Scanning Transmission Electron Microscopy

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1 Scanning Transmission Electron Microscopy

3 Scanning Transmission Electron Microscopy Imaging and Analysis Edited by Stephen J. Pennycook Peter D. Nellist 123

4 Editors Stephen J. Pennycook Materials Science and Technology Division Oak Ridge National Laboratory 1 Bethel Valley Road Oak Ridge, TN , USA pennycooksj@ornl.gov Peter D. Nellist Department of Materials University of Oxford Parks Road Oxford, OX1 3PH, UK peter.nellist@materials.ox.ac.uk ISBN e-isbn DOI / Springer New York Dordrecht Heidelberg London Springer Science+Business Media, LLC 2011 All rights reserved. This work may not be translated or copied in whole or in part without the written permission of the publisher (Springer Science+Business Media, LLC, 233 Spring Street, New York, NY 10013, USA), except for brief excerpts in connection with reviews or scholarly analysis. Use in connection with any form of information storage and retrieval, electronic adaptation, computer software, or by similar or dissimilar methodology now known or hereafter developed is forbidden. The use in this publication of trade names, trademarks, service marks, and similar terms, even if they are not identified as such, is not to be taken as an expression of opinion as to whether or not they are subject to proprietary rights. Printed on acid-free paper Springer is part of Springer Science+Business Media (

5 Preface Over the last two decades, scanning transmission electron microscopy (STEM) has become a very popular and widespread technique, with the number of publications and presentations making use of STEM techniques increasing by about an order of magnitude. Although the strengths of the technique for providing high-resolution structural and analytical information have been known and understood for much longer than that, the key to its more recent popularity has undoubtedly been the availability of STEM modes on instruments available from the major TEM manufacturers. Gone are the days when researchers wanting the unique capabilities of high-resolution STEM had to undertake the task of keeping a VG dedicated STEM instrument operating. Given the current interest in the technique, we felt that the time was right to review the current state of knowledge about STEM and STEM-related techniques and their application to a range of materials problems. The purpose of this volume is both to educate those who wish to deepen their understanding of STEM and to inform those who are seeking a review of the latest applications and methods associated with STEM. We are delighted that so many of our colleagues accepted our invitation to contribute to this volume, and we are indebted to them for their efforts in creating such excellent contributions. The following chapters illustrate how close STEM has brought us to the ultimate materials characterisation challenge of analysing materials atom by atom. We hope that the following chapters demonstrate the spectacular results that can be achieved when performing the relatively simple experiment of focusing a beam of electrons down to an atomic scale and measuring the scattering that results. Stephen J. Pennycook Peter D. Nellist v

7 Contents 1 A Scan Through the History of STEM 1 Stephen J. Pennycook 2 The Principles of STEM Imaging 91 Peter D. Nellist 3 The Electron Ronchigram 117 Andrew R. Lupini 4 Spatially Resolved EELS: The Spectrum-Imaging Technique and Its Applications 163 Mathieu Kociak, Odile Stéphan, Michael G. Walls, Marcel Tencé and Christian Colliex 5 Energy Loss Near-Edge Structures 207 Guillaume Radtke and Gianluigi A. Botton 6 Simulation and Interpretation of Images 247 Leslie J. Allen, Scott D. Findlay and Mark P. Oxley 7 X-Ray Energy-Dispersive Spectrometry in Scanning Transmission Electron Microscopes 291 Masashi Watanabe 8 STEM Tomography 353 Paul A. Midgley and Matthew Weyland 9 Scanning Electron Nanodiffraction and Diffraction Imaging 393 Jian-Min Zuo and Jing Tao 10 Applications of Aberration-Corrected Scanning Transmission Electron Microscopy and Electron Energy Loss Spectroscopy to Complex Oxide Materials 429 Maria Varela, Jaume Gazquez, Timothy J. Pennycook, Cesar Magen, Mark P. Oxley and Stephen J. Pennycook vii

8 viii Contents 11 Application to Ceramic Interfaces 467 Yuichi Ikuhara and Naoya Shibata 12 Application to Semiconductors 523 James M. LeBeau, Dmitri O. Klenov and Susanne Stemmer 13 Nanocharacterization of Heterogeneous Catalysts by Ex Situ and In Situ STEM 537 Peter A. Crozier 14 Structure of Quasicrystals 583 Eiji Abe 15 Atomic-Resolution STEM at Low Primary Energies 615 Ondrej L. Krivanek, Matthew F. Chisholm, Niklas Dellby and Matthew F. Murfitt 16 Low-Loss EELS in the STEM 659 Nigel D. Browning, Ilke Arslan, Rolf Erni and Bryan W. Reed 17 Variable Temperature Electron Energy-Loss Spectroscopy 689 Robert F. Klie, Weronika Walkosz, Guang Yang and Yuan Zhao 18 Fluctuation Microscopy in the STEM 725 Paul M. Voyles, Stephanie Bogle and John R. Abelson Index 757

