose imaging schemes in scanning transmission electron microscopy., Comment: 11 pages, 6 figures; improve ref formatting + revise text

The phase coexistence present through a first-order phase transition means there will be finite regions between the two phases where the structure of the system will vary from one phase to the other, known as a phase boundary wall. This region is said to play an important but unknown role in the dynamics of the first-order phase transitions. Here, by using both x-ray photon correlation spectroscopy and magnetometry techniques to measure the temporal isothermal development at various points through the thermally activated first-order metamagnetic phase transition present in the near-equiatomic FeRh alloy, we are able to isolate the dynamic behavior of the domain walls in this system. These investigations reveal that relaxation behavior of the domain walls changes when phase coexistence is introduced into the system and that the domain wall dynamics is different to the macroscale behavior. We attribute this to the effect of the exchange coupling between regions of either magnetic phase changing the dynamic properties of domain walls relative to bulk regions of either phase. We also believe this behavior comes from the influence of the phase boundary wall on other magnetic objects in the system., Main Paper: 13 pages, 8 figures. Supplementary information: 13 pages, 8 figures

Light–electron interaction is the seminal ingredient in free-electron lasers and dynamical investigation of matter. Pushing the coherent control of electrons by light to the attosecond timescale and below would enable unprecedented applications in quantum circuits and exploration of electronic motions and nuclear phenomena. Here we demonstrate attosecond coherent manipulation of a free-electron wave function, and show that it can be pushed down to the zeptosecond regime. We make a relativistic single-electron wavepacket interact in free-space with a semi-infinite light field generated by two light pulses reflected from a mirror and delayed by fractions of the optical cycle. The amplitude and phase of the resulting electron–state coherent oscillations are mapped in energy-momentum space via momentum-resolved ultrafast electron spectroscopy. The experimental results are in full agreement with our analytical theory, which predicts access to the zeptosecond timescale by adopting semi-infinite X-ray pulses., Manipulation of the electron–photon coupling is crucial for quantum circuits and exploration of electronic motions and nuclear phenomena. Here the authors discuss a scheme to coherently control the electron wave function from attosecond to zeptosecond timescales by using semi-infinite light fields.

Hybrid pixel detectors (HPDs) have been shown to be highly effective for diffraction-based and time-resolved studies in transmission electron microscopy, but their performance is limited by the fact that high-energy electrons scatter over long distances in their thick Si sensors. An advantage of HPDs compared to monolithic active pixel sensors (MAPS) is that their sensor does not need to be fabricated from Si. We have compared the performance of the Medipix3 HPD with a Si sensor and with a GaAs:Cr sensor using primary electrons in the energy range of 60 - 300keV. We describe the measurement and calculation of the detectors' modulation transfer function (MTF) and detective quantum efficiency (DQE), which show that the performance of the GaAs:Cr device is markedly superior to that of the Si device for high-energy electrons., Comment: 15 pages + references, 13 figures

No abstract available.

Determining the three-dimensional (3D) crystallography of a material with subnanometer resolution is essential to understanding strain effects in epitaxial thin films. A scanning transmission electron microscopy imaging technique is demonstrated that visualizes the presence and strength of atomic movements leading to a period doubling of the unit cell along the beam direction, using the intensity in an extra Laue zone ring in the back focal plane recorded using a pixelated detector method. This method is used together with conventional atomic resolution imaging in the plane perpendicular to the beam direction to gain information about the 3D crystal structure in an epitaxial thin film of LaFeO3 sandwiched between a substrate of (111) SrTiO3 and a top layer of La0.7Sr0.3MnO3. It is found that a hitherto unreported structure of LaFeO3 is formed under the unusual combination of compressive strain and (111) growth, which is triclinic with a periodicity doubling from primitive perovskite along one of the three ⟨110⟩ directions lying in the growth plane. This results from a combination of La-site modulation along the beam direction, and modulation of oxygen positions resulting from octahedral tilting. This transition to the period-doubled cell is suppressed near both the substrate and near the La0.7Sr0.3MnO3 top layer due to the clamping of the octahedral tilting by the absence of tilting in the substrate and due to an incompatible tilt pattern being present in the La0.7Sr0.3MnO3 layer. This work shows a rapid and easy way of scanning for such transitions in thin films or other systems where disorder-order transitions or domain structures may be present and does not require the use of atomic resolution imaging, and could be done on any scanning transmission electron microscopy instrument equipped with a suitable camera.

