45 results on '"Dunin-Borkowski, Rafal E."'
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2. Macroscopic magnetic hardening due to nanoscale spinodal decomposition in Fe–Cr
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Vojtech, Vladimir, Charilaou, Michalis, Kovács, András, Firlus, Alexander, Gerstl, Stephan S.A., Dunin-Borkowski, Rafal E., Löffler, Jörg F., and Schäublin, Robin
- Subjects
Atom probe tomography ,Fusion reactor ,Fe-Cr ,Hardness ,Phase decomposition ,Lorentz transmission electron microscopy ,Magnetism - Abstract
The Fe–Cr alloy system is the basis of ferritic steels, which are important structural materials for many applications, including their use in future fusion reactors. However, when exposed to elevated temperatures and radiation, the Fe–Cr system can undergo phase separation, resulting in Fe-rich (α) and Cr-rich (α’) nanoscale regions. This in turn generates the so-called “475 °C embrittlement” and modifies the magnetic properties. The correlation between the microstructural and magnetic changes is however poorly understood, which currently prevents the possibility of assessing the material in a non-destructive way by magnetometry. Here, we study the microstructural decomposition of an Fe–40Cr alloy induced by annealing at 500 °C for extensive time scales and its impact on the magnetic properties using magnetometry and advanced experimental methods, such as atom probe tomography, transmission electron microscopy (TEM), and micromagnetic simulations. Upon annealing, the alloy rapidly exhibits a spinodal decomposition morphology with a typical length scale of about 10 nm. With increasing annealing time, the hardness assessed by Vickers testing, the magnetic saturation, and the coercivity increase, which correlates with an increase in α-volume fraction and the system's heterogeneity. The magnetic domain patterns imaged by TEM and interpreted with the help of micromagnetic simulations reveal at the nanometer scale the impact of decomposition on the magnetic response of Fe–Cr., Acta Materialia, 240, ISSN:1359-6454
- Published
- 2022
3. Quantitative electric field mapping between electrically biased needles by scanning transmission electron microscopy and electron holography.
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Dushimineza JF, Jo J, Dunin-Borkowski RE, and Müller-Caspary K
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Stray electric fields in free space generated by two biased gold needles have been quantified in comprehensive finite-element (FE) simulations, accompanied by first moment (FM) scanning TEM (STEM) and electron holography (EH) experiments. The projected electrostatic potential and electric field have been derived numerically under geometrical variations of the needle setup. In contrast to the FE simulation, application of an analytical model based on line charges yields a qualitative understanding. By experimentally probing the electric field employing FM STEM and EH under alike conditions, a discrepancy of about 60% became apparent initially. However, the EH setup suggests the reconstructed phase to be significantly affected by the perturbed reference wave effect, opposite to STEM where the field-free reference was recorded subsequently with unbiased needles in which possibly remaining electrostatic influences are regarded as being minor. In that respect, the observed discrepancy between FM imaging and EH is resolved after including the long-range potential landscape from FE simulations into the phase of the reference wave in EH., Competing Interests: Declaration of competing interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: Knut Mueller–Caspary reports financial support was provided by Helmholtz Association of German Research Centres. Knut Mueller–Caspary reports financial support was provided by German Research Foundation. Jean Felix Dushimineza reports financial support was provided by Helmholtz Association of German Research Centres. Janghyun Jo reports financial support was provided by German Research Foundation., (Copyright © 2023 The Author(s). Published by Elsevier B.V. All rights reserved.)
- Published
- 2023
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4. TEMGYM Advanced: Software for electron lens aberrations and parallelised electron ray tracing.
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Landers D, Clancy I, Dunin-Borkowski RE, Weber D, and Stewart A
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Characterisation of the electron beams trajectory in an electron microscope is possible in a few select commercial software packages, but these tools and their source code are not available in a free and accessible manner. This paper introduces the free and open-source software TEMGYM Advanced, which implements ray tracing methods that calculate the path of electrons through a magnetic or electrostatic lens and allow evaluation of the first-order properties and third-order geometric aberrations. Validation of the aberration coefficient calculations is performed by implementing two independent methods - the aberration integral and differential algebra (DA) methods and by comparing the results of each. This paper also demonstrates parallelised electron ray tracing through a series of magnetic components, which enables near real-time generation of a physically accurate beam-spot including aberrations and brings closer the realisation of a digital twin of an electron microscope. TEMGYM Advanced represents a valuable resource for the electron microscopy community, providing an accessible and open source means of characterising electron lenses. This software utilises the Python programming language to complement the growing ecosystem of free and open-source software within the electron microscopy community, and to facilitate the application of machine learning to an electron microscope digital twin for instrument automation. The software is available under GNU Public License number Three (GPL 3)., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 The Author(s). Published by Elsevier B.V. All rights reserved.)
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- 2023
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5. Near-real-time diagnosis of electron optical phase aberrations in scanning transmission electron microscopy using an artificial neural network.
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Bertoni G, Rotunno E, Marsmans D, Tiemeijer P, Tavabi AH, Dunin-Borkowski RE, and Grillo V
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- Microscopy, Electron, Scanning Transmission methods, Artificial Intelligence, Neural Networks, Computer, Electrons, Lenses
- Abstract
The key to optimizing spatial resolution in a state-of-the-art scanning transmission electron microscope is the ability to measure and correct for electron optical aberrations of the probe-forming lenses precisely. Several diagnostic methods for aberration measurement and correction have been proposed, albeit often at the cost of relatively long acquisition times. Here, we illustrate how artificial intelligence can be used to provide near-real-time diagnosis of aberrations from individual Ronchigrams. The demonstrated speed of aberration measurement is important because microscope conditions can change rapidly. It is also important for the operation of MEMS-based hardware correction elements, which have less intrinsic stability than conventional electromagnetic lenses., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: Vincenzo Grillo reports financial support was provided by Horizon 2020. Rafal E. Dunin-Borkowski reports financial support was provided by Horizon 2020., (Copyright © 2022 The Authors. Published by Elsevier B.V. All rights reserved.)