9 Contributors Eiji Abe Department of Materials Science and Engineering, University of Tokyo, Tokyo, Japan John R. Abelson Department of Materials Science and Engineering, University of Illinois, Urbana-Champaign, IL, USA Leslie J. Allen School of Physics, University of Melbourne, Melbourne, VIC, Australia Ilke Arslan Department of Chemical Engineering and Materials Science, University of California-Davis, Davis, CA, USA Stephanie Bogle Department of Materials Science and Engineering, University of Illinois, Urbana-Champaign, IL, USA Gianluigi A. Botton Department of Materials Science and Engineering, McMaster University, Hamilton, ON, Canada Nigel D. Browning Departments of Chemical Engineering and Materials Science, Molecular and Cellular Biology, University of California-Davis, Davis, CA, USA; Physical and Life Sciences Directorate, Lawrence Livermore National Laboratory, Livermore, CA, USA Matthew F. Chisholm Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA Christian Colliex Laboratoire de Physique des Solides, CNRS/UMR8502, Université Paris-Sud, Orsay, France ix

10 x Contributors Peter A. Crozier School of Mechanical, Aerospace, Chemical and Materials Engineering, Arizona State University, Tempe, AZ, USA Niklas Dellby Nion Co., th St., Kirkland, WA, USA Rolf Erni Electron Microscopy Center, Empa, Swiss Federal Laboratories for Materials Science and Technology, Dubendorf, Switzerland Scott D. Findlay Institute of Engineering Innovation, The University of Tokyo, Tokyo, Japan Jaume Gazquez Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA; Departament de Física Aplicada III, University Complutense of Madrid, Madrid, Spain Yuichi Ikuhara Institute of Engineering Innovation, The University of Tokyo, Tokyo, Japan Dmitri O. Klenov FEI Company, Eindhoven, The Netherlands Robert F. Klie Department of Physics, University of Illinois, Chicago, IL, USA Mathieu Kociak Laboratoire de Physique des Solides, CNRS/UMR8502, Université Paris-Sud, Orsay, France Ondrej L. Krivanek Nion Co., th St., Kirkland, WA, USA James M. LeBeau Materials Department, University of California, Santa Barbara, CA, USA Andrew R. Lupini Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA Cesar Magen Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA; Instituto de Nanociencia de Aragon-ARAID and Departamento de Física de la Materia Condensada, Universidad de Zaragoza, Spain

11 Contributors xi Paul A. Midgley Department of Materials Science and Metallurgy, University of Cambridge, Cambridge, UK Matthew F. Murfitt Nion Co., th St., Kirkland, WA, USA Peter D. Nellist Department of Materials, University of Oxford, Oxford, UK Mark P. Oxley Department of Physics and Astronomy, Vanderbilt University, Nashville, TN, USA; Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA Stephen J. Pennycook Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA Timothy J. Pennycook Department of Physics and Astronomy, Vanderbilt University, Nashville, TN, USA; Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA Guillaume Radtke Institut Matériaux Microélectronique Nanoscience de Provence, UMR CNRS 6242, Université Paul Cézanne Aix-Marseille III, Marseille, France Bryan W. Reed Physical and Life Sciences Directorate, Lawrence Livermore National Laboratory, Livermore, CA, USA Naoya Shibata Institute of Engineering Innovation, The University of Tokyo, Tokyo, Japan Susanne Stemmer Materials Department, University of California, Santa Barbara, CA, USA Odile Stéphan Laboratoire de Physique des Solides, CNRS/UMR8502, Université Paris-Sud, Orsay, France Jing Tao Brookhaven National Laboratory, Upton, NY, USA

12 xii Contributors Marcel Tencé Laboratoire de Physique des Solides, CNRS/UMR8502, Université Paris-Sud, Orsay, France Maria Varela Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA; Departament de Física Aplicada III, University Complutense of Madrid, Madrid, Spain Paul M. Voyles Department of Materials Science and Engineering, University of Wisconsin, Madison, WI, USA Weronika Walkosz Department of Physics, University of Illinois, Chicago, IL, USA Michael G. Walls Laboratoire de Physique des Solides, CNRS/UMR8502, Université Paris-Sud, Orsay, France Masashi Watanabe Department of Materials Science and Engineering, Lehigh University, Bethlehem, PA, USA Matthew Weyland Monash Centre for Electron Microscopy, Monash University, Melbourne, VIC, Australia Guang Yang Department of Physics, University of Illinois, Chicago, IL, USA Yuan Zhao Department of Physics, University of Illinois, Chicago, IL, USA Jian-Min Zuo Department of Materials Science and Engineering and Frederick Seitz Materials Research Laboratory, University of Illinois at Urbana-Champaign, Urbana, IL, USA

Transportation Research, Economics and Policy

Transportation Research, Economics and Policy Series Editors David Gillen Werner Rothengatter For further volumes: http://www.springer.com/series/6647 David M. Levinson Henry X. Liu Michael Bell Editors