Vortex-carrying matter waves, such as chiral electron beams, are of significant interest in both applied and fundamental science. Continuous wave electron vortex beams are commonly prepared via passive phase masks imprinting a transverse phase modulation on the electron's wave function. Here, we show that femtosecond chiral plasmonic near fields enable the generation and dynamic control on the ultrafast timescale of an electron vortex beam. The vortex structure of the resulting electron wavepacket is probed in both real and reciprocal space using ultrafast transmission electron microscopy. This method offers a high degree of scalability to small length scales and a highly efficient manipulation of the electron vorticity with attosecond precision. Besides the direct implications in the investigation of nanoscale ultrafast processes in which chirality plays a major role, we further discuss the perspectives of using this technique to shape the wave function of charged composite particles, such as protons, and how it can be used to probe their internal structure., 14 pages, 4 figures

To advance the use of thermally-activated magnetic materials in device applications it is necessary to examine their behaviour on the localised scale in operando conditions. Equi-atomic FeRh undergoes a magnetostructural transition from an antiferromagnetic (AF) to a ferromagnetic (FM) phase above room temperature (~ 75 to 105 {\deg}C) and hence is considered a very desirable material for the next generation of novel nanomagnetic or spintronic devices. For this to be realised, we must fully understand the intricate details of AF to FM transition and associated FM domain growth on the scale of their operation. Here we combine in-situ heating with a comprehensive suite of advanced transmission electron microscopy techniques to investigate directly the magnetostructural transition in nano-scale FeRh thin films. Differential phase contrast imaging visualizes the stages of FM domain growth in both cross-sectional and planar FeRh thin films as a function of temperature. Small surface FM signals are also detected due to interfacial strain with the MgO substrate and Fe deficiency after HF etching of the substrate, providing a directional bias for FM domain growth. Our work provides high resolution imaging and quantitative measurements throughout the transition, which were previously inaccessible, and offers new fundamental insight into their potential use in magnetic devices.

International audience; Selective control of the switching path in multiferroics such as BiFeO3 (BFO) is one of the main challenge for the design of non-volatile memories based on magnetoelectric coupling. Here, we demonstrate an alternative way to control binary states of ferroic orders (ferroelectric or ferroelastic) using an array of BFO nanoislands exhibiting two ferroelectric domains. The study of electronic transport properties and domain orientations using atomic force microscopy (AFM) based techniques enabled us to determine electric and mechanical parameters at which ferroelectric and ferroelastic resistive switching can be observed. Ferroelastic switching was associated with a symmetry-breaking induced by electromechanical coupling between the AFM tip and the BFO thin film. It led to out-ofplane polarization pinning that allows performing only in-plane switching accompanied with nucleation and propagation of a conductive domain wall. Nanoislands exhibited binary states of high (OFF) and low resistance (ON) controlled by the tip contact force and the external electric field, without scaling effect (down to 50 nm). High performance characteristics with up to 10 4 OFF/ON ratio, good endurance and retention characteristics were evidenced. Binary states of different ferroic orders with selective control of switching mechanisms by flexoelectric effect can find potential application in non-volatile memory with multilevel data storage capacity.

