In-situ Electron Microscopy E-Book

• Herausgeber: Wiley-VCH
• Kategorie: Wissenschaft und neue Technologien
• Sprache: Englisch

Seitenzahl: 685

Veröffentlichungsjahr: 2012

Beschreibung

Adopting a didactical approach from fundamentals to actual experiments and applications, this handbook and ready reference covers
real-time observations using modern scanning electron microscopy and transmission electron microscopy, while also providing information
on the required stages and samples. The text begins with introductory material and the basics, before describing advancements and applications in dynamic transmission electron microscopy and reflection electron microscopy. Subsequently, the techniques needed to determine growth processes, chemical reactions and oxidation, irradiation effects, mechanical, magnetic, and ferroelectric properties as well as cathodoluminiscence and electromigration are discussed.

Leseprobe

Contents

Cover

Related Titles

Title Page

Copyright

List of Contributors

Preface

Part 1: Basics and Methods

Chapter 1: Introduction to Scanning Electron Microscopy

1.1 Components of the Scanning Electron Microscope

1.2 Electron–Matter Interaction

1.3 Contrast Mechanisms

1.4 Electron Backscattered Diffraction (EBSD)

1.5 Dispersive X-Ray Spectroscopy

1.6 Other Signals

1.7 Summary

References

Chapter 2: Conventional and Advanced Electron Transmission Microscopy

2.1 Introduction

2.2 High-Resolution Transmission Electron Microscopy

2.3 Conventional TEM of Defects in Crystals

2.4 Lorentz Microscopy

2.5 Off-Axis and Inline Electron Holography

2.6 Electron Diffraction Techniques

2.7 Convergent Beam Electron Diffraction

2.8 Scanning Transmission Electron Microscopy and Z-Contrast

2.9 Analytical TEM

References

Chapter 3: Dynamic Transmission Electron Microscopy

3.1 Introduction

3.2 How Does Single-Shot DTEM Work?

3.3 Experimental Applications of DTEM

3.4 Crystallization Under Far-from-Equilibrium Conditions

3.5 Space Charge Effects in Single-Shot DTEM

3.6 Next-Generation DTEM

3.7 Conclusions

Acknowledgments

References

Chapter 4: Formation of Surface Patterns Observed with Reflection Electron Microscopy

4.1 Introduction

4.2 Reflection Electron Microscopy

4.3 Silicon Substrate Preparation

4.4 Monatomic Steps

4.5 Step Bunching

4.6 Surface Reconstructions

4.7 Epitaxial Growth

4.8 Thermal Oxygen Etching

4.9 Conclusions

Acknowledgments

References

Part 2: Growth and Interactions

Chapter 5: Electron and Ion Irradiation

5.1 Introduction

5.2 The Physics of Irradiation

5.3 Radiation Defects in Solids

5.4 Setup in the Electron Microscope

5.5 Experiments

5.6 Outlook

5.7 Acknowledgments

References

Chapter 6: Observing Chemical Reactions Using Transmission Electron Microscopy

6.1 Introduction

6.2 Instrumentation

6.3 Types of Chemical Reaction Suitable for TEM Observation

6.4 Experimental Setup

6.5 Available Information Under Reaction Conditions

6.6 Limitations and Future Developments

Acknowledgements

References

Chapter 7: In-Situ TEM Studies of Vapor- and Liquid-Phase Crystal Growth

7.1 Introduction

7.2 Experimental Considerations

7.3 Vapor-Phase Growth Processes

7.4 Liquid-Phase Growth Processes

7.5 Summary

Acknowledgments

References

Chapter 8: In-Situ TEM Studies of Oxidation

8.1 Introduction

8.2 Experimental Approach

8.3 Oxidation Phenomena

8.4 Future Developments

8.5 Summary

References

Part 3: Mechanical Properties

Chapter 9: Mechanical Testing with the Scanning Electron Microscope

9.1 Introduction

9.2 Technical Requirements and Specimen Preparation

9.3 In-Situ Loading of Macroscopic Samples

9.4 In-Situ Loading of Micron-Sized Samples

9.5 Summary and Outlook

References

Chapter 10: In-Situ TEM Straining Experiments: Recent Progress in Stages and Small-Scale Mechanics