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- 2023
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6. Electron-beam-induced charging of an Al 2 O 3 nanotip studied using off-axis electron holography.
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Zheng F, Beleggia M, Migunov V, Pozzi G, and Dunin-Borkowski RE
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Electrostatic charging of specimens during electron, photon or ion irradiation is a complicated and poorly understood phenomenon, which can affect the acquisition and interpretation of experimental data and alter the functional properties of the constituent materials. It is usually linked to secondary electron emission, but also depends on the geometry and electrical properties of the specimen. Here, we use off-axis electron holography in the transmission electron microscope to study electron-beam-induced charging of an insulating Al
2 O3 nanotip on a conducting support. The measurements are performed under parallel electron illumination conditions as a function of specimen temperature, electron dose, primary electron energy and surface cleanliness. We observe a lack of reproducibility of charge density measurements after cycling the specimen temperature. Surprisingly, we find both positively and negatively charged regions in closely adjacent parts of the specimen., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 The Author(s). Published by Elsevier B.V. All rights reserved.)- Published
- 2022
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7. Imaging biological macromolecules in thick specimens: The role of inelastic scattering in cryoEM.
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Dickerson JL, Lu PH, Hristov D, Dunin-Borkowski RE, and Russo CJ
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- Cryoelectron Microscopy methods, Microscopy, Electron, Microscopy, Phase-Contrast, Monte Carlo Method, Electrons
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We investigate potential improvements in using electron cryomicroscopy to image thick specimens with high-resolution phase contrast imaging. In particular, using model experiments, electron scattering theory, Monte Carlo and multislice simulations, we determine the potential for improving electron cryomicrographs of proteins within a cell using chromatic aberration (C
c ) correction. We show that inelastically scattered electrons lose a quantifiable amount of spatial coherence as they transit the specimen, yet can be used to enhance the signal from thick biological specimens (in the 1000 to 5000 Å range) provided they are imaged close to focus with an achromatic lens. This loss of information quantified here, which we call "specimen induced decoherence", is a fundamental limit on imaging biological molecules in situ. We further show that with foreseeable advances in transmission electron microscope technology, it should be possible to directly locate and uniquely identify sub-100 kDa proteins without the need for labels, in a vitrified specimen taken from a cell., (Copyright © 2022 MRC Laboratory of Molecular Biology. Published by Elsevier B.V. All rights reserved.)- Published
- 2022
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8. Prospect for measuring two-dimensional van der Waals magnets by electron magnetic chiral dichroism.
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Song D, Zheng F, and Dunin-Borkowski RE
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Two-dimensional (2D) van der Waals magnets have drawn considerable attention in recent years triggered by the huge interest in novel magnetism and spintronic devices. Magnetic measurement of 2D van der Waals (vdW) magnets is crucial to understand the physical origin of magnetism in 2D limits. Therefore, advanced magnetic characterization techniques are highly required. However, only a limited number of such techniques are available due to the extremely small volume of 2D vdW magnets. Here, we introduce the electron magnetic chiral dichroism (EMCD) technique in transmission electron microscope (TEM) to measure 2D vdW crystals. In comparison with some other already-employed techniques in 2D magnets, EMCD is able to quantitatively measure magnetic parameters in three orthogonal directions at nanometer or even at atomic scale. We then perform EMCD simulations on several typical 2D vdW magnets with respect to the accelerating voltage, the number of atomic layers and beam tilt under zone axial orientation. The intensity and distribution of EMCD signals in three orthogonal directions are given in the diffraction plane, thereby providing an optimized design to achieve EMCD measurements. Finally, we discuss the signal-to-noise-ratio and required electron dose in order to obtain a measurable EMCD signal for 2D vdW magnets. Our results provide a feasibility analysis and guideline to measure 2D vdW magnets in future experiments., (Copyright © 2022 The Authors. Published by Elsevier B.V. All rights reserved.)
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- 2022
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9. Continuous illumination picosecond imaging using a delay line detector in a transmission electron microscope.
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Weßels T, Däster S, Murooka Y, Zingsem B, Migunov V, Kruth M, Finizio S, Lu PH, Kovács A, Oelsner A, Müller-Caspary K, Acremann Y, and Dunin-Borkowski RE
- Abstract
Progress towards analysing transitions between steady states demands improvements in time-resolved imaging, both for fundamental research and for applications in information technology. Transmission electron microscopy is a powerful technique for investigating the atomic structure, chemical composition and electromagnetic properties of materials with high spatial resolution and precision. However, the extraction of information about dynamic processes in the ps time regime is often not possible without extensive modification to the instrument while requiring careful control of the operation conditions to not compromise the beam quality. Here, we avoid these drawbacks by combining a delay line detector with continuous illumination in a transmission electron microscope. We visualize the gyration of a magnetic vortex core in real space and show that magnetization dynamics up to frequencies of 2.3 GHz can be resolved with down to ∼122ps temporal resolution by studying the interaction of an electron beam with a microwave magnetic field. In the future, this approach promises to provide access to resonant dynamics by combining high spatial resolution with sub-ns temporal resolution., (Copyright © 2021 The Authors. Published by Elsevier B.V. All rights reserved.)
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- 2022
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10. Combining quantitative ADF STEM with SiN x membrane-based MEMS devices: A simulation study with Pt nanoparticles.
