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At least 1,135 records · Page 63

Imaging Photonic Resonances within an All‐Dielectric Metasurface via Photoelectron Emission Microscopy

Dielectric metasurfaces, through volume‐type photonic resonances, enable precise control of light‐matter interactions for applications including imaging, holography, and sensing. The application space of dielectric metasurfaces has extended from infrared to visible wavelengths by incorporating high refractive index materials, such as titanium dioxide (TiO 2 ). Understanding the fundamental and fabrication limits for these applications requires metrology with nanoscale resolution, sensitivity to electromagnetic fields within the meta‐atom volume, and far‐field excitation. In this work, photoelectron emission microscopy (PEEM) is used to image field distributions of photonic resonances in a TiO 2 metasurface excited with far‐field, visible‐wavelength illumination. The local volumetric field variations within the meta‐atoms are analyzed as a function of illumination angle and polarization by comparing photoelectron images to finite‐difference time‐domain simulations. This study determines the inelastic mean free path of very low‐energy (<1 eV) photoelectrons to be 35 ± 10 nm, which is comparable to the meta‐atom height thereby highlighting PEEM sensitivity to resonances within the volume. Additionally, the simulations reveal high sensitivity of PEEM images to an in‐plane component of the illumination k ‐vector. These results demonstrate that photoelectron imaging with subwavelength resolution offers unique advantages for examining light‐matter interactions in volume‐type (as opposed to surface) photonic modes within dielectric nanophotonic structures.

electron inelastic mean free path↗

STOCK: Structure mapper and online coarse-graining kit for molecular simulations

We present a web toolkit STructure mapper and Online Coarse-graining Kit for setting up coarse-grained molecular simulations. The kit consists of two tools: structure mapping and Boltzmann inversion tools. The aim of the first tool is to define a molecular mapping from high, e.g. all-atom, to low, i.e. coarse-grained, resolution. Using a graphical user interface it generates input files, which are compatible with standard coarse-graining packages, e.g. VOTCA and DL_CGMAP. Our second tool generates effective potentials for coarse-grained simulations preserving the structural properties, e.g. radial distribution functions, of the underlying higher resolution model. The required distribution functions can be provided by any simulation package. Simulations are performed on a local machine and only the distributions are uploaded to the server. The applicability of the toolkit is validated by mapping atomistic pentane and polyalanine molecules to a coarse-grained representation. Effective potentials are derived for systems of TIP3P (transferable intermolecular potential 3 point) water molecules and salt solution. The presented coarse-graining web toolkit is available at http://stock.cmm.ki.si.

74 ATOMIC AND MOLECULAR PHYSICS↗

Influence of orbital symmetry on diffraction imaging with rescattering electron wave packets

The ability to directly follow and time-resolve the rearrangement of the nuclei within molecules is a frontier of science that requires atomic spatial and few-femtosecond temporal resolutions. While laser-induced electron diffraction can meet these requirements, it was recently concluded that molecules with particular orbital symmetries (such as pg) cannot be imaged using purely backscattering electron wave packets without molecular alignment. Here, we demonstrate, in direct contradiction to these findings, that the orientation and shape of molecular orbitals presents no impediment for retrieving molecular structure with adequate sampling of the momentum transfer space. We overcome previous issues by showcasing retrieval of the structure of randomly oriented O 2 and C 2 H 2 molecules, with π g and π u symmetries, respectively, and where their ionization probabilities do not maximize along their molecular axes. As a result, while this removes a serious bottleneck for laser-induced diffraction imaging, we find unexpectedly strong backscattering contributions from low-Z atoms.

74 ATOMIC AND MOLECULAR PHYSICS↗

Cross-Scale Molecular Analysis of Chemical Heterogeneity in Shale Rocks

The organic and mineralogical heterogeneity in shale at micrometer and nanometer spatial scales contributes to the quality of gas reserves, gas flow mechanisms and gas production. Here, we demonstrate two molecular imaging approaches based on infrared spectroscopy to obtain mineral and kerogen information at these mesoscale spatial resolutions in large-sized shale rock samples. The first method is a modified microscopic attenuated total reflectance measurement that utilizes a large germanium hemisphere combined with a focal plane array detector to rapidly capture chemical images of shale rock surfaces spanning hundreds of micrometers with micrometer spatial resolution. The second method, synchrotron infrared nano-spectroscopy, utilizes a metallic atomic force microscope tip to obtain chemical images of micrometer dimensions but with nanometer spatial resolution. This chemically "deconvoluted" imaging at the nano-pore scale is then used to build a machine learning model to generate a molecular distribution map across scales with a spatial span of 1000 times, which enables high-throughput geochemical characterization in greater details across the nano-pore and micro-grain scales and allows us to identify co-localization of mineral phases with chemically distinct organics and even with gas phase sorbents. Finally, this characterization is fundamental to understand mineral and organic compositions affecting the behavior of shales.