Holography relies on the interference between a known reference and a signal of interest to reconstruct both the amplitude and the phase of that signal. With electrons, the extension of holography to the ultrafast time domain remains a challenge, although it would yield the highest possible combined spatiotemporal resolution. Here, we show that holograms of local electromagnetic fields can be obtained with combined attosecond/nanometer resolution in an ultrafast transmission electron microscope (UEM). Unlike conventional holography, where signal and reference are spatially separated and then recombined to interfere, our method relies on electromagnetic fields to split an electron wave function in a quantum coherent superposition of different energy states. In the image plane, spatial modulation of the electron energy distribution reflects the phase relation between reference and signal fields. Beyond imaging applications, this approach allows implementing quantum measurements in parallel, providing an efficient and versatile tool for electron quantum optics., Science Advances, 5 (5), ISSN:2375-2548

The antiferromagnetic-to-ferromagnetic phase transition in B2-ordered FeRh is imaged in laterally confined nanopatterned islands using photoemission electron microscopy with x-ray magnetic circular dichroism contrast. The resulting magnetic images directly detail the progression in the shape and size of the FM phase domains during heating and cooling through the transition. In 5-\ud μ\ud m\ud -square islands this domain development during heating is shown to proceed in three distinct modes—nucleation, growth, and merging—each with subsequently greater energy costs. In 0.5-\ud μ\ud m\ud islands, which are smaller than the typical final domain size, the growth mode is stunted and the transition temperature is found to be reduced by 20 K. The modification to the transition temperature is found by high-resolution scanning transmission electron microscopy to be due to a 100-nm chemically disordered edge grain present as a result of ion implantation damage during the patterning. FeRh has unique possibilities for magnetic memory applications; the inevitable changes to its magnetic properties due to subtractive nanofabrication will need to be addressed in future work in order to progress from sheet films to suitable patterned devices.

No abstract available.

The authors became aware of a mistake in the original version of this Article. Specifically, an extra factor γ was incorrectly included in a number of mathematical equations and expressions. As a result of this, a number of changes have been made to both the PDF and the HTML versions of the Article. A full list of these changes is available online.

Three-dimensional orientation of the ferroelectric (FE) domain structure of a BiFeO3 epitaxial film was investigated by scanning electron microscopy (SEM) using back-scattered electrons and piezoresponse-force microscopy (PFM). By changing the crystallographic orientation of the sample and the electron collection angle relative to the detector, we establish a link between the orientation of polarization vectors (out-of-plane and in-plane) in the BiFeO3 film and the back-scattered electron image contrast in agreement with PFM investigations. The different FE polarization states in the domains correspond to altered crystalline environments for the impingent primary beam electrons. We postulate that the resultant back-scattered electron domain contrast arises as a result of either differential absorption (through a channelling effect) or through back-diffraction from the sample, which leads to a projected diffraction pattern super-imposed with the diffuse conventional back-scattered electron intensity. We de...

Self-forming, vertically-aligned, ZnO moth-eye-like nanoarrays were grown by catalyst-free pulsed laser deposition on a-SiO2/Si (1 1 1) substrates. X-Ray Diffraction (XRD) and Cathodoluminescence (CL) studies indicated that nanostructures were highly c-axis oriented wurtzite ZnO with strong near band edge emission. The nanostructures were used as templates for the growth of non-polar GaN by metal organic vapor phase epitaxy. XRD, scanning electron microscopy, energy dispersive X-ray microanalysis and CL revealed ZnO encapsulated with GaN, without evidence of ZnO back-etching. XRD showed compressive epitaxial strain in the GaN, which is conducive to stabilization of the higher indium contents required for more efficient green light emitting diode (LED) and photovoltaic (PV) operation. Angular-dependent specular reflection measurements showed a relative reflectance of less than 1% over the wavelength range of 400–720 nm at all angles up to 60°. The superior black-body performance of this moth-eye-like structure would boost LED light extraction and PV anti-reflection performance compared with existing planar or nanowire LED and PV morphologies. The enhancement in core conductivity, provided by the ZnO, would also improve current distribution and increase the effective junction area compared with nanowire devices based solely on GaN.

We present results from an aberration corrected scanning transmission electron microscope which has been customised for high resolution quantitative Lorentz microscopy with the sample located in a magnetic field free or low field environment. We discuss the innovations in microscope instrumentation and additional hardware that underpin the imaging improvements in resolution and detection with a focus on developments in differential phase contrast microscopy. Examples from materials possessing nanometre scale variations in magnetisation illustrate the potential for aberration corrected Lorentz imaging as a tool to further our understanding of magnetism on this lengthscale.