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MacArthur KE, Clement A, Heggen M, and Dunin-Borkowski RE
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Computer simulations are used to assess the influence of a 20-nm-thick SiN
x membrane on the quantification of atomic-resolution annular dark-field (ADF) scanning transmission electron microscopy images of Pt nanoparticles. The discussions include the effect of different nanoparticle/membrane arrangements, accelerating voltage, nanoparticle thickness and the presence of adjacent atomic columns on the accuracy with which the number of Pt atoms in each atom column can be counted. The results, which are based on the use of ADF scattering cross-sections, show that an accuracy of better than a single atom is attainable at 200 and 300 kV. At 80kV, the scattering in a typical SiNx membrane is sufficiently strong that the best possible atom counting accuracy is reduced to +/- 2 atoms. The implications of the work for quantitative studies of Pt nanoparticles imaged through SiNx membranes are discussed., (Copyright © 2021. Published by Elsevier B.V.)- Published
- 2021
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11. Introduction to a special issue on Frontiers of Aberration Corrected Electron Microscopy in honour of Wolfgang Baumeister, Colin Humphreys, John Spence and Knut Urban on the occasion of their 75th, 80th, 75th and 80th birthdays.
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Dunin-Borkowski RE, Mayer J, Sachse C, and Tillmann K
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- History, 20th Century, Microscopy, Electron
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- 2021
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12. A sorter for electrons based on magnetic elements.
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Pozzi G, Rosi P, Tavabi AH, Karimi E, Dunin-Borkowski RE, and Grillo V
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The orbital angular momentum (OAM) sorter is an electron optical device for the measurement of an electron's OAM. It is based on two phase elements, which are referred to as an "unwrapper" and a "corrector" and are located in Fourier conjugate planes. The simplest implementation of the sorter is based on electrostatic phase elements, such as a charged needle for the unwrapper and electrodes with alternating charges or potentials for the corrector. Here, we use a formal analogy between phase shifts introduced by charges and vertical currents to propose alternative designs for the sorter elements, which are based on phase shifts introduced by magnetic fields. We use this concept to provide a general guide for phase element design, which promises to provide improved reliability of phase control in electron optics., (Copyright © 2021. Published by Elsevier B.V.)
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- 2021
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13. Efficient large field of view electron phase imaging using near-field electron ptychography with a diffuser.
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Allars F, Lu PH, Kruth M, Dunin-Borkowski RE, Rodenburg JM, and Maiden AM
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Most implementations of ptychography on the electron microscope operate in scanning transmission (STEM) mode, where a small focussed probe beam is rapidly scanned across the sample. In this paper we introduce a different approach based on near-field ptychography, where the focussed beam is replaced by a wide-field, structured illumination, realised through a purpose-designed etched Silicon Nitride window. We show that fields of view as large as 100 μm
2 can be imaged using the new approach, and that quantitative electron phase images can be reconstructed from as few as nine near-field diffraction pattern measurements., (Copyright © 2021. Published by Elsevier B.V.)- Published
- 2021
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14. Extraction of 3D quantitative maps using EDS-STEM tomography and HAADF-EDS bimodal tomography.
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Yuan Y, MacArthur KE, Collins SM, Brodusch N, Voisard F, Dunin-Borkowski RE, and Gauvin R
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Electron tomography has been widely applied to three-dimensional (3D) morphology characterization and chemical analysis at the nanoscale. A HAADF-EDS bimodal tomographic (HEBT) reconstruction technique has been developed to extract high resolution element-specific information. However, the reconstructed elemental maps cannot be directly converted to quantitative compositional information. In this work, we propose a quantification approach for obtaining elemental weight fraction maps from the HEBT reconstruction technique using the physical parameters extracted from a Monte Carlo code, MC X-ray. A similar quantification approach is proposed for the EDS-STEM tomographic reconstruction. The performance of the two quantitative reconstruction methods, using the simultaneous iterative reconstruction technique, are evaluated and compared for a simulated dataset of a two-dimensional phantom sample. The effects of the reconstruction parameters including the number of iterations and the weight of the HAADF signal are discussed. Finally, the two approaches are applied to an experimental dataset to show the 3D structure and quantitative elemental maps of a particle of flux melted metal-organic framework glass., (Copyright © 2020 Elsevier B.V. All rights reserved.)
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- 2021
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15. A cartridge-based turning specimen holder with wireless tilt angle measurement for magnetic induction mapping in the transmission electron microscope.
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Diehle P, Kovács A, Duden T, Speen R, Žagar Soderžnik K, and Dunin-Borkowski RE
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Magnetic induction mapping in the transmission electron microscope using phase contrast techniques such as off-axis electron holography and differential phase contrast imaging often requires the separation of the magnetic contribution to the recorded signal from the electrostatic contribution. When using off-axis electron holography, one of the experimental approaches that can be used to achieve this separation is to evaluate half of the difference between phase shift images that have been recorded before and after turning the sample over. Here, we introduce a cartridge-based sample mounting system, which is based on an existing on-axis tomography specimen holder and can be used to turn a sample over inside the electron microscope, thereby avoiding the need to remove the holder from the microscope to turn the sample over manually. We present three cartridge designs, which are compatible with all pole piece designs and can be used to support conventional 3-mm-diameter sample grids, Si
3 N4 -based membrane chips and needle-shaped specimens. We make use of a wireless inclinometer that has a precision of 0.1° to monitor the sample holder tilt angle independently of the microscope goniometer readout. We also highlight the need to remove geometrical image distortions when aligning pairs of phase shift images that have been recorded before and after turning the sample over. The capabilities of the cartridge-based specimen holder and the turning approach are demonstrated by using off-axis electron holography to record magnetic induction maps of lithographically-patterned soft magnetic Co elements, a focused ion beam milled hard magnetic Nd-Fe-B lamella and an array of four Fe3 O4 nanocrystals., (Copyright © 2020 The Authors. Published by Elsevier B.V. All rights reserved.)- Published
- 2021
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16. Corrigendum to "Spherical aberration correction in a scanning transmission electron microscope using a sculpted thin film" [Ultramicroscopy 189 (2018) 46-53].
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Shiloh R, Remez R, Lu PH, Jin L, Lereah Y, Tavabi AH, Dunin-Borkowski RE, and Arie A
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- 2020
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17. Direct measurement of electrostatic potentials at the atomic scale: A conceptual comparison between electron holography and scanning transmission electron microscopy.
