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Edited by
Gerhard Dehm, James M. Howe,
and Josef Zweck
In-situ Electron Microscopy

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Edited by
Gerhard Dehm, James M. Howe,
and Josef Zweck
In-situ Electron Microscopy
Applications in Physics, Chemistry and Materials Science

The Editors All books published by Wiley-VCH are carefully
produced. Nevertheless, authors, editors, and pub-
Prof. Dr. Gerhard Dehm lisher do not warrant the information contained in
Montanuniversität Leoben these books, including this book, to be free of errors.
Dept. Materialphysik Readers are advised to keep in mind that statements,
Jahnstr. 12 data, illustrations, procedural details or other items
8700 Leoben may inadvertently be inaccurate.
Austria
Library of Congress Card No.: applied for
Prof. Dr. James M. Howe British Library Cataloguing-in-Publication Data

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116 Engineer's Way
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V
Contents
List of Contributors XIII

Preface XVII
Part I Basics and Methods 1
1 Introduction to Scanning Electron Microscopy 3

Christina Scheu and Wayne D. Kaplan
1.1 Components of the Scanning Electron Microscope 4
1.1.1 Electron Guns 6
1.1.2 Electromagnetic Lenses 9
1.1.3 Deflection System 13
1.1.4 Electron Detectors 13
1.1.4.1 Everhart–Thornley Detector 13
1.1.4.2 Scintillator Detector 15
1.1.4.3 Solid-State Detector 16
1.1.4.4 In-Lens or Through-the-Lens Detectors 16
1.2 Electron–Matter Interaction 16
1.2.1 Backscattered Electrons (BSEs) 20
1.2.2 Secondary Electrons (SEs) 22
1.2.3 Auger Electrons (AEs) 25
1.2.4 Emission of Photons 25
1.2.4.1 Emission of X-Rays 25
1.2.4.2 Emission of Visible Light 26
1.2.5 Interaction Volume and Resolution 26
1.2.5.1 Secondary Electrons 27
1.2.5.2 Backscattered Electrons 27
1.2.5.3 X-Rays 27
1.3 Contrast Mechanisms 28
1.3.1 Topographic Contrast 28
1.3.2 Composition Contrast 31
1.3.3 Channeling Contrast 31
VI Contents
1.4 Electron Backscattered Diffraction (EBSD) 31

1.5 Dispersive X-Ray Spectroscopy 34
1.6 Other Signals 36
1.7 Summary 36
References 37
2 Conventional and Advanced Electron Transmission Microscopy 39

Christoph Koch
2.1 Introduction 39
2.1.1 Introductory Remarks 39
2.1.2 Instrumentation and Basic Electron Optics 40
2.1.3 Theory of Electron–Specimen Interaction 42
2.2 High-Resolution Transmission Electron Microscopy 48
2.3 Conventional TEM of Defects in Crystals 54
2.4 Lorentz Microscopy 55
2.5 Off-Axis and Inline Electron Holography 57
2.6 Electron Diffraction Techniques 59
2.6.1 Fundamentals of Electron Diffraction 59
2.7 Convergent Beam Electron Diffraction 61
2.7.1 Large-Angle Convergent Beam Electron Diffraction 63
2.7.2 Characterization of Amorphous Structures by Diffraction 63
2.8 Scanning Transmission Electron Microscopy and Z-Contrast 63
2.9 Analytical TEM 66
References 67
3 Dynamic Transmission Electron Microscopy 71

Thomas LaGrange, Bryan W. Reed, Wayne E. King,
Judy S. Kim, and Geoffrey H. Campbell
3.1 Introduction 71
3.2 How Does Single-Shot DTEM Work? 72
3.2.1 Current Performance 74
3.2.2 Electron Sources and Optics 75
3.2.3 Arbitrary Waveform Generation Laser System 80
3.2.4 Acquiring High Time Resolution Movies 81
3.3 Experimental Applications of DTEM 82
3.3.1 Diffusionless First-Order Phase Transformations 82
3.3.2 Observing Transient Phenomena in Reactive Multilayer Foils 85
3.4 Crystallization Under Far-from-Equilibrium Conditions 88
3.5 Space Charge Effects in Single-Shot DTEM 90
3.5.1 Global Space Charge 90
3.5.2 Stochastic Blurring 91
3.6 Next-Generation DTEM 91
3.6.1 Novel Electron Sources 91
3.6.2 Relativistic Beams 92
3.6.3 Pulse Compression 93
Contents VII
3.6.4 Aberration Correction 93

3.7 Conclusions 94
References 95
4 Formation of Surface Patterns Observed with Reflection

Electron Microscopy 99
Alexander V. Latyshev
4.1 Introduction 99
4.2 Reflection Electron Microscopy 102
4.3 Silicon Substrate Preparation 107
4.4 Monatomic Steps 109
4.5 Step Bunching 111
4.6 Surface Reconstructions 114
4.7 Epitaxial Growth 115
4.8 Thermal Oxygen Etching 116
4.9 Conclusions 119
References 119
Part II Growth and Interactions 123
5 Electron and Ion Irradiation 125

Florian Banhart
5.1 Introduction 125
5.2 The Physics of Irradiation 126
5.2.1 Scattering of Energetic Particles in Solids 126
5.2.2 Scattering of Electrons 128
5.2.3 Scattering of Ions 129
5.3 Radiation Defects in Solids 129
5.3.1 The Formation of Defects 129
5.3.2 The Migration of Defects 130
5.4 The Setup in the Electron Microscope 131
5.4.1 Electron Irradiation 131
5.4.2 Ion Irradiation 132
5.5 Experiments 132
5.5.1 Electron Irradiation 133
5.5.2 Ion Irradiation 140
5.6 Outlook 141
References 142
6 Observing Chemical Reactions Using Transmission Electron

Microscopy 145
Renu Sharma
6.2 Instrumentation 146
6.3 Types of Chemical Reaction Suitable for TEM Observation 150
VIII Contents
6.3.1 Oxidation and Reduction (Redox) Reactions 150

6.3.2 Phase Transformations 151
6.3.3 Polymerization 151
6.3.4 Nitridation 152
6.3.5 Hydroxylation and Dehydroxylation 152
6.3.6 Nucleation and Growth of Nanostructures 153
6.4 Experimental Setup 154
6.4.1 Reaction of Ambient Environment with Various TEM Components 154
6.4.2 Reaction of Grid/Support Materials with the Sample or with
Each Other 154
6.4.3 Temperature and Pressure Considerations 155
6.4.4 Selecting Appropriate Characterization Technique(s) 156
6.4.5 Recording Media 156
6.4.6 Independent Verification of the Results, and the Effects of the
Electron Beam 157
6.5 Available Information Under Reaction Conditions 157
6.5.1 Structural Modification 158
6.5.1.1 Electron Diffraction 158
6.5.1.2 High-Resolution Imaging 158
6.5.2 Chemical Changes 161
6.5.3 Reaction Rates (Kinetics) 164
6.6 Limitations and Future Developments 164
References 165
7 In-Situ TEM Studies of Vapor- and Liquid-Phase Crystal Growth 171