04 OIL SHALES AND TAR SANDS↗

Atomic-Scale Surface Studies of Bulk Metallic Glasses. Final Report

Bulk metallic glasses (BMGs) are of both scientific and technological interest because the absence of periodic atomic arrangements provides them with unique physical, chemical, and mechanical properties. Their high strength, superior elasticity, and an ability to be easily formed into virtually unlimited shapes with feature sizes from centimeters to Angstroms by blow molding and thermoplastic forming makes them an attractive choice for more and more practical applications and products. Due to their complex internal structure, however, experiments that yield insight into their exact atomic arrangements have been scarce. As a result, glass physics is one of the last remaining unexplored fields of materials science despite the scientific and technological importance of glasses in our daily lives, and the question how to characterize and control matter away from equilibrium, as glasses are, was listed as one of five Grand Challenges in a recent DoE report. The main reason for the slow progress in glass physics is the lack of experimental tools that enable access to atomic-scale structural and behavioral information for disordered materials. Such atomic-scale knowledge is mandatory to establish structure-property relationships that ultimately could allow to custom-design alloys featuring specific desired characteristics. With no such relationships available, theory development in glass remains basic and the few that exist are often untested. The aim of this research was to enable progress in our understanding of BMGs by developing a new approach that will allow a meaningful application of local surface science methods to specially prepared BMG samples to obtain a wealth of quantitative information on their atomic arrangements. Key was the availability of specially prepared samples whose surfaces feature large atomically flat terraces despite being entirely amorphous, which we have produced from a Pt 57.5 Cu 14.7 Ni 5.3 P 22.5 alloy (‘Pt-BMG’) both under ambient conditions as well as in ultrahigh vacuum using a unique setup that has been specially developed within this grant. Our approach starts with the in-situ preparation of oxide crystals that are terminated by large terraces, from which exact mirror images out of BMG will be produced using thermoplastic forming (TPF); for the research within this grant, we have successfully used (001)-oriented SrTiO 3 single crystal surfaces as well as (100)-, (110)-, and (111)-oriented single crystals made from LaAlO 3 . Since the resulting BMG replicas display all features of the original crystal with sub-Angstrom fidelity, thereby mimicking the original crystal’s termination by atomically flat terraces without being crystalline themselves, they are ideally suited for further investigation. The following atomic-scale local studies were then carried within this proposal: (i) high-resolution surface imaging and local spectroscopy using scanning probe microscopy, which showed disordered atom-like features and revealed changes in the gradient of the local surface potential on a 1-2 nm length scale; (ii) characterization of atomic-scale plastic flow with affected volumes as low as 1000 atoms, which showed local hardness near or above the theoretically predicted maximum and, once plastic deformation was initiated, homogeneous flow of the atoms involved; (iii) characterization of surface relaxation processes and the onset of crystallization induced by annealing, which showed that upon heating over the material’s glass transition temperature, the surface rearranges and relaxes towards a more stable, denser packed glass, which increases on-terrace surface roughness, while surface tension smoothens step edges; and (iv) studies that investigate the dependence of the material’s mechanical properties and structure on processing parameters, revealing that relaxed glasses get denser, harder, and more elastic. In combination, this information allows to combine structural models with mechanical properties and preparation history, thereby facilitating the development of preparation-structure-property relationships for metallic glasses. With the availability of such information, bulk metallic glasses can be further optimized to be used in more and more applications in industry.

36 MATERIALS SCIENCE↗

Three-dimensional nanoscale characterisation of materials by atom probe tomography

The development of three-dimensional (3D), characterization techniques with high spatial and mass resolution is crucial for understanding and developing advanced materials for many engineering applications as well as for understanding natural materials. In recent decades, atom probe tomography (APT) which combines a point projection microscope and time-of-flight mass spectrometer has evolved to be an excellent characterization technique capable of providing 3D nanoscale characterization of materials with sub-nanometer scale spatial resolution, with equal sensitivity for all elements. This review discusses the current state as of beginning of the year 2016 of APT instrumentation, new developments in sample preparation methods, experimental procedures for different material classes, reconstruction of APT results, the current status of correlative microscopy, and application of APT for microstructural characterization in established scientific areas like structural materials as well as new applications in semiconducting nanowires, semiconductor devices, battery materials, catalyst materials, geological materials and biological materials. Finally, a brief perspective is given regarding the future of APT.