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Winkler F, Barthel J, Dunin-Borkowski RE, and Müller-Caspary K
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Off-axis electron holography and first moment STEM are sensitive to electromagnetic potentials or fields, respectively. In this work, we investigate in what sense the results obtained from both techniques are equivalent and work out the major differences. The analysis is focused on electrostatic (Coulomb) potentials at atomic spatial resolution. It is shown that the probe-forming/objective aperture strongly affects the reconstructed electrostatic potentials and that, as a result of the different illumination setups, dynamical diffraction effects show a specific response with increasing specimen thickness. It is shown that thermal diffuse scattering is negligible for a wide range of specimen thicknesses, when evaluating the first moment of diffraction patterns., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier B.V. All rights reserved.)
- Published
- 2020
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18. Design of electrostatic phase elements for sorting the orbital angular momentum of electrons.
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Pozzi G, Grillo V, Lu PH, Tavabi AH, Karimi E, and Dunin-Borkowski RE
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The orbital angular momentum (OAM) sorter is a new electron optical device for measuring an electron's OAM. It is based on two phase elements, which are referred to as the "unwrapper" and "corrector" and are placed in Fourier-conjugate planes in an electron microscope. The most convenient implementation of this concept is based on the use of electrostatic phase elements, such as a charged needle as the unwrapper and a set of electrodes with alternating charges as the corrector. Here, we use simulations to assess the role of imperfections in such a device, in comparison to an ideal sorter. We show that the finite length of the needle and the boundary conditions introduce astigmatism, which leads to detrimental cross-talk in the OAM spectrum. We demonstrate that an improved setup comprising three charged needles can be used to compensate for this aberration, allowing measurements with a level of cross-talk in the OAM spectrum that is comparable to the ideal case., (Copyright © 2019 Elsevier B.V. All rights reserved.)
- Published
- 2020
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19. Introduction to a special issue on Frontiers of Aberration Corrected Electron Microscopy in honour of Christian Colliex, Archie Howie and Hannes Lichte on the occasion of their 75th, 85th and 75th birthdays.
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Dunin-Borkowski RE, Mayer J, Sachse C, and Tillmann K
- Published
- 2019
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20. Quantitative measurement of nanoscale electrostatic potentials and charges using off-axis electron holography: Developments and opportunities.
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McCartney MR, Dunin-Borkowski RE, and Smith DJ
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Off-axis electron holography has evolved into a powerful electron-microscopy-based technique for characterizing electromagnetic fields with nanometer-scale resolution. In this paper, we present a review of the application of off-axis electron holography to the quantitative measurement of electrostatic potentials and charge density distributions. We begin with a short overview of the theoretical and experimental basis of the technique. Practical aspects of phase imaging, sample preparation and microscope operation are outlined briefly. Applications of off-axis electron holography to a wide range of materials are then described in more detail. Finally, challenges and future opportunities for electron holography investigations of electrostatic fields and charge density distributions are presented., (Copyright © 2019. Published by Elsevier B.V.)
- Published
- 2019
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21. Nanoscale measurement of giant saturation magnetization in α″-Fe 16 N 2 by electron energy-loss magnetic chiral dichroism.
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Chen X, Higashikozono S, Ito K, Jin L, Ho PL, Yu CP, Tai NH, Mayer J, Dunin-Borkowski RE, Suemasu T, and Zhong X
- Abstract
Metastable α″-Fe
16 N2 thin films were reported to have a giant saturation magnetization of above 2200 emu/cm3 in 1972 and have been considered as candidates for next-generation rare-earth-free permanent magnetic materials. However, their magnetic properties have not been confirmed unequivocally. As a result of the limited spatial resolution of most magnetic characterization techniques, it is challenging to measure the saturation magnetization of the α″-Fe16 N2 phase, as it is often mixed with the parent α'-Fe8 N phase in thin films. Here, we use electron energy-loss magnetic chiral dichroism (EMCD), aberration-corrected transmission electron microscopy, X-ray diffraction and macroscopic magnetic measurements to study α″-Fe16 N2 (containing ordered N atoms) and α'-Fe8 N (containing disordered N atoms). The ratio of saturation magnetization in α″-Fe16 N2 to that in α'-Fe8 N is determined to be 1.31 ± 0.10 from quantitative EMCD measurements and dynamical diffraction calculations, confirming the giant saturation magnetization of α″-Fe16 N2 . Crystallographic information is also obtained about the two phases, which are mixed on the nanoscale., (Copyright © 2019 Elsevier B.V. All rights reserved.)- Published
- 2019
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22. A single slice approach for simulating two-beam electron diffraction of nanocrystals.
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Gontard LC, Barroso-Bogeat A, Dunin-Borkowski RE, and Calvino JJ
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A simple computational method that can be used to simulate TEM image contrast of an electron beam diffracted by a crystal under two-beam dynamical scattering conditions is presented. The approach based on slicing the shape factor is valid for a general crystal morphology, with and without crystalline defects, avoids the column approximation, and provides the complex exit wave at the focal and the image planes also under weak-beam conditions. The approach is particularly efficient for large crystals and the 3D model required for the calculations can be measured experimentally using electron tomography. The method is applied to show that the shape of a diffracted spot can be affected by shifts, broadening and secondary maxima of appreciable intensity, even for a perfect crystal. The methodology is extended for the case of electron precession diffraction, and to show how can be used to improve nanometrology from diffraction patterns. The method is used also to perform simulations of simple models of crystalline defects. The accuracy of the method is demonstrated through examples of experimental and simulated dark-field images of MgO and ZrO
2 nanocrystals and thin layers of CeO2 ., (Copyright © 2018 Elsevier B.V. All rights reserved.)- Published
- 2018
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23. Blind identification of magnetic signals in electron magnetic chiral dichroism using independent component analysis.
