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  • 21
    Publication Date: 2018-03-30
    Description: Publication date: May 2018 Source: Ultramicroscopy, Volume 188 Author(s): H. Schmid, E. Gilardi, G. Gregori, P. Longo, J. Maier, P.A. van Aken Epitaxial undoped and Gd 2 O 3 -doped ceria films were grown by pulsed laser deposition on (1 1 1) faced Y 2 O 3 -stabilized zirconia (YSZ). Highly localized cerium reduction at the film-substrate interfaces is revealed by atomically resolved valence EELS mapping using C s aberration-corrected scanning transmission electron microscopy. The chemical profiles reveal interdiffusion of Ce, (Gd), Y, Zr, forming an intermixing zone at the interface 7–9 (1 1 1) lattice planes wide. In its vicinity, the fraction of Ce 3+ raises gradually over 6–8 lattice planes from zero in the bulk ceria to ≈100% in one single plane at the interface. Beyond this plane the Ce 3+ fraction drops sharply within the YSZ substrate. In the vicinity of the interface systematic scan deflections are observed during EELS line scans. The advancing electron probe experiences a retarding force at the ceria side, and an accelerating force at the YSZ side, irrespective of the scan direction. This behavior is suggestive of coulombic interactions between the electron probe and a charged interface. This is interpreted as an indication of the presence of a space-charge situation at the YSZ/ceria interface, resulting from an excess negative charge at the ceria side (due to Ce 3+ cations) and an excess positive charge at the YSZ side (due to oxygen vacancies).
    Print ISSN: 0304-3991
    Topics: Electrical Engineering, Measurement and Control Technology , Natural Sciences in General , Physics
    Published by Elsevier
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  • 22
    Publication Date: 2018-03-29
    Description: Publication date: May 2018 Source: Ultramicroscopy, Volume 188 Author(s): A. Scholl, M.A. Marcus, A. Doran, J.R. Nasiatka, A.T. Young, A.A. MacDowell, R. Streubel, N. Kent, J. Feng, W. Wan, H.A. Padmore Aberration correction by an electron mirror dramatically improves the spatial resolution and transmission of photoemission electron microscopes. We will review the performance of the recently installed aberration corrector of the X-ray Photoemission Electron Microscope PEEM-3 and show a large improvement in the efficiency of the electron optics. Hartmann testing is introduced as a quantitative method to measure the geometrical aberrations of a cathode lens electron microscope. We find that aberration correction leads to an order of magnitude reduction of the spherical aberrations, suggesting that a spatial resolution of below 100 nm is possible at 100% transmission of the optics when using x-rays. We demonstrate this improved performance by imaging test patterns employing element and magnetic contrast.
    Print ISSN: 0304-3991
    Topics: Electrical Engineering, Measurement and Control Technology , Natural Sciences in General , Physics
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  • 23
    Publication Date: 2018-03-29
    Description: Publication date: April 2018 Source: Ultramicroscopy, Volume 187 Author(s): Jinsen Tian, Jing Wu, Yu-Lung Chiu The intensity profiles of backscattered and secondary electrons from a pure Mg sample have shown a variation with sample thickness and acceleration voltage in the range of 5–30 kV, depending on the specimen holder used. The intensities of backscattered electron (BSE) and secondary electron (SE) signals increases with the sample thickness until saturation when using a scanning transmission electron microscopy (STEM) holder with a closed tube below the sample. However the SE signal increases to the maximum and then decreases with the sample thickness when using a transmission Kikuchi diffraction (TKD) holder with no shielding below the sample whereas the BSE signal again increases until saturation. The influence of the holder on the SE signals is caused by the fact that secondary electrons emitted from the bottom surface could be detected only when using the TKD holder but not the STEM holder. The experimental results obtained are consistent with the Monte Carlo simulation results. Application of the magnitude of the SE and BSE signals to measurement of sample thickness has been considered and the BSE image profile shows a reasonably good accuracy.