Atom Probe Tomography, characterization, microstru↗

Computer synthesis of high resolution electron micrographs

Specimen damage, spherical aberration, low contrast and noisy sensors combine to prevent direct atomic viewing in a conventional electron microscope. The paper describes two methods for obtaining ultra-high resolution in biological specimens under the electron microscope. The first method assumes the physical limits of the electron objective lens and uses a series of dark field images of biological crystals to obtain direct information on the phases of the Fourier diffraction maxima; this information is used in an appropriate computer to synthesize a large aperture lens for a 1-A resolution. The second method assumes there is sufficient amplitude scatter from images recorded in focus which can be utilized with a sensitive densitometer and computer contrast stretching to yield fine structure image details. Cancer virus characterization is discussed as an illustrative example. Numerous photographs supplement the text.

Nathan, R.↗

Heterogeneity in M. tuberculosis β-lactamase inhibition by Sulbactam

Abstract For decades, researchers have elucidated essential enzymatic functions on the atomic length scale by tracing atomic positions in real-time. Our work builds on possibilities unleashed by mix-and-inject serial crystallography (MISC) at X-ray free electron laser facilities. In this approach, enzymatic reactions are triggered by mixing substrate or ligand solutions with enzyme microcrystals. Here, we report in atomic detail (between 2.2 and 2.7 Å resolution) by room-temperature, time-resolved crystallography with millisecond time-resolution (with timepoints between 3 ms and 700 ms) how the Mycobacterium tuberculosis enzyme BlaC is inhibited by sulbactam (SUB). Our results reveal ligand binding heterogeneity, ligand gating, cooperativity, induced fit, and conformational selection all from the same set of MISC data, detailing how SUB approaches the catalytic clefts and binds to the enzyme noncovalently before reacting to a trans- enamine. This was made possible in part by the application of singular value decomposition to the MISC data using a program that remains functional even if unit cell parameters change up to 3 Å during the reaction.

74 ATOMIC AND MOLECULAR PHYSICS↗

Revealing the Atomic Structures of Exposed Lateral Surfaces for Polymorphic Manganese Dioxide Nanowires

Polymorphic 1D MnO 2 nanostructures are widely applied in fields such as catalysis, sensing, and energy storage with the functionality mainly determined by the atomic patterns of their laterally exposed facets, which largely remain unclear so far. Herein, by high‐resolution transmission electron microscopy (HRTEM) imaging directly along their axial directions, the atomic structures of the outmost lateral facets of polymorphic MnO 2 nanowires are disclosed. To generalize the findings, four most commonly seen phases with characteristic tunnel structures are targeted, i.e., β‐, γ‐, α‐, and todorokite(t)‐MnO 2 , which are synthesized conventionally using a hydrothermal method reported in the literature. Axially imaging these MnO 2 nanowires via HRTEM, the {hkl} facets covering the lateral surfaces are accurately indexed, the atomic pattern of each {hkl} facet is revealed, and it is further coupled with the outmost tunnel configuration that can significantly affect the physicochemical property of MnO 2 materials via tunnel‐driven mass adsorption/transport. This work provides a reliable reference for atomic modeling of MnO 2 to benefit the pursuit of its structure–property relationship; in addition, it can benefit surface engineering strategies to better rationalize the facet growth control with optimized functionality.

Yuan, Yifei↗

Graphene-enabled electron microscopy and correlated super-resolution microscopy of wet cells

The application of electron microscopy to hydrated biological samples has been limited by high-vacuum operating conditions. Traditional methods utilize harsh and laborious sample dehydration procedures, often leading to structural artefacts and creating difficulties for correlating results with high-resolution fluorescence microscopy. Here, we utilize graphene, a single-atom-thick carbon meshwork, as the thinnest possible impermeable and conductive membrane to protect animal cells from vacuum, thus enabling high-resolution electron microscopy of wet and untreated whole cells with exceptional ease. Our approach further allows for facile correlative super-resolution and electron microscopy of wet cells directly on the culturing substrate. In particular, individual cytoskeletal actin filaments are resolved in hydrated samples through electron microscopy and well correlated with super-resolution results.