Frances M. Ross
7.2 Experimental Considerations 172
7.2.1 What Crystal Growth Experiments are Possible? 172
7.2.2 How Can These Experiments be Made Quantitative? 173
7.2.3 How Relevant Can These Experiments Be? 175
7.3 Vapor-Phase Growth Processes 175
7.3.1 Quantum Dot Growth Kinetics 176
7.3.2 Vapor–Liquid–Solid Growth of Nanowires 177
7.3.3 Nucleation Kinetics in Nanostructures 180
7.4 Liquid-Phase Growth Processes 183
7.4.1 Observing Liquid Samples Using TEM 183
7.4.2 Electrochemical Nucleation and Growth in the TEM System 184
7.5 Summary 187
References 188
8 In-Situ TEM Studies of Oxidation 191

Guangwen Zhou and Judith C. Yang
8.2 Experimental Approach 192
Contents IX
8.2.1 Environmental Cells 192

8.2.2 Surface and Environmental Conditions 193
8.2.3 Gas-Handling System 194
8.2.4 Limitations 195
8.3 Oxidation Phenomena 196
8.3.1 Surface Reconstruction 196
8.3.2 Nucleation and Initial Oxide Growth 197
8.3.3 Role of Surface Defects on Surface Oxidation 198
8.3.4 Shape Transition During Oxide Growth in Alloy Oxidation 199
8.3.5 Effect of Oxygen Pressure on the Orientations of Oxide Nuclei 202
8.3.6 Oxidation Pathways Revealed by High-Resolution TEM Studies
of Oxidation 203
8.4 Future Developments 205
8.5 Summary 206
References 206
Part III Mechanical Properties 209
9 Mechanical Testing with the Scanning Electron Microscope 211

Christian Motz
9.2 Technical Requirements and Specimen Preparation 212
9.3 In-Situ Loading of Macroscopic Samples 214
9.3.1 Static Loading in Tension, Compression, and Bending 214
9.3.2 Dynamic Loading in Tension, Compression, and Bending 216
9.3.3 Applications of In-Situ Testing 216
9.4 In-Situ Loading of Micron-Sized Samples 217
9.4.1 Static Loading of Micron-Sized Samples in Tension, Compression,
and Bending 218
9.4.2 Applications of In-Situ Testing of Small-Scale Samples 220
9.4.3 In-Situ Microindentation and Nanoindentation 222
9.5 Summary and Outlook 223
References 223
10 In-Situ TEM Straining Experiments: Recent Progress in Stages

and Small-Scale Mechanics 227
Gerhard Dehm, Marc Legros, and Daniel Kiener
10.2 Available Straining Techniques 228
10.2.1 Thermal Straining 228
10.2.2 Mechanical Straining 229
10.2.3 Instrumented Stages and MEMS/NEMS Devices 230
10.3 Dislocation Mechanisms in Thermally Strained Metallic Films 233
10.3.1 Basic Concepts 233
10.3.2 Dislocation Motion in Single Crystalline Films and Near Interfaces 235
X Contents
10.3.3 Dislocation Nucleation and Multiplication in Thin Films 236

10.3.4 Diffusion-Induced Dislocation Plasticity in Polycrystalline
Cu Films 239
10.4 Size-Dependent Dislocation Plasticity in Metals 239
10.4.1 Plasticity in Geometrically Confined Single Crystal
fcc Metals 241
10.4.2 Size-Dependent Transitions in Dislocation Plasticity 243
10.4.3 Plasticity by Motion of Grain Boundaries 244
10.4.4 Influence of Grain Size Heterogeneities 245
10.5 Conclusions and Future Directions 247
References 248
11 In-Situ Nanoindentation in the Transmission Electron Microscope 255

Andrew M. Minor
11.1.1 The Evolution of In-Situ Mechanical Probing in a TEM 255
11.1.2 Introduction to Nanoindentation 256
11.2 Experimental Methodology 260
11.3 Example Studies 263
11.3.1 In-Situ TEM Nanoindentation of Silicon 263
11.3.2 In-Situ TEM Nanoindentation of Al Thin Films 269
11.4 Conclusions 272
References 274
Part IV Physical Properties 279
12 Current-Induced Transport: Electromigration 281

Ralph Spolenak
12.1 Principles 281
12.2 Transmission Electron Microscopy 283
12.2.1 Imaging 283
12.2.2 Diffraction 288
12.2.3 Convergent Beam Electron Diffraction (CBED):
Measurements of Elastic Strain 288
12.3 Secondary Electron Microscopy 289
12.3.1 Imaging 289
12.3.2 Elemental Analysis 291
12.3.3 Electron Backscatter Diffraction (EBSD) 292
12.4 X-Radiography Studies 292
12.4.1 Microscopy and Tomography 292
12.4.2 Spectroscopy 293
12.4.3 Topography 294
12.4.4 Microdiffraction 294
12.5 Specialized Techniques 295
12.5.1 Focused Ion Beams 295
Contents XI
12.5.2 Reflective High-Energy Electron Diffraction (RHEED) 296

12.5.3 Scanning Probe Methods 296
12.6 Comparison of In-Situ Methods 297
References 299
13 Cathodoluminescence in Scanning and Transmission

Electron Microscopies 303
Yutaka Ohno and Seiji Takeda
13.2 Principles of Cathodoluminsecence 304
13.2.1 The Generation and Recombination of Electron-Hole Pairs 304
13.2.2 Characteristic of CL Spectroscopy 305
13.2.3 CL Imaging and Contrast Analysis 306
13.2.4 Spatial Resolution of CL Imaging and Spectroscopy 306
13.2.5 CL Detection Systems 307
13.3 Applications of CL in Scanning and Transmission Electron
Microscopies 307
13.3.1 Assessments of Group III–V Compounds 308
13.3.1.1 Nitrides 308
13.3.1.2 III–V Compounds Except Nitrides 309
13.3.2 Group II–VI Compounds and Related Materials 310
13.3.2.1 Oxides 310
13.3.2.2 Group II–VI Compounds, Except Oxides 312
13.3.3 Group IV and Related Materials 313
13.4 Concluding Remarks 313
References 313
14 In-Situ TEM with Electrical Bias on Ferroelectric Oxides 321