10.1 Introduction

10.2 Available Straining Techniques

10.3 Dislocation Mechanisms in Thermally Strained Metallic Films

10.4 Size-Dependent Dislocation Plasticity in Metals

10.5 Conclusions and Future Directions

Acknowledgments

References

Chapter 11: In-Situ Nanoindentation in the Transmission Electron Microscope

11.1 Introduction

11.2 Experimental Methodology

11.3 Example Studies

11.4 Conclusions

Acknowledgments

References

Part 4: Physical Properties

Chapter 12: Current-Induced Transport: Electromigration

12.1 Principles

12.2 Transmission Electron Microscopy

12.3 Secondary Electron Microscopy

12.4 X-Radiography Studies

12.5 Specialized Techniques

12.6 Comparison of In-Situ Methods

References

Chapter 13: Cathodoluminescence in Scanning and Transmission Electron Microscopies

13.1 Introduction

13.2 Principles of Cathodoluminsecence

13.3 Applications of CL in Scanning and Transmission Electron Microscopies

13.4 Concluding Remarks

References

Chapter 14: In-Situ TEM with Electrical Bias on Ferroelectric Oxides

14.1 Introduction

14.2 Experimental Details

14.3 Domain Polarization Switching

14.4 Grain Boundary Cavitation

14.5 Domain Wall Fracture

14.6 Antiferroelectric-to-Ferroelectric Phase Transition

14.7 Relaxor-to-Ferroelectric Phase Transition

Acknowledgments

References

Chapter 15: Lorentz Microscopy

15.1 Introduction

15.2 The In-Situ Creation of Magnetic Fields

15.3 Examples

15.4 Problems

15.5 Conclusions

Acknowledgments

References

Index

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List of Contributors

Florian Banhart

Université de Strasbourg

Institut de Physique et Chimie des Matériaux, UMR 7504

23 rue du Loess

67034 Strasbourg

France

Nigel D. Browning

Lawrence Livermore National Laboratory

Physical and Life Sciences Directorate

7000 East Avenue

Livermore

California 94550

USA

Geoffrey H. Campbell

Lawrence Livermore National Laboratory

Physical and Life Sciences Directorate

7000 East Avenue

Livermore

California 94550

USA

Gerhard Dehm

Austrian Academy of Sciences

Erich Schmid Institute of Materials Science

Jahnstr. 12

8700 Leoben

Austria

and

Montanuniversität Leoben

Department Materials Physics

Franz-Josef-Str. 18

8700 Leoben

Austria

Wayne D. Kaplan

Technion – Israel Institute of Technology

Department of Materials Engineering

Haifa 32000

Israel

Daniel Kiener

Montanuniversität Leoben

Department Materials Physics

Franz-Josef-Str. 18

8700 Leoben

Austria

Judy S. Kim

Lawrence Livermore National Laboratory

Physical and Life Sciences Directorate

7000 East Avenue

Livermore

California 94550

USA

and

University of California

Department of Chemical Engineering and Materials Science

One Shields Avenue

Davis

California 95616

USA

Wayne E. King

Lawrence Livermore National Laboratory

Physical and Life Sciences Directorate

7000 East Avenue

Livermore

California 94550

USA

Christoph Koch

Max-Planck-Institut für Metallforschung

Heisenbergstr. 3

70569 Stuttgart

Germany

Thomas LaGrange

Lawrence Livermore National Laboratory

Physical and Life Sciences Directorate

7000 East Avenue

Livermore

California 94550

USA

Alexander V. Latyshev

Siberian Branch of Russian Academy of Sciences

Institute of Semiconductor Physics

Prospect Lavrent'eva 13

630090 Novosibirsk

Russia

Marc Legros

CEMES-CNRS

29 Rue Jeanne Marvig

31055 Toulouse

France

Andrew M. Minor

University of California, Berkeley and National Center for Electron Microscopy

Department of Materials Science and Engineering, Lawrence Berkeley National Laboratory

One Cyclotron Road, MS 72

Berkeley

CA 94720

USA

Christian Motz

Österreichische Akademie der Wissenschaften

Erich Schmid Institut für Materialwissenschaft

Jahnstr. 12

8700 Leoben

Austria

Yutaka Ohno

Tohoku University

Institute for Materials Research

Katahira 2-1-1

Aoba-ku

Sendai 980-8577

Japan

Bryan W. Reed

Lawrence Livermore National Laboratory

Physical and Life Sciences Directorate

7000 East Avenue

Livermore

California 94550

USA

Frances M. Ross

IBM T. J. Watson Research Center

1101 Kitchawan Road

Yorktown Heights

NY 10598

USA

Christina Scheu

1Ludwig-Maximilians-Universität München

Department Chemie & Center for NanoScience (CeNS)