Magnetic skyrmions are promising candidates as information carriers in logic or storage devices thanks to their robustness, guaranteed by the topological protection, and their nanometric size. Currently, little is known about the influence of parameters such as disorder, defects or external stimuli, on the long-range spatial distribution and temporal evolution of the skyrmion lattice. Here, using a large (7.3x7.3{\mu}m$^{2}$) single crystal nano-slice of Cu$_{2}$OSeO$_{3}$, we image up to 70,000 skyrmions, by means of cryo-Lorentz Transmission Electron Microscopy as a function of the applied magnetic field. The emergence of the skyrmion lattice from the helimagnetic phase is monitored, revealing the existence of a glassy skyrmion phase at the phase transition field, where patches of an octagonally distorted skyrmion lattice are also discovered. In the skyrmion phase, dislocations are shown to cause the emergence and switching between domains with different lattice orientations and the temporal fluctuations of these domains is filmed. These results demonstrate the importance of direct-space and real-time imaging of skyrmion domains for addressing both their long-range topology and stability., Comment: 31 pages (16 + 15 supplementary material),17 figures (4 + 13 supplementary material)

We describe a technique using a focused ion beam instrument to fabricate high quality plan-view specimens for transmission electron microscopy studies. The technique is simple, site-specific and is capable of fabricating multiple large, >100 μm 2 electron transparent windows within epitaxially grown thin films. A film of La 0.67 Sr 0.33 MnO 3 is used to demonstrate the technique and its structural and functional properties are surveyed by high resolution imaging, electron spectroscopy, atomic force microscopy and Lorentz electron microscopy. The window is demonstrated to have good thickness uniformity and a low defect density that does not impair the film's Curie temperature. The technique will enable the study of in-plane structural and functional properties of a variety of epitaxial thin film systems.

Devices comprised of CoFeB nanostructures with perpendicular magnetic anisotropy and non-magnetic Ta channel were operated in thermal lateral spin valve (LSV) mode and studied by magnetotransport measurements and magnetic scanning gate microscopy (SGM). Due to the short spin diffusion length of Ta, the spin diffusion signal was suppressed, allowing the study of the contribution from the anomalous Nernst (ANE) and anomalous Hall effects (AHE). The magnetotransport measurements identified the switching fields of the CoFeB nanostructures and demonstrated a combination of AHE and ANE when the devices were operated in thermally-driven spin-injection mode. Modified scanning probe microscopy probes were fabricated by placing a NdFeB magnetic bead (MB) on the apex of a commercial Si probe. The dipole magnetic field distribution around the MB was characterized by using differential phase contrast technique and direct measurement of the switching field induced by the bead in the CoFeB nanodevices. Using SGM we demonstrate the influence of localized magnetic field on the CoFeB nanostructures near the non-magnetic channel. This approach provides a promising route towards the study of thermal and spin diffusion effects using local magnetic fields.Devices comprised of CoFeB nanostructures with perpendicular magnetic anisotropy and non-magnetic Ta channel were operated in thermal lateral spin valve (LSV) mode and studied by magnetotransport measurements and magnetic scanning gate microscopy (SGM). Due to the short spin diffusion length of Ta, the spin diffusion signal was suppressed, allowing the study of the contribution from the anomalous Nernst (ANE) and anomalous Hall effects (AHE). The magnetotransport measurements identified the switching fields of the CoFeB nanostructures and demonstrated a combination of AHE and ANE when the devices were operated in thermally-driven spin-injection mode. Modified scanning probe microscopy probes were fabricated by placing a NdFeB magnetic bead (MB) on the apex of a commercial Si probe. The dipole magnetic field distribution around the MB was characterized by using differential phase contrast technique and direct measurement of the switching field induced by the bead in the CoFeB nanodevices. Using SGM we demo...