Xiaoli Tan
14.2 Experimental Details 323
14.3 Domain Polarization Switching 324
14.4 Grain Boundary Cavitation 326
14.5 Domain Wall Fracture 331
14.6 Antiferroelectric-to-Ferroelectric Phase Transition 335
14.7 Relaxor-to-Ferroelectric Phase Transition 341
References 345
15 Lorentz Microscopy 347

Josef Zweck
15.2 The In-Situ Creation of Magnetic Fields 350
15.2.1 Combining the Objective Lens Field with Specimen Tilt 351
15.2.2 Magnetizing Stages Using Coils and Pole-Pieces 352
15.2.3 Magnetizing Stages Without Coils 356
XII Contents
15.2.3.1 Oersted Fields 356

15.2.3.2 Spin Torque Applications 358
15.2.3.3 Self-Driven Devices 361
15.3 Examples 362
15.3.1 Demagnetization and Magnetization of Ring Structures 362
15.3.2 Determination of Wall Velocities 364
15.3.3 Determination of Stray Fields 365
15.4 Problems 366
15.5 Conclusions 367
References 367
Index 371
XIII
List of Contributors
Florian Banhart and

Université de Strasbourg Montanuniversität Leoben
Institut de Physique et Chimie des Department Materials Physics
Matériaux, UMR 7504 Franz-Josef-Str. 18
23 rue du Loess 8700 Leoben
67034 Strasbourg Austria
France
Wayne D. Kaplan
Nigel D. Browning Technion - Israel Institute of Technology
Lawrence Livermore National Department of Materials Engineering
Laboratory Haifa 32000
Physical and Life Sciences Directorate Israel
7000 East Avenue
Livermore Daniel Kiener
California 94550 Montanuniversität Leoben
USA Department Materials Physics
Franz-Josef-Str. 18
Geoffrey H. Campbell 8700 Leoben
Lawrence Livermore National Austria
Laboratory
Physical and Life Sciences Directorate Judy S. Kim
7000 East Avenue Lawrence Livermore National
Livermore Laboratory
California 94550 Physical and Life Sciences Directorate
USA 7000 East Avenue
Livermore
Gerhard Dehm California 94550
Austrian Academy of Sciences USA
Erich Schmid Institute of Materials
Science
Jahnstr. 12
8700 Leoben
Austria
XIV List of Contributors
and Marc Legros

University of California CEMES-CNRS
Department of Chemical Engineering 29 Rue Jeanne Marvig
and Materials Science 31055 Toulouse
One Shields Avenue France
Davis
California 95616 Andrew M. Minor
USA University of California, Berkeley and
National Center for Electron Microscopy
Wayne E. King Department of Materials Science and
Lawrence Livermore National Engineering, Lawrence Berkeley
Laboratory National Laboratory
Physical and Life Sciences Directorate One Cyclotron Road, MS 72
7000 East Avenue Berkeley
Livermore CA 94720
California 94550 USA
USA
Christian Motz
Christoph Koch Österreichische Akademie der
Max-Planck-Institut für Wissenschaften
Metallforschung Erich Schmid Institut für
Heisenbergstr. 3 Materialwissenschaft
70569 Stuttgart Jahnstr. 12
Germany 8700 Leoben
Austria
Thomas LaGrange
Lawrence Livermore National Yutaka Ohno
Laboratory Tohoku University
Physical and Life Sciences Directorate Institute for Materials Research
7000 East Avenue Katahira 2-1-1
Livermore Aoba-ku
California 94550 Sendai 980-8577
USA Japan
Alexander V. Latyshev Bryan W. Reed

Siberian Branch of Russian Academy of Lawrence Livermore National
Sciences Laboratory
Institute of Semiconductor Physics Physical and Life Sciences Directorate
Prospect Lavrent’eva 13 7000 East Avenue
630090 Novosibirsk Livermore
Russia California 94550
USA
List of Contributors XV
Frances M. Ross Seiji Takeda

IBM T. J. Watson Research Center Osaka University
1101 Kitchawan Road The Institute of Scientific and Industrial
Yorktown Heights Research
NY 10598 Mihogaoka 8-1
USA Ibaraki
Osaka 567-0047
Christina Scheu Japan
1Ludwig-Maximilians-Universität
München Xiaoli Tan
Department Chemie & Center for Iowa State University
NanoScience (CeNS) Department of Materials Science and
Butenandstr. 5-13, Gerhard-Ertl- Engineering
Gebäude (Haus E) 2220 Hoover Hall
81377 München Ames
Germany IA 50011
USA
Renu Sharma
National Institute of Science and Judith C. Yang
Technology University of Pittsburgh
Center for Nanoscale Science and Department of Chemical and Petroleum
Technology Engineering
100 Bureau Drive 1249 Benedum Hall
Gaithersburg Pittsburgh
MD 20899-6201 PA 15261
USA USA
Ralph Spolenak Guangwen Zhou

ETH Zurich P. O. Box 6000
Laboratory of Nanometallurgy, 85 Murray Hill Road
Department of Material Binghampton
Wolfgang-Pauli-Str. 10 NY 13902
8093 Zurich USA
Switzerland
Josef Zweck
University of Regensburg
Physics Faculty
Physics Building Office Phy 7.3.05
93040 Regensburg
Germany
XVII
Preface
Today, transmission electron microscopy (TEM) represents one of the most impor-
tant 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 pro-
cesses. 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).
XVIII Preface
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 Micro-
scopy are also included in Part One, to highlight the science which emanates from
these fields.
Gerhard Dehm, Leoben, Austria