    Print ISSN: 0304-3991
    Topics: Electrical Engineering, Measurement and Control Technology , Natural Sciences in General , Physics
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  • 24
    Publication Date: 2018-03-29
    Description: Publication date: April 2018 Source: Ultramicroscopy, Volume 187 Author(s): Federico Gramazio, Matteo Lorenzoni, Francesc Pérez-Murano, Laura Evangelio, Jordi Fraxedas The determination of nanomechanical properties is an intensive topic of study in several fields of nanophysics, from surface and materials science to biology. At the same time, amplitude modulation force microscopy is one of the most established techniques for nanoscale characterization. In this work, we combine these two topics and propose a method able to extract quantitative nanomechanical information from higher harmonic amplitude imaging in atomic force microscopy. With this method it is possible to discriminate between different materials in the stiffness range of 1–3 GPa, in our case thin films of PS-PMMA based block copolymers. We were able to obtain a critical lateral resolution of less than 20 nm and discriminate between materials with less than a 1 GPa difference in modulus. We show that within this stiffness range, reliable values of the Young's moduli can be obtained under usual imaging conditions and with standard dynamic AFM probes.
    Print ISSN: 0304-3991
    Topics: Electrical Engineering, Measurement and Control Technology , Natural Sciences in General , Physics
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  • 25
    Publication Date: 2018-03-29
    Description: Publication date: April 2018 Source: Ultramicroscopy, Volume 187 Author(s): Ivan Khalakhan, Andrei Choukourov, Mykhailo Vorokhta, Peter Kúš, Iva Matolínová, Vladimír Matolín A platinum catalyst undergoes complex deterioration process during its operation as a cathode in a proton exchange membrane fuel cell. By using in situ electrochemical atomic force microscopy (EC-AFM) with super-sharp probes, we quantitatively describe the roughening of platinum thin films during electrochemical cycling to different upper potentials, which simulate critical operation regimes of the proton exchange membrane fuel cell. The comprehensive quantitative analysis of morphology changes obtained using common roughness descriptors such as the root mean square roughness, the correlation length and the roughness exponent is correlated with cyclic voltammetry performed simultaneously.
    Print ISSN: 0304-3991
    Topics: Electrical Engineering, Measurement and Control Technology , Natural Sciences in General , Physics
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  • 26
    Publication Date: 2018-03-29
    Description: Publication date: April 2018 Source: Ultramicroscopy, Volume 187 Author(s): Elena Pascal, Saransh Singh, Patrick G. Callahan, Ben Hourahine, Carol Trager-Cowan, Marc De Graef Transmission Kikuchi diffraction (TKD) has been gaining momentum as a high resolution alternative to electron back-scattered diffraction (EBSD), adding to the existing electron diffraction modalities in the scanning electron microscope (SEM). The image simulation of any of these measurement techniques requires an energy dependent diffraction model for which, in turn, knowledge of electron energies and diffraction distances distributions is required. We identify the sample-detector geometry and the effect of inelastic events on the diffracting electron beam as the important factors to be considered when predicting these distributions. However, tractable models taking into account inelastic scattering explicitly are lacking. In this study, we expand the Monte Carlo (MC) energy-weighting dynamical simulations models used for EBSD [1] and ECP [2] to the TKD case. We show that the foil thickness in TKD can be used as a means of energy filtering and compare band sharpness in the different modalities. The current model is shown to correctly predict TKD patterns and, through the dictionary indexing approach, to produce higher quality indexed TKD maps than conventional Hough transform approach, especially close to grain boundaries.
    Print ISSN: 0304-3991
    Topics: Electrical Engineering, Measurement and Control Technology , Natural Sciences in General , Physics
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  • 27
    Publication Date: 2018-03-29
    Description: Publication date: April 2018 Source: Ultramicroscopy, Volume 187 Author(s): E. Di Russo, I. Blum, J. Houard, M. Gilbert, G. Da Costa, D. Blavette, L. Rigutti A systematic study of the biases occurring in the measurement of the composition of GaN by Atom Probe Tomography was carried out, in which the role of surface electric field and laser pulse intensity has been investigated. Our data confirm that the electric field is the main factor influencing the measured composition, which exhibits a deficiency of N at low field and a deficiency of Ga at high field. The deficiency of Ga at high field is interpreted in terms of preferential evaporation of Ga. The detailed analysis of multiple evaporation events reveals that the measured composition is not affected by pile-up phenomena occurring in detection system. The analysis of correlation histograms yields the signature of the production of neutral N 2 due to the dissociation of GaN 3 2+ ions. However, the amount of N 2 neutral molecules that can be detected cannot account for the N deficiency found at low field. Therefore, we propose that further mechanisms of neutral N evaporation could be represented by dissociation reactions such as GaN + → Ga + + N and GaN 2+ → Ga 2 + + N.