Butenandstr. 5-13, Gerhard-Ertl-Gebäude (Haus E)

81377 München

Germany

Renu Sharma

National Institute of Science and Technology

Center for Nanoscale Science and Technology

100 Bureau Drive

Gaithersburg

MD 20899-6201

USA

Ralph Spolenak

ETH Zurich

Laboratory of Nanometallurgy, Department of Material

Wolfgang-Pauli-Str. 10

8093 Zurich

Switzerland

Seiji Takeda

Osaka University

The Institute of Scientific and Industrial Research

Mihogaoka 8-1

Ibaraki

Osaka 567-0047

Japan

Xiaoli Tan

Iowa State University

Department of Materials Science and Engineering

2220 Hoover Hall

Ames

IA 50011

USA

Judith C. Yang

University of Pittsburgh

Department of Chemical and Petroleum Engineering

1249 Benedum Hall

Pittsburgh

PA 15261

USA

Guangwen Zhou

P. O. Box 6000

85 Murray Hill Road

Binghampton

NY 13902

USA

Josef Zweck

University of Regensburg

Physics Faculty

Physics Building Office Phy 7.3.05

93040 Regensburg

Germany

Preface

Today, transmission electron microscopy (TEM) represents one of the most important tools used to characterize materials. Electron diffraction provides information on the crystallographic structure of materials, conventional TEM with bright-field and dark-field imaging on their microstructure, high-resolution TEM on their atomic structure, scanning TEM on their elemental distributions, and analytical TEM on their chemical composition and bonding mechanisms. Each of these techniques is explained in detail in various textbooks on TEM techniques, including Transmission Electron Microscopy: A Textbook for Materials Science (D.B. Williams and C.B. Carter, Plenum Press, New York, 1996), and Transmission Electron Microscopy and Diffractometry of Materials (3rd edition, B. Fultz and J. M. Howe, Springer-Verlag, Berlin, Heidelberg, 2008).

Most interestingly, however, TEM also enables dynamical processes in materials to be studied through dedicated in-situ experiments. To watch changes occurring in a material of interest allows not only the development but also the refinement of models, so as to explain the underlying physics and chemistry of materials processes. The possibilities for in-situ experiments span from thermodynamics and kinetics (including chemical reactions, oxidation, and phase transformations) to mechanical, electrical, ferroelectric, and magnetic material properties, as well as materials synthesis.

The present book is focused on the state-of-the-art possibilities for performing dynamic experiments inside the electron microscope, with attention centered on TEM but including scanning electron microscopy (SEM). Whilst seeing is believing is one aspect of in-situ experiments in electron microscopy, the possibility to obtain quantitative data is of almost equal importance when accessing critical data in relation to physics, chemistry, and the materials sciences. The equipment needed to obtain quantitative data on various stimuli – such as temperature and gas flow for materials synthesis, load and displacement for mechanical properties, and electrical current and voltage for electrical properties, to name but a few examples – are described in the individual sections that relate to Growth and Interactions (Part Two), Mechanical Properties (Part Three), and Physical Properties (Part Four).

During the past decade, interest in in-situ electron microscopy experiments has grown considerably, due mainly to new developments in quantitative stages and micro-/nano-electromechanical systems (MEMS/NEMS) that provide a “lab on chip” platform which can fit inside the narrow space of the pole-pieces in the transmission electron microscope. In addition, the advent of imaging correctors that compensate for the spherical and, more recently, the chromatic aberration of electromagnetic lenses has not only increased the resolution of TEM but has also permitted the use of larger pole-piece gaps (and thus more space for stages inside the microscope), even when designed for imaging at atomic resolution. Another driving force of in-situ experimentation using electron probes has been the small length-scales that are accessible with focused ion beam/SEM platforms and TEM instruments. These are of direct relevance for nanocrystalline materials and thin-film structures with micrometer and nanometer dimensions, as well as for structural defects such as interfaces in materials.