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Spiegelberg J, Song D, Dunin-Borkowski RE, Zhu J, and Rusz J
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Electron magnetic chiral dichroism (EMCD) is a promising technique to investigate local magnetic structures in the electron microscope. However, recognition of the EMCD signal, or also finding optimal parameter settings for given materials and sample orientations typically requires extensive simulations to aid the experiment. Here, we discuss how modern data processing techniques, in particular independent component analysis, can be used to identify magnetic signals in an unsupervised manner from energy filtered transmission electron microscopy (EFTEM) images. On the background of the recent advent of 4D scanning transmission electron microscopy, we discuss how this data processing may enable simultaneous tracking of all three spatial components of the magnetic momenta for arbitrary materials and several sample orientations without the previous need of complementary simulations., (Copyright © 2018. Published by Elsevier B.V.)
- Published
- 2018
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24. Effect of cation ratio and order on magnetic circular dichroism in the double perovskite Sr 2 Fe 1+ x Re 1- x O 6 .
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Ho PL, Yu CP, Zhang Q, Song K, Buban JP, Choi SY, Dunin-Borkowski RE, Mayer J, Tai NH, Zhu J, Jin L, and Zhong X
- Abstract
Superexchange-based magnetic coupling of the two B-site cations in rock-salt-ordered double perovskite oxides is extremely sensitive to the cation ratio and degree of order. However, as a result of the limited spatial resolution of most magnetic characterization techniques, it is challenging to establish a direct relationship between magnetic properties and structure in these materials, including the effects of elemental segregation and cation disorder. Here, we use electron energy-loss magnetic chiral dichroism together with aberration-corrected electron microscopy and spectroscopy to record magnetic circular dichroism (MCD) spectra at the nm scale, in combination with structural and chemical information at the atomic scale from the very same region. We study nanoscale phases in ordered Sr
2 [Fe][Re]O6 , ordered Sr2 [Fe][Fe1/5 Re4/5 ]O6 and disordered Sr[Fe4/5 Re1/5 ]O3 individually, in order to understand the role of cation ratio and order on local magnetic coupling. When compared with ordered Sr2 [Fe][Re]O6 , we find that antiferromagnetic Fe3+ -O2- -Fe3+ superexchange interactions arising from an excess of Fe suppress the MCD signal from Fe cations in ordered Sr2 [Fe][Fe1/5 Re4/5 ]O6 , while dominant Fe3+ -O2- -Fe3+ antiferromagnetic coupling in disordered Sr[Fe4/5 Re1/5 ]O3 leads to a decrease in MCD signal down to the noise level. Our work demonstrates a protocol that can be used to correlate crystallographic, electronic and magnetic information in materials such as Sr2 Fe1+ x Re1- x O6 , in order to provide insight into structure-property relationships in double perovskite oxides at the atomic scale., (Copyright © 2018 Elsevier B.V. All rights reserved.)- Published
- 2018
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25. Spherical aberration correction in a scanning transmission electron microscope using a sculpted thin film.
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Shiloh R, Remez R, Lu PH, Jin L, Lereah Y, Tavabi AH, Dunin-Borkowski RE, and Arie A
- Abstract
Nearly eighty years ago, Scherzer showed that rotationally symmetric, charge-free, static electron lenses are limited by an unavoidable, positive spherical aberration. Following a long struggle, a major breakthrough in the spatial resolution of electron microscopes was reached two decades ago by abandoning the first of these conditions, with the successful development of multipole aberration correctors. Here, we use a refractive silicon nitride thin film to tackle the second of Scherzer's constraints and demonstrate an alternative method for correcting spherical aberration in a scanning transmission electron microscope. We reveal features in Si and Cu samples that cannot be resolved in an uncorrected microscope. Our thin film corrector can be implemented as an immediate low cost upgrade to existing electron microscopes without re-engineering of the electron column or complicated operation protocols and can be extended to the correction of additional aberrations., (Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.)
- Published
- 2018
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26. Fine electron biprism on a Si-on-insulator chip for off-axis electron holography.
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Duchamp M, Girard O, Pozzi G, Soltner H, Winkler F, Speen R, Dunin-Borkowski RE, and Cooper D
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Off-axis electron holography allows both the amplitude and the phase shift of an electron wavefield propagating through a specimen in a transmission electron microscope to be recovered. The technique requires the use of an electron biprism to deflect an object wave and a reference wave to form an interference pattern. Here, we introduce an approach based on semiconductor processing technology to fabricate fine electron biprisms with rectangular cross-sections. By performing electrostatic calculations and preliminary experiments, we demonstrate that such biprisms promise improved performance for electron holography experiments., (Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.)
- Published
- 2018
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27. Generation of electron vortex beams using line charges via the electrostatic Aharonov-Bohm effect.
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Pozzi G, Lu PH, Tavabi AH, Duchamp M, and Dunin-Borkowski RE
- Abstract
It has recently been shown that an electron vortex beam can be generated by the magnetic field surrounding the tip of a dipole-like magnet. This approach can be described using the magnetic Aharonov-Bohm effect and is associated with the fact that the end of a long magnetic rod can be treated approximately as a magnetic monopole. However, it is difficult to vary the magnetisation of the rod in such a setup and the electron beam vorticity is fixed for a given tip shape. Here, we show how a similar behaviour, which has the advantage of easy tuneability, can be achieved by making use of the electrostatic Aharonov-Bohm effect associated with an electrostatic dipole line. We highlight the analogies between the magnetic and electrostatic cases and use simulations of in-focus, Fresnel and Fraunhofer images to show that a device based on two parallel, oppositely charged lines that each have a constant charge density can be used to generate a tuneable electron vortex beam. We assess the effect of using a dipole line that has a finite length and show that if the charge densities on the two lines are different then an additional biprism-like effect is superimposed on the electron-optical phase., (Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.)
- Published
- 2017
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28. Prospects for quantitative and time-resolved double and continuous exposure off-axis electron holography.