James M. Howe, Charlottesville, USA
Josef Zweck, Regensburg, Germany
January 2012
j1
Part I
Basics and Methods
In-situ Electron Microscopy: Applications in Physics, Chemistry and Materials Science, First Edition.
Edited by Gerhard Dehm, James M. Howe, and Josef Zweck.
Ó 2012 Wiley-VCH Verlag GmbH & Co. KGaA. Published 2012 by Wiley-VCH Verlag GmbH & Co. KGaA.
j3
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.
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.
In-situ Electron Microscopy: Applications in Physics, Chemistry and Materials Science, First Edition.
Edited by Gerhard Dehm, James M. Howe, and Josef Zweck.
Ó 2012 Wiley-VCH Verlag GmbH & Co. KGaA. Published 2012 by Wiley-VCH Verlag GmbH & Co. KGaA.
4 j 1 Introduction to Scanning Electron Microscopy
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]; Ó 2008, John Wiley & Sons.
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).
1.1 Components of the Scanning Electron Microscope j5
. 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.
Before discussing these major components, a few words should be mentioned
regarding the vacuum system. Within the microscope, different levels of vacuum are
required for three main reasons. First, the electron source must be protected against
Figure 1.2 Schematic drawing of the major probe, and to control the beam current density.
components of a scanning electron The demagnified beam is than scanned across
microscope. The electron lenses and apertures the sample. Various detectors are used to
are used to demagnify the electron beam that is register the signals arising from various
emitted from the electron source into a small electron–matter interactions.
oxidation, which would limit the lifetime of the gun and may cause instabilities in the
intensity of the emitted electrons. Second, a high level of vacuum is required to
prevent the scattering of electrons as they traverse the column from the gun to the
specimen. Third, it is important to reduce the partial pressure of water and carbon in
the vicinity of the sample, as any interaction of the incident electron beam with such
molecules on the surface of the sample may lead to the formation of what is
commonly termed a carbonaceous (or contamination) layer, which can obscure
the sample itself. The prevention of carbonaceous layer formation depends both on
the partial pressure of water and carbon in the vacuum near the sample, and the
amount of carbon and water molecules that are adsorbed onto the surface of the
sample prior to its introduction into the microscope. Thus, while a minimum level of
vacuum is always required to prevent the scattering of electrons by molecules (the
concentration of which in the vacuum is determined from a measure of partial
pressure), it is the partial pressure of oxygen in the region of the electron gun, and the
partial pressure of carbon and water in the region of the specimen, that are in fact
critical to operation of the microscope. Unfortunately, most scanning electron
microscopes do not provide such measures of partial pressure, but rather maintain
different levels of vacuum in the different regions of the instrument. Normally, the
highest vacuum (i.e., the lowest pressure) is in the vicinity of the electron gun and,
depending on the type of electron source, an ultra-high-vacuum (UHV) level
(pressure <108 Pa) may be attained. The nominal pressure in the vicinity of the
specimen is normally in the range of 103 Pa. Some scanning electron microscopes
that have been designed for the characterization of low-vapor pressure liquids,
moist biological specimens or nonconducting materials, have differential
apertures between the regions of the microscope. This allows a base vacuum as
high as approximately 0.3 Pa close to the sample. These instruments, which
are often referred to as environmental scanning electron microscopes, offer
unique possibilities, but their detailed description is beyond the scope of the present
chapter.
1.1.1
Electron Guns
The role of the electron gun is to produce a high-intensity source of electrons which
can be focused into a fine electron beam. In principle, free electrons can be generated
by thermal emission or field emission from a metal surface (Figure 1.3). In thermal
emission, the energy necessary to overcome the work function is supplied by heating
the tip. In order to reduce the work function an electric field is applied (Schottky
effect). If the electric field is of the order of 10 V nm1, the height and width of the
potential barrier is strongly reduced, such that the electrons may leave the metal via
field emission.
Although several different electron sources have been developed, their basic
design is rather similar (see Figure 1.4). In a thermionic source, the electrons are
extracted from a heated filament at a low bias voltage that is applied between the
source and a cylindrical cap (the Wehnelt cylinder). This beam of thermionic
Figure 1.3 Schematic drawing of the The work function can be lowered by applying an
electrostatic potential barrier at a metal surface. electric field (Schottky effect). If the field is very
In order to remove an electron from the metal high, the electrons can tunnel through the
surface, the work function must be overcome. potential barrier. Redrawn from Ref. [1].
electrons is brought to a focus by the electrostatic field and then accelerated by an

anode beneath the Wehnelt cylinder.
The beam that enters the microscope column is characterized by the effective
source size dgun, the divergence angle of the beam a0, the energy of the electrons E0,
and the energy spread of the electron beam DE.
An important quantity here is the axial gun brightness (b), which is defined as the
current DI passing through an area DS into a solid angle DV ¼ pa2, where a is the
angular spread of the electrons. With j ¼ DI/DS being the current density in A cm2,
the following is obtained:
DI j
b¼ ¼ ¼ const: ð1:1Þ
DSDV pa2
The brightness is a conserved quantity, which means that its value is the same for
all points along the optical axis, independent of which apertures are inserted, or how
many lenses are present.
Currently, three different types of electron sources are in common use (Figure 1.4);
the characteristics of these are summarized in Table 1.1. A heated tungsten filament
is capable of generating a brightness of the order of 104 A cm2 sr1, from an effective
source size, defined by the first cross-over of the electron beam, approximately 15 mm
across. The thermionic emission temperatures are high, which explains the selection
of tungsten as the filament material. A lanthanum hexaboride LaB6 crystal can
generate a brightness of about 105 A cm2 sr1, but this requires a significantly
higher vacuum level in the vicinity of the source, and is now infrequently used in SEM
instruments. The limited effective source size of thermionic electron guns, which
must be demagnified by the electromagnetic lens system before impinging on the
sample, leads to microscopes equipped with thermionic sources being defined as
conventional scanning electron microscopes.
Figure 1.4 Schematic drawings of (a) a Wehnelt cylinder). (e) In FEGs, the electrons are
tungsten filament and (b) a LaB6 tip for extracted by a high electric field applied to the
thermionic electron sources. (c) For a field- sharp tip by a counterelectrode aperture, and
emission gun (FEG) source, a sharp tungsten then focused by an anode to image the
tip is used. (d) In thermionic sources the source. Reproduced with permission from
filament or tip is heated to eject electrons, which Ref. [4]; Ó 2008, John Wiley & Sons.
are then focused with an electrostatic lens (the
The effective source size can be significantly reduced (leading to the term high-
resolution SEM) by using a cold field emission gun (FEG), in which the electrons
tunnel out of a sharp tip under the influence of a high electric field (Figures 1.3
and 1.4). Cold FEG sources can generate a brightness of the order of 107 A cm2 sr1,
and the sharp tip of the tungsten needle that emits the electrons is of the order of
0.2 mm in diameter; hence, the effective source size is less than 5 nm. More often, a
hot source replaces the cold source, in which case a sharp tungsten needle is
heated to enhance the emission (this is termed a thermal field emitter, or TFE). The
heating of the tip leads to a self-cleaning process; this has proved to be another benefit
of TFEs in that they can be operated at a lower vacuum level (higher pressures). In the
Table 1.1 A comparison of the properties of different electron sources.
Source type Thermionic Thermionic Schottky Cold FEG
Cathode material W LaB6 W(100) þ ZrO W(310)