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    Topics: Electrical Engineering, Measurement and Control Technology , Natural Sciences in General , Physics
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  • 28
    Publication Date: 2018-03-29
    Description: Publication date: Available online 26 March 2018 Source: Ultramicroscopy Author(s): Zirong Peng, Francois Vurpillot, Pyuck-Pa Choi, Yujiao Li, Dierk Raabe, Baptiste Gault In atom probe tomography (APT), multiple events can arise as a consequence of e.g. correlated field evaporation and molecular ion dissociation. They represent challenging cases for single-particle detectors and can cause compositional as well as spatial inaccuracies. Here, two state-of-the-art atom probe microscopes (Cameca LEAP 5000 XS and 5000 XR) were used to investigate cemented tungsten carbide, which exhibits high amounts of multiple events. By advanced data analysis methods, the natural character of the multiple events, as well as the performance of the APT detectors, are assessed. Accordingly, possible signal loss mechanisms are discussed.
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    Topics: Electrical Engineering, Measurement and Control Technology , Natural Sciences in General , Physics
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  • 29
    Publication Date: 2018-03-29
    Description: Publication date: May 2018 Source: Ultramicroscopy, Volume 188 Author(s): W. Verhoeven, J.F.M. van Rens, E.R. Kieft, P.H.A. Mutsaers, O.J. Luiten Ultrashort, low-emittance electron pulses can be created at a high repetition rate by using a TM 110 deflection cavity to sweep a continuous beam across an aperture. These pulses can be used for time-resolved electron microscopy with atomic spatial and temporal resolution at relatively large average currents. In order to demonstrate this, a cavity has been inserted in a transmission electron microscope, and picosecond pulses have been created. No significant increase of either emittance or energy spread has been measured for these pulses. At a peak current of 814 ± 2 pA, the root-mean-square transverse normalized emittance of the electron pulses is ɛ n , x = ( 2.7 ± 0.1 ) · 10 − 12  m rad in the direction parallel to the streak of the cavity, and ɛ n , y = ( 2.5 ± 0.1 ) · 10 − 12  m rad in the perpendicular direction for pulses with a pulse length of 1.1–1.3 ps. Under the same conditions, the emittance of the continuous beam is ɛ n , x = ɛ n , y = ( 2.5 ± 0.1 ) · 10 − 12  m rad. Furthermore, for both the pulsed and the continuous beam a full width at half maximum energy spread of 0.95 ± 0.05 eV has been measured.
    Print ISSN: 0304-3991
    Topics: Electrical Engineering, Measurement and Control Technology , Natural Sciences in General , Physics
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  • 30
    Publication Date: 2018-03-29
    Description: Publication date: April 2018 Source: Ultramicroscopy, Volume 187 Author(s): A. Pofelski, S.Y. Woo, B.H. Le, X. Liu, S. Zhao, Z. Mi, S. Löffler, G.A. Botton A strain characterization technique based on Moiré interferometry in a scanning transmission electron microscope (STEM) and geometrical phase analysis (GPA) method is demonstrated. The deformation field is first captured in a single STEM Moiré hologram composed of multiple sets of periodic fringes (Moiré patterns) generated from the interference between the periodic scanning grating, fixing the positions of the electron probe on the sample, and the crystal structure. Applying basic principles from sampling theory, the Moiré patterns arrangement is then simulated using a STEM electron micrograph reference to convert the experimental STEM Moiré hologram into information related to the crystal lattice periodicities. The GPA method is finally applied to extract the 2D relative strain and rotation fields. The STEM Moiré interferometry enables the local information to be de-magnified to a large length scale, comparable to what can be achieved in dark-field electron holography. The STEM Moiré GPA method thus extends the conventional high-resolution STEM GPA capabilities by providing comparable quantitative 2D strain mapping with a larger field of view (up to a few microns).
    Print ISSN: 0304-3991
    Topics: Electrical Engineering, Measurement and Control Technology , Natural Sciences in General , Physics
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