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Migunov V, Dwyer C, Boothroyd CB, Pozzi G, and Dunin-Borkowski RE
- Abstract
The technique of double exposure electron holography, which is based on the superposition of two off-axis electron holograms, was originally introduced before the availability of digital image processing to allow differences between electron-optical phases encoded in two electron holograms to be visualised directly without the need for holographic reconstruction. Here, we review the original method and show how it can now be extended to permit quantitative studies of phase shifts that oscillate in time. We begin with a description of the theory of off-axis electron hologram formation for a time-dependent electron wave that results from the excitation of a specimen using an external stimulus with a square, sinusoidal, triangular or other temporal dependence. We refer to the more general method as continuous exposure electron holography, present preliminary experimental measurements and discuss how the technique can be used to image electrostatic potentials and magnetic fields during high frequency switching experiments., (Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.)
- Published
- 2017
- Full Text
- View/download PDF
29. Quantitative measurement of mean inner potential and specimen thickness from high-resolution off-axis electron holograms of ultra-thin layered WSe 2 .
- Author
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Winkler F, Tavabi AH, Barthel J, Duchamp M, Yucelen E, Borghardt S, Kardynal BE, and Dunin-Borkowski RE
- Abstract
The phase and amplitude of the electron wavefunction that has passed through ultra-thin flakes of WSe
2 is measured from high-resolution off-axis electron holograms. Both the experimental measurements and corresponding computer simulations are used to show that, as a result of dynamical diffraction, the spatially averaged phase does not increase linearly with specimen thickness close to an [001] zone axis orientation even when the specimen has a thickness of only a few layers. It is then not possible to infer the local specimen thickness of the WSe2 from either the phase or the amplitude alone. Instead, we show that the combined analysis of phase and amplitude from experimental measurements and simulations allows an accurate determination of the local specimen thickness. The relationship between phase and projected potential is shown to be approximately linear for extremely thin specimens that are tilted by several degrees in certain directions from the [001] zone axis. A knowledge of the specimen thickness then allows the electrostatic potential to be determined from the measured phase. By using this combined approach, we determine a value for the mean inner potential of WSe2 of 18.9±0.8V, which is 12% lower than the value calculated from neutral atom scattering factors., (Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.)- Published
- 2017
- Full Text
- View/download PDF
30. Introduction to a special issue on Frontiers of Aberration Corrected Electron Microscopy in honour of Robert Sinclair and Nestor J. Zaluzec on the occasion of their 70th and 65th birthdays.
- Author
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Dunin-Borkowski RE, Mayer J, and Tillmann K
- Published
- 2017
- Full Text
- View/download PDF
31. Automated discrete electron tomography - Towards routine high-fidelity reconstruction of nanomaterials.
- Author
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Zhuge X, Jinnai H, Dunin-Borkowski RE, Migunov V, Bals S, Cool P, Bons AJ, and Batenburg KJ
- Abstract
Electron tomography is an essential imaging technique for the investigation of morphology and 3D structure of nanomaterials. This method, however, suffers from well-known missing wedge artifacts due to a restricted tilt range, which limits the objectiveness, repeatability and efficiency of quantitative structural analysis. Discrete tomography represents one of the promising reconstruction techniques for materials science, potentially capable of delivering higher fidelity reconstructions by exploiting the prior knowledge of the limited number of material compositions in a specimen. However, the application of discrete tomography to practical datasets remains a difficult task due to the underlying challenging mathematical problem. In practice, it is often hard to obtain consistent reconstructions from experimental datasets. In addition, numerous parameters need to be tuned manually, which can lead to bias and non-repeatability. In this paper, we present the application of a new iterative reconstruction technique, named TVR-DART, for discrete electron tomography. The technique is capable of consistently delivering reconstructions with significantly reduced missing wedge artifacts for a variety of challenging data and imaging conditions, and can automatically estimate its key parameters. We describe the principles of the technique and apply it to datasets from three different types of samples acquired under diverse imaging modes. By further reducing the available tilt range and number of projections, we show that the proposed technique can still produce consistent reconstructions with minimized missing wedge artifacts. This new development promises to provide the electron microscopy community with an easy-to-use and robust tool for high-fidelity 3D characterization of nanomaterials., (Copyright © 2017 Elsevier B.V. All rights reserved.)
- Published
- 2017
- Full Text
- View/download PDF
32. Photogrammetry of the three-dimensional shape and texture of a nanoscale particle using scanning electron microscopy and free software.
- Author
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Gontard LC, Schierholz R, Yu S, Cintas J, and Dunin-Borkowski RE
- Abstract
We apply photogrammetry in a scanning electron microscope (SEM) to study the three-dimensional shape and surface texture of a nanoscale LiTi2(PO4)3 particle. We highlight the fact that the technique can be applied non-invasively in any SEM using free software (freeware) and does not require special sample preparation. Three-dimensional information is obtained in the form of a surface mesh, with the texture of the sample stored as a separate two-dimensional image (referred to as a UV Map). The mesh can be used to measure parameters such as surface area, volume, moment of inertia and center of mass, while the UV map can be used to study the surface texture using conventional image processing techniques. We also illustrate the use of 3D printing to visualize the reconstructed model., (Copyright © 2016 Elsevier B.V. All rights reserved.)