Work function [eV] 4.5 2.7 2.7 4.5
Tip radius [mm] 50–100 10–20 0.5–1 <0.1
Operating temperature [K] 2800 1900 1800 300
Emission current density [A cm2] 1–3 20–50 500–5000 104–106
Total emission current [mA] 200 80 200 5
Maximum probe current [nA] 1000 1000 >20 0.2
Normalized brightness [A cm2 sr1] 104 105 107 2 107
Energy spread at gun exit [eV] 1.5–2.5 1.3–2.5 0.4–0.7 0.3–0.7
so-called Schottky emitters, the electrostatic field is mainly used to reduce the work
function, such that electrons leave the tip via thermal emission (see Figure 1.3). A
zirconium-coated tip is often used to reduce the work function even further.
Although Schottky emitters have a slightly larger effective source size than cold
field emission sources, they are more stable and require less stringent vacuum
requirements than cold FEG sources. Equally important, the probe current at
the specimen is significantly larger than for cold FEG sources; this is important
for other analytical techniques used with SEM, such as energy dispersive X-ray
spectroscopy (EDS).
1.1.2
Electromagnetic Lenses
Within the scanning electron microscope, the role of the general lens system is to
demagnify an image of the initial crossover of the electron probe to the final size of
the electron probe on the sample surface (1–50 nm), and to raster the probe across
the surface of the specimen. As a rule, this system provides demagnifications in the
range of 1000- to 10 000-fold. Since one is dealing with electrons rather than photons
the lenses may be either electrostatic or electromagnetic. The simplest example of
these is the electrostatic lens that is used in the electron gun.
Electromagnetic lenses are more commonly encountered, and consist of a large
number of turns of a copper wire wound around an iron core (the pole-piece). A small
gap located at the center of the core separates the upper and lower pole-pieces. The
magnetic flux of the lens is concentrated within a small volume by the pole-pieces,
and the stray field at the gap forms the magnetic field. The magnetic field distribution
is inhomogeneous in order to focus electrons traveling parallel to the optical axis onto
a point on the optical axis; otherwise, they would be unaffected. Thereby, the radial
component of the field will force these electrons to change their direction in such a
way that they possess a velocity component normal to the optical axis; the longitudinal
component of the field would then force them towards the optical axis. Accordingly,
the electrons move within the lens along screw trajectories about the optical axis due
to the Lorentz force associated with the longitudinal and radial magnetic field
components.
Generally, in order to determine the image position and magnification (demagni-
fication) for the given position of the object, it is possible to use the lens formula:
1 1 1
¼ þ ð1:2Þ
F U V
where F is the focal length of the lens, U is the distance between the object and the
lens, and V is the distance between the image and the lens. The magnification
(demagnification) of the image – that is, the ratio of the linear image size h to the
corresponding linear size of the object H – is equal to (see Figure 1.5):
h V
M¼ ¼ : ð1:3Þ
H U
If U F, then for the total demagnification of a three-lens system a spot is obtained
with a geometric diameter of
F1 F2 F3
d0 ¼ dgun ¼ Mdgun ð1:4Þ
U1 U2 U3
where dgun is the initial crossover diameter. To obtain d0 10 nm for a thermionic
cathode, which possesses an initial crossover dgun of 20–50 mm, the total demagni-
fication must be 1/5000. A Schottky or field-emission gun can result in dgun
10 nm, such that only one probe-forming (objective) lens is necessary to demagnify
the electron probe to d0 1 nm. The distance between the objective lens and the
sample surface is termed the working distance of the microscope. From the above
discussion, it follows that a short working distance will lead to a stronger demagni-
fication and thus to a smaller electron probe size.
Figure 1.5 Schematic drawing of the relationship between focal length and magnification for a
ideal thin lens. Reproduced with permission from Ref. [4]; Ó 2008, John Wiley & Sons.
As with any lens system, the final size (and shape) of the electron probe will
also depend on aberrations intrinsic to the electromagnetic lenses used in the
scanning electron microscope. In a simplistic approach, the three main lens
aberrations are spherical and chromatic aberrations (Figure 1.6) and astigmatism
(Figure 1.7):
. Spherical aberration results in electrons traversing different radial distances in the
lens (r1 and r2 in Figure 1.6a), to be focused at different focal lengths; this will
result in a blurring of the image (and a finite resolution).
. Due to chromatic aberrations, electrons having a difference in energy (wavelength)
are focused to different focal lengths along the optical column (Figure 1.6b). In
contrast to optical microscopy, electrons with shorter wavelengths (i.e., higher
energy) will reach a focal point at larger focal lengths.
. Finally, astigmatism results in different focal lengths for electrons entering the
lens at different tangential angles about the optical axis (Figure 1.7).
Figure 1.6 (a, b) Schematic drawings of the influence of (a) spherical and (b) chromatic
aberrations on the focused electron probe. In this schematic drawing the angles of deflection are
exaggerated. Reproduced with permission from Ref. [4]; Ó 2008, John Wiley & Sons.
Figure 1.7 Schematic drawing of the influence of astigmatism on size of a focused electron probe.
Reproduced with permission from Ref. [4]; Ó 2008, John Wiley & Sons.
The electron current density jp and the probe aperture-dependent semi-conver-

gence angle ap are linked via the gun brightness, b:
jp ¼ pba2p : ð1:5Þ
If it is assumed, for simplicity, that the current density is uniform over a circle of
diameter d0, then the total probe current will be given by:
p 2
ip ¼ d jp : ð1:6Þ
4 0
Then:
sffiffiffiffiffiffi
4ip 1 1
d0 ¼ ¼ C0 : ð1:7Þ
b pap ap
It is important to note that the parameters iP, d0 and aP cannot be varied

