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Register a new userDesign and Application of Variable Temperature Environmental Capsule for Scanning Electron Microscopy in Gases and Liquids at Ambient Conditions
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Scanning electron microscopy (SEM) of nanoscale objects in their native conditions and at different temperatures are of critical importance in revealing details of their interactions with ambient environments. Currently available environmental capsules are equipped with thin electron transparent membranes and allow imaging the samples at atmospheric pressure. However these capsules do not provide the temperature control over the sample. Here we developed and tested a thermoelectric cooling / heating setup for available environmental capsules to allow ambient pressure in situ SEM studies over the -15 {deg}C to 100 {deg}C temperature range in gaseous, liquid, and frozen environments. The design of the setup also allows correlation of the SEM with optical microscopy and spectroscopy. As a demonstration of the possibilities of the developed approach, we performed real-time in situ microscopy studies of water condensation on a surface of wing scales of Morpho sulkowskyi butterfly. We have found that the initial water nucleation takes place on the top of the scale ridges. These results confirmed earlier discovery of a polarity gradient of the ridges of Morpho butterflies. Our developed thermoelectric cooling / heating setup for available SEM environmental capsules promises to impact diverse needs for in-situ nano-characterization including materials science and catalysis, micro-instrumentation and device reliability, chemistry and biology.
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Due to its ultrahigh electron transmissivity in a wide electron energy range, molecular impermeability, high electrical conductivity and excellent mechanical stiffness the suspended graphene membranes appear to be a nearly ideal window material for in situ (in vivo) environmental electron microscopy of nano- and mesoscopic objects (including bio-medical samples) immersed in liquids and/or in dense gaseous media. In this communication, taking advantage of little modification of the graphene transfer protocol on to metallic and SiN supporting orifices, the reusable environmental cells with exchangeable graphene windows have been designed. Using colloidal gold nanoparticles (50 nm) dispersed in water as model objects for scanning electron microscopy in liquids, the different imaging conditions through graphene membrane have been tested. The limiting factors for electron microscopy in liquids such as electron beam induced water radiolysis and damage of graphene membrane at high electron doses were discussed.
The domain configuration of 50 nm thick La0.7SrMnO3 films has been directly investigated using scanning electron microscopy with polarization analysis (SEMPA), with magnetic contrast obtained without the requirement for prior surface preparation. The large scale domain structure reflects a primarily four-fold anisotropy, with a small uniaxial component, consistent with magneto-optic Kerr effect measurements. We also determine the domain transition profile and find it to be in agreement with previous estimates of the domain wall width in this material. The temperature dependence of the image contrast is investigated and compared to superconducting-quantum interference device magnetometry data. A faster decrease in the SEMPA contrast is revealed, which can be explained by the techniques extreme surface sensitivity, allowing us to selectively probe the surface spin polarization which due to the double exchange mechanism exhibits a distinctly different temperature dependence than the bulk magnetization.
Thin film oxides are a source of endless fascination for the materials scientist. These materials are highly flexible, can be integrated into almost limitless combinations, and exhibit many useful functionalities for device applications. While precision synthesis techniques, such as molecular beam epitaxy (MBE) and pulsed laser deposition (PLD), provide a high degree of control over these systems, there remains a disconnect between ideal and realized materials. Because thin films adopt structures and chemistries distinct from their bulk counterparts, it is often difficult to predict what properties will emerge. The complex energy landscape of the synthesis process is also strongly influenced by non-equilibrium growth conditions imposed by the substrate, as well as the kinetics of thin film crystallization and fluctuations in process variables, all of which can lead to significant deviations from targeted outcomes. High-resolution structural and chemical characterization techniques, as described in this volume, are needed to verify growth models, bound theoretical calculations, and guide materials design. While many characterization options exist, most are spatially-averaged or indirect, providing only partial insight into the complex behavior of these systems. Over the past several decades, scanning transmission electron microscopy (STEM) has become a cornerstone of oxide heterostructure characterization owing to its ability to simultaneously resolve structure, chemistry, and defects at the highest spatial resolution. STEM methods are an essential complement to averaged scattering techniques, offering a direct picture of resulting materials that can inform and refine the growth process to achieve targeted properties. There is arguably no other technique that can provide such a broad array of information at the atomic-scale, all within a single experimental session.
In this study, we have used a Zr-Nb alloy containing well-defined nano-precipitates as a model material in which to study imaging contrast
A simple, reliable method for preparation of bulk Cr tips for Scanning Tunneling Microscopy (STM) is proposed and its potentialities in performing high-quality and high-resolution STM and Spin Polarized-STM (SP-STM) are investigated. Cr tips show atomic resolution on ordered surfaces. Contrary to what happens with conventional W tips, rest atoms of the Si(111)-7x7 reconstruction can be routinely observed, probably due to a different electronic structure of the tip apex. SP-STM measurements of the Cr(001) surface showing magnetic contrast are reported. Our results reveal that the peculiar properties of these tips can be suited in a number of STM experimental situations.
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