- Published
- 2016
- Full Text
- View/download PDF
33. Mapping the electrostatic potential of Au nanoparticles using hybrid electron holography.
- Author
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Ozsoy-Keskinbora C, Boothroyd CB, Dunin-Borkowski RE, van Aken PA, and Koch CT
- Abstract
Electron holography is a powerful technique for characterizing electrostatic potentials, charge distributions, electric and magnetic fields, strain distributions and semiconductor dopant distributions with sub-nm spatial resolution. Mapping internal electrostatic and magnetic fields within nanoparticles and other low-dimensional materials by TEM requires both high spatial resolution and high phase sensitivity. Carrying out such an analysis fully quantitatively is even more challenging, since artefacts such as dynamical electron scattering may strongly affect the measurement. In-line electron holography, one of the variants of electron holography, features high phase sensitivity at high spatial frequencies, but suffers from inefficient phase recovery at low spatial frequencies. Off-axis electron holography, in contrast, can recover low spatial frequency phase information much more reliably, but is less effective in retrieving phase information at high spatial frequencies when compared to in-line holography. We investigate gold nanoparticles using hybrid electron holography at both atomic-resolution and intermediate magnification. Hybrid electron holography is a novel technique that synergistically combines off-axis and in-line electron holography, allowing the measurement of the complex wave function describing the scattered electrons with excellent signal-to-noise properties at both high and low spatial frequencies. The effect of dynamical electron scattering is minimized by beam tilt averaging., (Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.)
- Published
- 2016
- Full Text
- View/download PDF
34. Performance of a direct detection camera for off-axis electron holography.
- Author
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Chang SLY, Dwyer C, Barthel J, Boothroyd CB, and Dunin-Borkowski RE
- Abstract
The performance of a direct detection camera (DDC) is evaluated in the context of off-axis electron holographic experiments in a transmission electron microscope. Its performance is also compared directly with that of a conventional charge-coupled device (CCD) camera. The DDC evaluated here can be operated either by the detection of individual electron events (counting mode) or by the effective integration of many such events during a given exposure time (linear mode). It is demonstrated that the improved modulation transfer functions and detective quantum efficiencies of both modes of the DDC give rise to significant benefits over the conventional CCD cameras, specifically, a significant improvement in the visibility of the holographic fringes and a reduction of the statistical error in the phase of the reconstructed electron wave function. The DDC's linear mode, which can handle higher dose rates, allows optimisation of the dose rate to achieve the best phase resolution for a wide variety of experimental conditions. For suitable conditions, the counting mode can potentially utilise a significantly lower dose to achieve a phase resolution that is comparable to that achieved using the linear mode. The use of multiple holograms and correlation techniques to increase the total dose in counting mode is also demonstrated., (Copyright © 2015. Published by Elsevier B.V.)
- Published
- 2016
- Full Text
- View/download PDF
35. Surface effects on mean inner potentials studied using density functional theory.
- Author
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Pennington RS, Boothroyd CB, and Dunin-Borkowski RE
- Abstract
Quantitative materials characterization using electron holography frequently requires knowledge of the mean inner potential, but reported experimental mean inner potential measurements can vary widely. Using density functional theory, we have simulated the mean inner potential for materials with a range of different surface conditions and geometries. We use both "thin-film" and "nanowire" specimen geometries. We consider clean bulk-terminated surfaces with different facets and surface reconstructions using atom positions from both structural optimization and experimental data and we also consider surfaces both with and without adsorbates. We find that the mean inner potential is surface-dependent, with the strongest dependency on surface adsorbates. We discuss the outlook and perspective for future mean inner potential measurements., (Copyright © 2015 Elsevier B.V. All rights reserved.)
- Published
- 2015
- Full Text
- View/download PDF
36. Tunable caustic phenomena in electron wavefields.
- Author
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Tavabi AH, Migunov V, Dwyer C, Dunin-Borkowski RE, and Pozzi G
- Abstract
Novel caustic phenomena, which contain fold, butterfly and elliptic umbilic catastrophes, are observed in defocused images of two approximately collinear oppositely biased metallic tips in a transmission electron microscope. The observed patterns depend sensitively on defocus, on the applied voltage between the tips and on their separation and lateral offset. Their main features are interpreted on the basis of a projected electrostatic potential model for the electron-optical phase shift., (Copyright © 2015 Elsevier B.V. All rights reserved.)
- Published
- 2015
- Full Text
- View/download PDF
37. On the origin of differential phase contrast at a locally charged and globally charge-compensated domain boundary in a polar-ordered material.
- Author
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MacLaren I, Wang L, McGrouther D, Craven AJ, McVitie S, Schierholz R, Kovács A, Barthel J, and Dunin-Borkowski RE
- Abstract
Differential phase contrast (DPC) imaging in the scanning transmission electron microscope is applied to the study of a charged antiphase domain boundary in doped bismuth ferrite. A clear differential signal is seen, which matches the expected direction of the electric field at the boundary. However, further study by scanned diffraction reveals that there is no measurable deflection of the primary diffraction disc and hence no significant free E-field in the material. Instead, the DPC signal arises from a modulation of the intensity profile within the primary diffraction disc in the vicinity of the boundary. Simulations are used to show that this modulation arises purely from the local change in crystallographic structure at the boundary and not from an electric field. This study highlights the care that is required when interpreting signals recorded from ferroelectric materials using both DPC imaging and other phase contrast techniques., (Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.)
- Published
- 2015
- Full Text
- View/download PDF
38. Towards quantitative electrostatic potential mapping of working semiconductor devices using off-axis electron holography.
- Author
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Yazdi S, Kasama T, Beleggia M, Samaie Yekta M, McComb DW, Twitchett-Harrison AC, and Dunin-Borkowski RE
- Abstract
Pronounced improvements in the understanding of semiconductor device performance are expected if electrostatic potential distributions can be measured quantitatively and reliably under working conditions with sufficient sensitivity and spatial resolution. Here, we employ off-axis electron holography to characterize an electrically-biased Si p-n junction by measuring its electrostatic potential, electric field and charge density distributions under working conditions. A comparison between experimental electron holographic phase images and images obtained using three-dimensional electrostatic potential simulations highlights several remaining challenges to quantitative analysis. Our results illustrate how the determination of reliable potential distributions from phase images of electrically biased devices requires electrostatic fringing fields, surface charges, specimen preparation damage and the effects of limited spatial resolution to be taken into account., (Copyright © 2014 Elsevier B.V. All rights reserved.)