independently since, as mentioned above, the brightness remains constant. For a
fixed vale of d0 and aP, a large value of b will be required to obtain a large probe
current, iP.
This geometric probe diameter d0 is broadened by the action of the lens aberra-
tions. Assuming a Gaussian distribution for both the geometric electron probe profile
and all the aberrations, one obtains for the probe size:
dp2 ¼ d02 þ dd2 þ ds2 þ dc2 ð1:8Þ
h i
2 2 DE 2 2
dp2 ¼ C0 þ ð0:6lÞ ap þ 0:25Cs ap þ Cc
2 2 6
ap ð1:9Þ
E
where C0 contains the probe current and the gun brightness, dd is the diffraction limit
due to the apertures, and CS and CC are the spherical and chromatic aberration
coefficients, respectively. When using a scanning electron microscope with a
thermionic cathode, the constant C0 is much larger than l, which means that the
diffraction error can be neglected. The dominant terms are those containing C0 and
CS because, for energies in the 10 to 20 kV range, the term that contains CC becomes
small due to the presence of DE/E. When operating with E < 5 keV, the chromatic
error term dominates and C0 is increased owing to the decrease in b (which is
proportional to E).
1.1.3
Deflection System
As mentioned above, the image is formed by scanning a focused electron beam along
a raster where, at each point, a signal produced by the interaction between the
incident electron beam and the sample is detected, amplified, and displayed.
Scanning over a raster is accomplished by two pairs of scanning coils which deflect
the electron beam along a line; the coils then move the beam to the beginning of the
next line where it is again deflected. By repeating this process the entire rastered area
can be scanned. Simultaneously, a spot is scanned over the viewing screen, and
displays the detected signal at each point. The viewing screen is either a cathode ray
tube (these are rarely used in modern systems) or a liquid crystal display (LCD)
computer monitor-based system.
Due to the image formation process, the magnification M of a scanning electron
microscope is given by the ratio of the length of the raster on the viewing screen
LScreen and the length of the raster on the sample surface LSample:

M ¼ LScreen L : ð1:10Þ
Sample
1.1.4
Electron Detectors
As will be described in detail later, electron–matter interaction can lead to the

emission of secondary electrons (SEs) and backscattered electrons (BSEs). These
are distinguished by their energy, with electrons having energies <50 eV being
considered as SEs, while those with energies close to that of the incident electron
beam are labeled BSEs. Both can be used in the imaging process in the scanning
electron microscope, while several different types of detectors are required to
differentiate between them.
1.1.4.1 Everhart–Thornley Detector

One of the most frequently used detectors, the Everhart–Thornley (ET), can be used to
detect both SEs and BSEs. The basic components of an ET detector (see Figure 1.8)
include a scintillator which is surrounded by a metal collector grid, a light guide, and a
photomultiplier system. Any electrons that enter the detector are collected if their
energy is sufficient to create photons in the scintillator; the photons are then guided
via a light guide to a photomultiplier system where the photon causes electrons to be
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landed, stretched himself in the sun, and got without undue haste
into a rather summary costume. There was plenty of time before
breakfast to make a more ordered toilet, and his hair would be dry
and tied back with a ribbon by then. Perukes and short hair were
convenient, but, fashionable or no, he found the former hot. When he
was Lochiel’s age, perhaps, he would wear one.
Before long he was striding off towards the house, whistling a
French air as he went.
(2)
Between the red crag and the spot where he had rated his foster-
brother that morning Ardroy stood alone now with his betrothed. The
loch was almost more beautiful in the sunset light than when its
waters had closed over his head all those hours ago, and even with
Alison on his arm Ewen was conscious of this, for he adored Loch na
h-Iolaire with little less than passion. So they stood, close together,
looking at it, while here and there a fish rose and made his little
circle, widening until it died out in the glassy infinity, and near shore
a shelduck with her tiny bobbing brood swam hastily from one patch
of reeds to another.
Presently Ewen took off his plaid and spread it for Alison to sit
upon, and threw himself down too on the carpet of cranberries; and
now he looked, not at the loch, but at her, his own (or nearly his own)
at last. Alison’s hand, waited for so patiently . . . no, not always so
patiently . . . strayed among the tiny leaves, and Ewen caught the
little fingers, with his ring upon the least but one, and kissed them.
“And to think,” he said softly, “that by this time to-morrow we shall
be contracted in writing, and you not able to get away from me!”
Alison looked down at him. In her dark eyes swam all kinds of
sweetness, but mischief woke and danced now at the corners of her
small, fine, close-shut mouth, which could be so tender too.
“Oh, Ewen, does the contract make you more sure of me? You’d
not hold me to a bit of paper if I were to change my mind one fine
morning and say, ‘Ardroy, I’m sweir to tell it, but wed you I cannot’?”
“Would I not hold you to it! Try, and see!”
One of Alison’s dimples appeared. “Indeed, I’m minded to try it,
just for that, to see what you would do. What would you do, Eoghain
mhóir?”
“Carry you off,” replied Ewen promptly.
“And marry me by force?”
“And marry you by force.”
“There speaks the blood of Hieland reivers! I’d think shame to
say such a thing!”