This book provides an overview of dynamic experiments in electron microscopy, and is especially targeted at students, scientists, and engineers working in the fields of chemistry, physics, and the materials sciences. Although experience in electron microscopy techniques is not a prerequisite for readers, as the basic information on these techniques is summarized in the first two chapters of Part One, Basics and Methods, some basic knowledge would help to use the book to its full extent. Details of specialized in-situ methods, such as Dynamic TEM and Reflection Electron Microscopy are also included in Part One, to highlight the science which emanates from these fields.

Gerhard Dehm, Leoben, AustriaJames M. Howe, Charlottesville, USAJosef Zweck, Regensburg, GermanyJanuary 2012

Part I

Basics and Methods

Chapter 1

Introduction to Scanning Electron Microscopy

Christina Scheu and Wayne D. Kaplan

The scanning electron microscope is without doubt one of the most widely used characterization tools available to materials scientists and materials engineers. Today, modern instruments achieve amazing levels of resolution, and can be equipped with various accessories that provide information on local chemistry and crystallography. These data, together with the morphological information derived from the sample, are important when characterizing the microstructure of materials used in a wide number of applications. A schematic overview of the signals that are generated when an electron beam interacts with a solid sample, and which are used in the scanning electron microscope for microstructural characterization, is shown in Figure 1.1. The most frequently detected signals are high-energy backscattered electrons, low-energy secondary electrons and X-rays, while less common signals include Auger electrons, cathodoluminescence, and measurements of beam-induced current. The origin of these signals will be discussed in detail later in the chapter.

Figure 1.1 Schematic drawing of possible signals created when an incident electron beam interacts with a solid sample. Reproduced with permission from Ref. [4]; © 2008, John Wiley & Sons.

Due to the mechanisms by which the image is formed in the scanning electron microscope, the micrographs acquired often appear to be directly interpretable; that is, the contrast in the image is often directly associated with the microstructural features of the sample. Unfortunately, however, this may often lead to gross errors in the measurement of microstructural features, and in the interpretation of the microstructure of a material. At the same time, the fundamental mechanisms by which the images are formed in the scanning electron microscope are reasonably straightforward, and a little effort from the materials scientist or engineer in correlating the microstructural features detected by the imaging mechanisms makes the technique of scanning electron microscopy (SEM) being extremely powerful.

Unlike conventional optical microscopy or conventional transmission electron microscopy (TEM), in SEM a focused beam of electrons is rastered across the specimen, and the signals emitted from the specimen are collected as a function of position of the incident focused electron beam. As such, the final image is collected in a sequential manner across the surface of the sample. As the image in SEM is formed from signals emitted due to the interaction of a focused incident electron probe with the sample, two critical issues are involved in understanding SEM images, as well as in the correlated analytical techniques: (i) the nature of the incident electron probe; and (ii) the manner by which incident electrons interact with matter.

The electron–optical system in a scanning electron microscope is actually designed to demagnify rather than to magnify, in order to form the small incident electron probe which is then rastered across the specimen. As such, the size of the incident probe depends on the electron source (or gun), and the electromagnetic lens system which focuses the emitted electrons into a fine beam that then interacts with the sample. The probe size is the first parameter involved in defining the spatial resolution of the image, or of the analytical measurements. However, the signals (e.g., secondary electrons, backscattered electrons, X-rays) that are used to form the image emanate from regions in the sample that may be significantly larger than the diameter of the incident electron beam. Thus, electron–matter interaction must be understood, together with the diameter of the incident electron probe, to understand both the resolution and the contrast in the acquired image.

The aim of this chapter is to provide a fundamental introduction to SEM and its associated analytical techniques (further details are available in Refs [1–5]).

1.1 Components of the Scanning Electron Microscope

It is convenient to consider the major components of a scanning electron microscope as divided into four major sections (see Figure 1.2):

The electron source (or electron gun).The electromagnetic lenses, which are used to focus the electron beam and demagnify it into a small electron probe.The deflection system.The detectors, which are used to collect signals emitted from the sample.

Figure 1.2 Schematic drawing of the major components of a scanning electron microscope. The electron lenses and apertures are used to demagnify the electron beam that is emitted from the electron source into a small probe, and to control the beam current density. The demagnified beam is than scanned across the sample. Various detectors are used to register the signals arising from various electron–matter interactions.