- Published
- 2015
- Full Text
- View/download PDF
39. Optimising electron holography in the presence of partial coherence and instrument instabilities.
- Author
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Chang SLY, Dwyer C, Boothroyd CB, and Dunin-Borkowski RE
- Abstract
Off-axis electron holography provides a direct means of retrieving the phase of the wavefield in a transmission electron microscope, enabling measurement of electric and magnetic fields at length scales from microns to nanometers. To maximise the accuracy of the technique, it is important to acquire holograms using experimental conditions that optimise the phase resolution for a given spatial resolution. These conditions are determined by a number of competing parameters, especially the spatial coherence and the instrument instabilities. Here, we describe a simple, yet accurate, model for predicting the dose rate and exposure time that give the best phase resolution in a single hologram. Experimental studies were undertaken to verify the model of spatial coherence and instrument instabilities that are required for the optimisation. The model is applicable to electron holography in both standard mode and Lorentz mode, and it is relatively simple to apply., (Copyright © 2014 Elsevier B.V. All rights reserved.)
- Published
- 2015
- Full Text
- View/download PDF
40. Introduction to a Special Issue on Frontiers of Aberration Corrected Electron Microscopy dedicated to Harald Rose on the occasion of his 80th Birthday.
- Author
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Dunin-Borkowski RE, Mayer J, and Tillmann K
- Published
- 2015
- Full Text
- View/download PDF
41. Introduction to a special issue in honour of W. Owen Saxton, David J. Smith and Dirk Van Dyck on the occasion of their 65th birthdays.
- Author
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Dunin-Borkowski RE, Lichte H, Tillmann K, Van Aert S, and Van Tendeloo G
- Subjects
- Computer Simulation, History, 20th Century, History, 21st Century, Humans, Holography methods, Microscopy, Electron, Transmission methods, Optics and Photonics methods
- Published
- 2013
- Full Text
- View/download PDF
42. Geometric reconstruction methods for electron tomography.
- Author
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Alpers A, Gardner RJ, König S, Pennington RS, Boothroyd CB, Houben L, Dunin-Borkowski RE, and Joost Batenburg K
- Abstract
Electron tomography is becoming an increasingly important tool in materials science for studying the three-dimensional morphologies and chemical compositions of nanostructures. The image quality obtained by many current algorithms is seriously affected by the problems of missing wedge artefacts and non-linear projection intensities due to diffraction effects. The former refers to the fact that data cannot be acquired over the full 180° tilt range; the latter implies that for some orientations, crystalline structures can show strong contrast changes. To overcome these problems we introduce and discuss several algorithms from the mathematical fields of geometric and discrete tomography. The algorithms incorporate geometric prior knowledge (mainly convexity and homogeneity), which also in principle considerably reduces the number of tilt angles required. Results are discussed for the reconstruction of an InAs nanowire., (Copyright © 2013 Elsevier B.V. All rights reserved.)
- Published
- 2013
- Full Text
- View/download PDF
43. A simple algorithm for measuring particle size distributions on an uneven background from TEM images.
- Author
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Cervera Gontard L, Ozkaya D, and Dunin-Borkowski RE
- Subjects
- Image Processing, Computer-Assisted, X-Ray Diffraction, Algorithms, Microscopy, Electron, Transmission, Nanoparticles analysis, Particle Size
- Abstract
Nanoparticles have a wide range of applications in science and technology. Their sizes are often measured using transmission electron microscopy (TEM) or X-ray diffraction. Here, we describe a simple computer algorithm for measuring particle size distributions from TEM images in the presence of an uneven background. The approach is based on adaptive thresholding, making use of local threshold values that change with spatial coordinate. The algorithm allows particles to be detected and characterized with greater accuracy than using more conventional methods, in which a global threshold is used. Its application to images of heterogeneous catalysts is presented., (Copyright © 2010 Elsevier B.V. All rights reserved.)
- Published
- 2011
- Full Text
- View/download PDF
44. Quantitative electron holographic tomography for the 3D characterisation of semiconductor device structures.
- Author
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Twitchett-Harrison AC, Yates TJ, Dunin-Borkowski RE, and Midgley PA
- Abstract
Electron tomography and electron holography experiments have been combined to investigate the 3D electrostatic potential distribution in semiconductor devices. The experimental procedure for the acquisition and data reconstruction of holographic tilt series of silicon p-n junction specimens is described. A quantitative analysis of the experimental results from specimens of two different thicknesses is presented, revealing the 3D electrostatic potential variations arising from the presence of surfaces and damage generated by focused ion beam (FIB) sample preparation. Close to bulk-like properties are measured in the centre of the tomographic reconstruction of the specimen, revealing higher electrically active dopant concentrations compared to the measurements obtained at the specimen surfaces. A comparison of the experimental results from the different thickness specimens has revealed a 'critical' thickness for this specimen preparation method of 350nm that is required for this device structure to retain 'bulk'-like properties in the centre of the membrane.
- Published
- 2008
- Full Text
- View/download PDF
45. Conventional and back-side focused ion beam milling for off-axis electron holography of electrostatic potentials in transistors.
- Author
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Dunin-Borkowski RE, Newcomb SB, Kasama T, McCartney MR, Weyland M, and Midgley PA
- Abstract
Off-axis electron holography is used to characterize a linear array of transistors, which was prepared for examination in cross-sectional geometry in the transmission electron microscope (TEM) using focused ion beam (FIB) milling from the substrate side of the semiconductor device. The measured electrostatic potential is compared with results obtained from TEM specimens prepared using the more conventional 'trench' FIB geometry. The use of carbon coating to remove specimen charging effects, which result in electrostatic fringing fields outside 'trench' specimens, is demonstrated. Such fringing fields are not observed after milling from the substrate side of the device. Analysis of the measured holographic phase images suggests that the electrically inactive layer on the surface of each FIB-milled specimen typically has a thickness of 100 nm.
- Published
- 2005
- Full Text
- View/download PDF
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