“And are you not Hieland yourself, Miss Grant?” enquired her
lover. “And was there never cattle-lifting done in Glenmoriston?”
“Cattle!” exclaimed Alison, the other dimple in evidence. “That I
should be likened, by him that’s contracted to be married to me, to a
steer or a cow!”
“I likened you to no such thing! You are like a hind, a hind that
one sees just a glimpse of before it is gone, drinking at the lake on a
misty morning. Oh, my heart’s darling,” he went on, dropping into
Gaelic, “do not make jests upon our marriage! If I thought that you
were in earnest—Alison, say that you are not in earnest!”
Alison Grant looked into the clear blue eyes, which had really
grown troubled, and was instantly remorseful. “Oh, my dear, what a
wretch am I to torment you thus! No, no, I was teasing; Loch na h-
Iolaire shall run dry before I break my troth to you. I’ll never force you
to carry me off; ’tis like I’ll be at the kirk before you.” She let him draw
her head without words upon his shoulder, and they sat there silent,
looking at happiness: both the happiness which they knew now, and
the greater, the long happiness which was coming to them—as
stable and secure in their eyes as the changeless mountains round
them.
Yet Alison knew her lover’s mind, or at least a part of it, so well
that she presently said, “And yet I am not jesting, Ewen, when I say
that I think you would be hard put to it to choose between me and
Loch na h-Iolaire—Loch na h-Iolaire and the house of Ardroy.”
His arm tightened round her. “Alison, how can you——”
“But you’ll never have to choose, m’eudail. I love this place most
dearly already. I have never had a home like it to love, living as we
have for so long, now in France, now in Holland. But your heart is as
strongly rooted here as . . . the red crag yonder.”
Ewen gave a little sigh. “You see a long way into my heart, you
that are the core of it. Indeed, when I am dying I think this is the last
place I shall have sight of in my mind. I hope I may be seeing it with
my eyes also.”
Alison did not shudder or change the subject, or implore him not
to speak of such things, for she was Highland too, with her race’s
half-mystical preoccupation with the dead. But she thought, “I hope
I’ll die the same day, the same hour. . . .”
The shadows on the loch crept a little farther. Behind them Ben
Tee changed colour for the hundredth time; his pointed peak seemed
to soar. It grew cooler too, and Ewen wrapped the ends of the plaid
about his lady.
“On Wednesday we will spend the day at Loch Arkaig,” he
announced. “We will take ponies, and you and Mr. Grant shall ride.”
“And Miss Cameron?”
“Aunt Marget detests such jaunts. Meals for the parlour, and the
parlour for meals, that is her creed.—Alison, are you not cold?”
“In this?” She fingered the plaid where it hung over her shoulders,
and added after a moment: “How strange it will be, to wear another
tartan than one’s own!”
“You shall always wear the Grant if it pleases you better.”
“No, it does not please me better,” answered Alison softly. “I feel .
. . very warm in the Cameron.”
He kissed her for that, smiling, and, raising his head from his
kiss, became aware of a dark object beating towards them out of the
sunset sky. It was the solitary heron of the island, winging his strong
way home with a deceptive slowness. The sight reminded Ewen of
his morning’s encounter with Lachlan, and he was about to tell
Alison of it when Fate’s messenger, who for the last five minutes had
been hurrying round the loch, came past the red crag of Ardroy, and
Ewen’s quick ear caught the snap of a breaking stick under the
deerskin brogues. He looked quickly round. A bearded Highlander
was trotting towards them under the birches and pines.
“It is Neil—what can he want? Forgive me!” He rose to his feet,
and Neil MacMartin, who was Lachlan’s elder brother and Ewen’s
piper, broke into a run.
“Mac Dhomhnuill Duibh has just sent this by a man on
horseback,” he said somewhat breathlessly, pulling a letter from his
sporran.
Ewen broke the seal. “Perhaps it is to say that Lochiel cannot
come to-morrow,” he observed to his betrothed. But as he read his
face showed stupefaction. “Great God!”
Alison sprang to her feet. “Ewen! Not bad news?”
“Bad? No, no!” He waved Neil out of hearing and turned to her
with sparkling eyes. “The Prince has landed in Scotland!”
She was at first as amazed as he. “The Prince! Landed! When . .
. where?”
Ewen consulted his letter again. “He landed at Borradale in
Arisaig on the twenty-fifth. Lochiel desires me to go to Achnacarry at
once.”
“He has come—at last!” said Alison to herself, almost with awe.
“And you will go with Lochiel to kiss his hand, to—Oh, Ewen, how I
envy you!”
The light which had come into her lover’s eyes died out a little. “I
do not know that Lochiel is going to Arisaig, darling.” He glanced at
the letter again. “He is troubled, I can see; there are no troops with
the Prince, none of the hoped-for French help.”
“But what of that?” cried the girl. “It is not to be thought of that
Lochiel’s sword, of all others, should stay in the scabbard!”
“Lochiel will do what is right and honourable; it is impossible for
him ever to act otherwise,” answered Ewen, who was devoted to his
Chief. “And he wants speech with me; I must set out at once. Yes,
Clan Cameron will rise, not a doubt of it!”
And, youth and the natural ardour of a fighting race reasserting
themselves, he snatched up his bonnet and tossed it into the air.
“Ah, now I know why Lachlan and I thought we saw blood on his dirk
this morning!” Then he caught Alison to him. “My dearest on earth,
give me your kiss!”
It was the title of one of the ancient pibrochs that he was quoting,
and the Highland girl put her arms round his neck and gave him what
he asked.
Loch na h-Iolaire, bereft of the echoing voices, sank into a silence