Science & Technology - Other Topics↗

Characterizing nanoscale scanning probes using electron microscopy: A novel fixture and a practical guide

The nanoscale geometry of probe tips used for atomic force microscopy (AFM) measurements determines the lateral resolution, contributes to the strength of the tip-surface interaction, and can be a significant source of uncertainty in the quantitative analysis of results. While inverse imaging of the probe tip has been used successfully to determine probe tip geometry, direct observation of the tip profile using electron microscopy (EM) confers several advantages: it provides direct (rather than indirect) imaging, requires fewer algorithmic parameters, and does not require bringing the tip into contact with a sample. In the past, EM-based observation of the probe tip has been achieved using ad hoc mounting methods that are constrained by low throughput, the risk of contamination, and repeatability issues. We report on a probe fixture designed for use in a commercial transmission electron microscope that enables repeatable mounting of multiple AFM probes as well as a reference grid for beam alignment. This communication describes the design, fabrication, and advantages of this probe fixture, including full technical drawings for machining. Further, best practices are discussed for repeatable, non-destructive probe imaging. Finally, examples of the fixture’s use are described, including characterization of common commercial AFM probes in their out-of-the-box condition.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Atomic Oxygen Abundance in Molecular Clouds: Absorption Toward Sagittarius B2

We have obtained high-resolution (approximately 35 km/s) spectra toward the molecular cloud Sgr B2 at 63 micrometers, the wavelength of the ground-state fine-structure line of atomic oxygen (O(I)), using the ISO-LWS instrument. Four separate velocity components are seen in the deconvolved spectrum, in absorption against the dust continuum emission of Sgr B2. Three of these components, corresponding to foreground clouds, are used to study the O(I) content of the cool molecular gas along the line of sight. In principle, the atomic oxygen that produces a particular velocity component could exist in any, or all, of three physically distinct regions: inside a dense molecular cloud, in the UV illuminated surface layer (PDR) of a cloud, and in an atomic (H(I)) gas halo. For each of the three foreground clouds, we estimate, and subtract from the observed O(I) column density, the oxygen content of the H(I) halo gas, by scaling from a published high-resolution 21 cm spectrum. We find that the remaining O(I) column density is correlated with the observed (13)CO column density. From the slope of this correlation, an average [O(I)]/[(13)CO] ratio of 270 +/- 120 (3-sigma) is derived, which corresponds to [O(I)]/[(13)CO] = 9 for a CO to (13)CO abundance ratio of 30. Assuming a (13)CO abundance of 1x10(exp -6) with respect to H nuclei, we derive an atomic oxygen abundance of 2.7x10(exp -4) in the dense gas phase, corresponding to a 15% oxygen depletion compared to the diffuse ISM in our Galactic neighborhood. The presence of multiple, spectrally resolved velocity components in the Sgr B2 absorption spectrum allows, for the first time, a direct determination of the PDR contribution to the O(I) column density. The PDR regions should contain O(I) but not (13)CO, and would thus be expected to produce an offset in the O(I)-(13)CO correlation. Our data do not show such an offset, suggesting that within our beam O(I) is spatially coexistent with the molecular gas, as traced by (13)CO. This may be a result of the inhomogeneous nature of the clouds.

Lis, D. C.↗

On the Efficiency $\eta$ and the Homogeneity of TiN Kinetic Inductance Detectors Produced through Atomic Layer Deposition

Microwave Kinetic Inductance Detectors (MKIDs) belong to non-equilibrium superconducting devices. It is a new promising device due to high quantum efficiency, low theoretical noise limit, multiplex frequency domain, photon-number-resolving, and energy resolving. In the case of MKIDs, a change in the kinetic inductance is produced by the breaking of Cooper pairs, modifying the electrodynamic response of the superconductor. The production process of an MKID consists of depositing a superconducting thin film on an insulating substrate and applying standard lithographic patterning techniques to produce a resonator structure. When an MKID is produced via sputtering, film nonuniformity is observed, producing instability, low yield, frequency collisions, and low energy resolution. We exploring film uniformity in films produced with Atomic Layer Deposition (ALD) and through ALD archive high values in the energy resolution. The uniformity of ALD is evaluated via measurement of the critical temperature of 4 MKIDs. Two MKIDs belong to the first fabrication process and the other two to another. The results obtained are: ΔTc/max(σT1,σT2) is 0.45 for A1-B1 and 0.21 for A2-B2. The difference in the Tc for MKIDs of the same wafer is around 5.1 mK and from different wafers, the maximum difference is 66 mk with a minimum of 48 mK. However, with the high uniformity archived, we obtained a poor response of the MKIDs when a photon is absorbed. As a consequence of the low response, we examined in the literature about the process of photon absorption. In this evaluation, we were focusing on the down-conversion efficiency as a possible cause for the degraded energy resolution. In this process, one part of the initial energy of the photon is lost, transferred to the creation of quasiparticles and phonons. The phonons that do not possess enough energy to break a Cooper pair are lost from the system. This loss in energy is accounted for by the eff iciency η which has a constant value reported as 0.57 (! from simulation). Due to the efficiency had been reported always as constant. We proceed to evaluate its value through a new method. The process consists of measuring the gain of the system via the photon transfer curve and thermal calibration. The efficiency obtained with this new method is of 0.008 which has a lower value in comparison with the simulation. The methods to obtain the critical temperature, as well as the new method to evaluate the efficiency of an MKID will be shown in this work.