Focused-electron-beam-induced deposition (FEBID) is employed to create freestanding magnetic nanostructures. By growing Fe nanopillars on top of a perpendicular magnetic domain wall (DW) conduit, pinning of the DWs is observed due to the stray fields emanating from the nanopillar. Furthermore, a different DW pinning behavior is observed between the up and down magnetic states of the pillar, allowing to deduce the switching fields of the pillar in a novel way. The implications of these results are two-fold: not only can 3-dimensional nano-objects be used to control DW motion in applications, it is also proposed that DW motion is a unique tool to probe the magnetic properties of nano-objects.

No abstract available.

Capturing and controlling plasmons at buried interfaces with nanometre and femtosecond resolution has yet to be achieved and is critical for next generation plasmonic devices. Here we use light to excite plasmonic interference patterns at a buried metal–dielectric interface in a nanostructured thin film. Plasmons are launched from a photoexcited array of nanocavities and their propagation is followed via photon-induced near-field electron microscopy (PINEM). The resulting movie directly captures the plasmon dynamics, allowing quantification of their group velocity at ∼0.3 times the speed of light, consistent with our theoretical predictions. Furthermore, we show that the light polarization and nanocavity design can be tailored to shape transient plasmonic gratings at the nanoscale. This work, demonstrating dynamical imaging with PINEM, paves the way for the femtosecond and nanometre visualization and control of plasmonic fields in advanced heterostructures based on novel two-dimensional materials such as graphene, MoS2, and ultrathin metal films., Visualizing surface plasmon polaritons at buried interfaces has remained elusive. Here, the authors develop a methodology to study the spatiotemporal evolution of buried near-fields within complex heterostructures, enabling the characterization of the next generation of plasmonic devices.

We present here a study of exploiting Lorentz transmission electron microscopy to observe the magnetic structure in a nanobridge formed by confining a magnetic domain wall. The domain wall is nucleated in an elliptical pad by magnetization reversal and is driven to be pinned at the constriction to form a complex magnetic structure. High-resolution Lorentz microscopy shows that such a structure is composed by a mixture of S and C states of smooth rotation of the magnetization through the nanobridge rather than a conventional single wall as observed previously. This confinement contributes a domain wall resistance observed via anisotropic magnetoresistance presented previously. A serial transformation from S state to S/C mixture, to C state and finally to S state of the topology of the flux is evidently confirmed.

The microstructural and electrochemical properties of La0.4Sr0.6Ti0.8Mn0.2O3±δ (LSTM) fabricated via liquid-phase impregnation have been investigated for solid oxide fuel cell (SOFC) applications. Scanning electron micrography (SEM) showed that LSTM uniformly covers the porous scaffold when heated in an oxidizing atmosphere, which transforms to fine particles when reduced. The electrical conductivity of a 10 wt % CeO2–50 wt % LSTM–8 mol % yttria-stabilized zirconia (8YSZ) composite anode was higher than that of a 50 wt % LSTM–8YSZ anode and was stable at 700, 800, and 900 °C under reducing conditions. When the 50 wt % LSTM-8YSZ was used as an anode, power densities of the sample were

The effect of substrate surface oxides on splat-substrate bonding was investigated by thermally spraying NiCr particles onto aluminum substrates with surface oxide layers grown hydrothermally and electrochemically. Cross sections of bonded solid and molten splats revealed substantial deformation of both the substrate and the surface oxide. In spite of the substantial substrate deformation, there was no significant loss of the surface oxide material and there was no observed diffusion of the substrate oxide into the NiCr particle or vice versa. For solid splats, the substrate oxide was still present over the entire splat-substrate interface, however for molten splats, the oxide had been penetrated in several locations allowing close proximity of the splat metal to the substrate metal. These results strengthen the theory that oxide layers impede bonding and that successful bonding occurs only when the surface oxide is substantially deformed or disrupted to produce mechanically interlocking features at the interface.