43 PARTICLE ACCELERATORS↗

On the existence of orthorhombic martensite in a near-α titanium base alloy used for additive manufacturing

Additive manufacturing is a state-of-the-art production technology to produce tailor-made and highly complex parts. Among various other alloys, Ti base alloys are frequently used in this manufacturing technique due to their well-balanced properties and their wide range of applications. Allotropic phases and the occurrence of athermal phase transformations are the main reasons why these alloys hold a great development potential and are the basis of extensive use. High cooling rates during manufacturing lead to martensitic phases and the formation of nanometer-sized microstructures resulting in extraordinary strength. Simultaneously, such high cooling rates cause a high amount of lattice defects and the occurrence of residual stresses, which finally may result in delamination effects and cracks. Usually, a common approach to reduce residual stresses during additive manufacturing is to decrease thermal gradients by increasing the heat input or preheating the building platform. Instead of applying the typical approaches to lower thermal gradients, this study deals with the origin of the ‘softer’ orthorhombic martensite by accelerating the solidification process. The implementation of the orthorhombic phase in bulk components was inspired by a new phase transformation herein reported for the first time in the powder material, which also validates the possible occurrence of two martensitic phases in the same alloy. Various sophisticated characterization techniques like high energy and high-temperature X-ray diffraction, high-resolution transmission electron microscopy as well as atom probe tomography were applied to characterize this softer orthorhombic martensitic phase in detail aiming to highlight the opportunities accompanied by this new approach for additive manufacturing of titanium alloys.

36 MATERIALS SCIENCE↗

Structural study of growth, orientation and defects characteristics in the functional microelectromechanical system material aluminium nitride

The real structure and morphology of piezoelectric aluminum nitride (AlN) thin films as essential components of magnetoelectric sensors are investigated via advanced transmission electron microscopy methods. State of the art electron diffraction techniques, including precession electron diffraction and automated crystal orientation mapping (ACOM), indicate a columnar growth of the AlN grains optimized for piezoelectric application with a (0 0 0 1) texture. Comparing ACOM with piezoresponse force microscopy measurements, a visual correlation of the structure and the piezoelectric properties is enabled. With a quantitative analysis of the ACOM measurements, a statistical evaluation of grain rotations is performed, indicating the presence of coincidence site lattices with Σ7, Σ13a, Σ13b, Σ25. Using a geometric phase analysis on high resolution micrographs, the occurrence of strain is detected almost exclusively at the grain boundaries. Moreover, high resolution imaging was applied for solving the atomic structure at stacking mismatch boundaries with a displacement vector of 1/2 〈1 0 -1 1〉. All real structural features can be interpreted via simulations based on crystallographic computing in terms of a supercell approach.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Synthesis of graphene by cobalt-catalyzed decomposition of methane in plasma-enhanced CVD: Optimization of experimental parameters with Taguchi method

This article describes the significant roles of process parameters in the deposition of graphene films via cobalt-catalyzed decomposition of methane diluted in hydrogen using plasma-enhanced chemical vapor deposition (PECVD). The influence of growth temperature (700–850 °C), molar concentration of methane (2%–20%), growth time (30–90 s), and microwave power (300–400 W) on graphene thickness and defect density is investigated using Taguchi method which enables reaching the optimal parameter settings by performing reduced number of experiments. Growth temperature is found to be the most influential parameter in minimizing the number of graphene layers, whereas microwave power has the second largest effect on crystalline quality and minor role on thickness of graphene films. The structural properties of PECVD graphene obtained with optimized synthesis conditions are investigated with Raman spectroscopy and corroborated with atomic-scale characterization performed by high-resolution transmission electron microscopy and scanning tunneling microscopy, which reveals formation of continuous film consisting of 2–7 high quality graphene layers.

36 MATERIALS SCIENCE↗