A dual FIB/SEM provides solutions to many challenges in atom probe specimen preparation. When combined with an in situ lift-out capability, the versatility of this tool allows almost any region of interest, in almost any geometry, to be placed at the apex of a specimen tip. Several preparation techniques have been developed in response to specific application requirements; for example, in cases where materials are not suitable for electropolishing, or where site-specific analysis is required. Two general techniques, with wide-ranging potential applications, are described in detail here. The first is a 'cut-out' technique that provides a relatively quick means of micro-tip specimen preparation from bulk material samples. The second method is a 'lift-out' technique that can be used in an in situ or ex situ mode and does not require the preparation of pre-sharpened mounting points.

A TiN thin film coating, approximately 4 μm in thickness, deposited on a ductile steel substrate, was subject to surface deformation via nanoindentation using a spherical indenter, 5 μm in radius, with loads up to 500 mN. Pop-ins were observed during loading, which are characteristic of the onset of cracking and the formation of shear steps at the coating–substrate interface. Focused ion beam microscopy was used to prepare cross-sections through the indentation that revealed the presence of both intercolumnar and inclined cracks. Three-dimensional reconstructions of the deformation zone beneath the indentation were performed using a dual-beam focus ion beam instrument. These constructions provided more detailed images of the morphology of cracks, which were observed to be consistent with theoretical models of plastic deformation of such brittle coatings.

The application of differential phase contrast imaging to the study of polycrystalline magnetic thin films and nanostructures has been hampered by the strong diffraction contrast resulting from the granular structure of the materials. In this paper we demonstrate how a pixelated detector has been used to detect the bright field disk in aberration corrected scanning transmission electron microscopy (STEM) and subsequent processing of the acquired data allows efficient enhancement of the magnetic contrast in the resulting images. Initial results from a charged coupled device (CCD) camera demonstrate the highly efficient nature of this improvement over previous methods. Further hardware development with the use of a direct radiation detector, the Medipix3, also shows the possibilities where the reduction in collection time is more than an order of magnitude compared to the CCD. We show that this allows subpixel measurement of the beam deflection due to the magnetic induction. While the detection and processing is data intensive we have demonstrated highly efficient DPC imaging whereby pixel by pixel interpretation of the induction variation is realised with great potential for nanomagnetic imaging.

Spatially resolved analysis of magnetic properties on the nanoscale remains challenging, yet strain and defects on this length-scale can profoundly affect a material's bulk performance. We present a detailed investigation of the magnetic properties of La0.67Sr0.33MnO3 thin films in both free-standing and nanowire form and assess the role of strain and local defects in modifying the films' magnetic properties. Lorentz transmission electron microscopy is used to measure the magnetocrystalline anisotropy and to map the Curie temperature and saturation magnetization with nanometric spatial resolution. Atomic-scale defects are identified as pinning sites for magnetic domain wall propagation. Measurement of domain wall widths and crystalline strain are used to identify a strong magnetoelastic contribution to the magnetic anisotropy. Together, these results provide unique insight into the relationship between the nanostructure and magnetic functionality of a ferromagnetic complex oxide film.

Ultramicroscopy 154, 57-63 (2015). doi:10.1016/j.ultramic.2015.03.016, Published by Elsevier Science, Amsterdam

Using Lorentz transmission electron microscopy we investigate the behavior of domain walls pinned at non-topographic defects in Cr(3 nm)/Permalloy(10 nm)/Cr(5 nm) nanowires of width 500 nm. The pinning sites consist of linear defects where magnetic properties are modified by a Ga ion probe with diameter ~ 10 nm using a focused ion beam microscope. We study the detailed change of the modified region (which is on the scale of the focused ion spot) using electron energy loss spectroscopy and differential phase contrast imaging on an aberration (Cs) corrected scanning transmission electron microscope. The signal variation observed indicates that the region modified by the irradiation corresponds to ~ 40-50 nm despite the ion probe size of only 10 nm. Employing the Fresnel mode of Lorentz transmission electron microscopy, we show that it is possible to control the domain wall structure and its depinning strength not only via the irradiation dose but also the line orientation., Comment: Accepted for publication in Physical Review Applied