that was not broken until the heron rose again from the island and
began to fly slowly towards the sunset. Then the stillness was rent
by a sharp report; the great bird turned over twice, its wings beating
wildly, and fell all huddled into the lake. A little boat shot out from the
side of the creag ruadh, and in a moment or two Lachlan MacMartin,
leaving his oars, was bending over the side with the end of a cord in
his hand. There was a splash as he threw overboard the large stone
to which the cord was fastened; and having thus removed the
evidence of his blind effort to outwit destiny, he pulled quickly back to
the shelter of the crag of Ardroy.
Soon the same unbroken calm, the same soft lap and ripple, the
same gently fading brightness were once more round Loch na h-
Iolaire; yet for all those who to-day had looked on its waters the
current of life was changed for ever.
I
THROUGH ENGLISH EYES
“One of them asked . . . how he liked the Highlands. The question seemed to
irritate him, for he answered, ‘How, sir, can you ask me what obliges me to speak
unfavourably of a country where I have been hospitably entertained? Who can like
the Highlands—I like the inhabitants very well.’”
—Boswell. Journal of a Tour to the Hebrides.
CHAPTER I
In all Lochaber—perhaps in all the Western Highlands—there was

no more bored or disgusted man this sixteenth of August than
Captain Keith Windham of the Royal Scots, as he rode down the
Great Glen with a newly-raised company of recruits from Perth; and
no more nervous or unhappy men than the recruits themselves. For
the first time in their lives the latter found themselves far north of ‘the
Highland line’, beyond which, to Lowland as well as to English
minds, there stretched a horrid region peopled by wild hill tribes,
where the King’s writ did not run, and where, until General Wade’s
recent road-making activities, horsed vehicles could not run either.
Yesterday only had they reached Fort Augustus, two companies of
them, and this afternoon, tired and apprehensive, were about half-
way through their thirty-mile march to Fort William. As for the English
officer, he was cursing with all his soul the young Adventurer whose
absurd landing on the coast of Moidart last month had caused all this
pother.
Had it not been for that event, Captain Windham might have
been allowed to return to Flanders, now that his wound of Fontenoy
was healed, to engage in real warfare against civilised troops,
instead of marching through barbarous scenery to be shut up in a
fort. He could not expect any regular fighting, since the savage
hordes of these parts would probably never face a volley.
Nevertheless, had he been in command of the column, he would
have judged it more prudent to have a picket out ahead; but he had
already had a slight difference of opinion with Captain Scott, of the
other company, who was senior to him, and, being himself of a
temper very intolerant of a snub, he did not choose to risk one.
Captain Windham had no great love for Scotsmen, though, ironically
enough, he bore a Scottish Christian name and served in a Scottish
regiment. As it happened, he was no more responsible for the one
fact than for the other.
It was hot in the Great Glen, though a languid wind walked
occasionally up Loch Lochy, by whose waters they were now
marching. From time to time Captain Windham glanced across to its
other side, and thought that he had never seen anything more
forbidding. The mountain slopes, steep, green and wrinkled with
headlong torrents, followed each other like a procession of
elephants, and so much did they also resemble a wall rising from the
lake that there did not appear to be space for even a track between
them and the water. And, though it was difficult to be sure, he
suspected the slopes beneath which they were marching to be very
nearly as objectionable. As a route in a potentially hostile country, a
defile, astonishingly straight, with a ten-mile lake in the middle of it,
did not appeal to him.
However, the mountains on the left did seem to be opening out at
last, and General Wade’s new military road, upon which they were
marching, was in consequence about to leave the lake and proceed
over more open moorland country, which pleased Captain Windham
better, even though the wide panorama into which they presently
emerged was also disfigured by high mountains, in particular by that
in front of them, which he had been told was the loftiest in Great
Britain. And about twelve miles off, under those bastions, lay Fort
William, their destination.
But where was the river which, as he knew, they had first to
cross? In this wide, rough landscape Captain Windham could not
see a sign of it. Then, farther down the slope and about a mile ahead
of them, he discerned a long, thick, winding belt of trees, and
remembered to have heard an officer of Guise’s regiment at Fort
Augustus say last night that the Spean, a very rapid stream, had
carved so deep a channel for itself as almost to flow in a ravine, and
that Wade must have had some ado to find a spot where he could
carry his road over it. He had done so, it appeared, on a narrow
stone structure whose elevation above the river-bed had earned it
the name of High Bridge. Indeed the Englishman now saw that the
road which they were following was making for this deeply sunken
river at an angle which suggested that General Wade had had little
choice in the position of his bridge.
Ahead of Captain Windham on his mettlesome horse the scarlet
ranks tramped down the gently sloping road through the heather;
ahead of them again, at the rear of the foremost company, Captain
Scott sat his white charger. The English officer looked with an
unwilling curiosity at the great mountain mass over Fort William; it
actually had traces of snow upon it . . . in August! What a country!
Now in Flanders—— What the devil was that?
It was, unmistakably, the skirl of a bagpipe, and came from the
direction of the still invisible bridge. But if the bridge was not to be
seen, something else was—tartan-clad forms moving rapidly in and
out of those sheltering trees. Evidently a considerable body of
Highlanders was massing by the river.
The senior officer halted his men and came riding back. “Captain
Windham, I believe there is an ambush set for us down yonder.”
“It does not sound like an ambush, egad!” replied his colleague
rather tartly, as the heathenish skirling grew louder. “But I certainly
think there are Highlanders posted at the bridge to dispute our
crossing.”
“I’ll just send forward a couple of men to get some notion of their
numbers,” said Scott, and rode back again. Keith shrugged his
shoulders. “Somewhat of a tardy precaution!” he thought to himself.
A sergeant and a private were thereupon dispatched by Captain
Scott to reconnoitre. Their fate was swift and not encouraging, for
they had not gone far ere, before the eyes of all their comrades, they
were suddenly pounced upon by two Highlanders who, with a yell,
darted out from the trees and hurried them out of sight.
The intimidated recruits began to shuffle and murmur. Captain
Windham spoke vigorously to his subaltern, and then rode forward to
consult with his senior.
Captain Scott wheeled his horse to meet him. “This is unco
awkward,” he said, dropping his voice. “The Deil knows how many of
those fellows there are down yonder, but do you observe them,
Captain Windham, skipping about like coneys among the trees? The
bridge, I’ve heard, is uncommon narrow and high, with naught but
rocks and torrent below. I doubt we can get the men over.”
“We must!” retorted Keith. “There’s no other means of reaching
Fort William. The Royals to hesitate before a few beggarly cattle-
thieves!”
Alas, the Royals did more than hesitate. Even as he spoke there
were signs that the half-seen ‘cattle-thieves’ on the bridge were
preparing for a rush, for loud orders could be heard, and the piping
swelled hideously. And at that the scarlet-clad ranks on the slope
wavered, broke, turned, and began to flee up the rise as fast as their
legs could carry them.
It was in vain that their two captains endeavoured to rally them. A
man on a horse cannot do much to stem a flood of fugitives save
perhaps on a narrow road, and here the road had unlimited space on
either side of it. Helter-skelter the recruits ran, and, despite their
fatigue and their accoutrements, never ceased running for two miles,
till they stopped, exhausted, by Loch Lochy side once more.
By that time Captain Windham was without suitable words in
which to address them; his vocabulary was exhausted. Captain Scott
was in like case. There was another hasty consultation beneath the
unmoved stare of those steep green mountains. Scott was for
sending back to Fort Augustus for a detachment of Guise’s regiment
to help them force the bridge, and Captain Windham, not seeing
what else was to be done, concurred in this opinion. Meanwhile the
recruits should be marched at an easy pace in the direction of Fort
Augustus to their junction with these reinforcements, which were, of
course, to come up with all speed. There had been no sign of pursuit
by the successful holders of the bridge, and it might be hoped that in
a little the morale of the fugitives would be somewhat restored.
Captain Scott thereupon suggested that Captain Windham
should lend one of the lieutenants his horse, which was much faster
than his own white charger—no other officers but they being
mounted—but Keith objected with truth that a strange rider would
never manage his steed, and offered to make over his company to
his lieutenant and himself ride back to Fort Augustus if Captain Scott
thought good. And Captain Scott hastily agreed to what both officers
felt was a somewhat unusual course justified by circumstances.
To a man who, three months ago, had borne his part in the
wonderful retreat at Fontenoy, that epic of steadiness under fire, and
who had even been complimented by the Duke of Cumberland on
his conduct, the last half-hour had been a nightmare of shame, and
Keith Windham, glad to be able to extricate himself from it with the
confidence that he was not abandoning his men on the eve of a fight,
he set spurs to his horse with great relief.
He had gone about five miles along the loch—always with those
abominable mountains on either side of him—when a report echoed
soundingly among them, and a bullet struck the road a little ahead of
him. His pulling, nervous horse reared and plunged; and Keith
swore. He was not unobserved, then, and might very well be picked
off by some unseen marksman up there. Bullets, however, did not
discompose him like cowardice, and, cramming his hat farther down
upon his head, he merely urged the animal to greater speed.
In the next few miles, as occasional bullets winged their way at
varying distances past his person, Keith Windham began to think
that the hapless Royals behind him were perhaps being outflanked
by some enemy marching parallel to them on the hillside—and
marching much faster. The prospect of their being attacked seemed
by no means so remote. Still, in any case, it was now his business to
go on. But when he came in sight of the village beyond the end of
Loch Lochy through which they had passed that morning, he could
see armed Highlanders there in such numbers that it was unlikely he
would be allowed to ride through it. Gad! he thought, the rout at the
bridge had served, then, as a spark to all this tinder! For a moment—
since under a mask of indifference and cynicism he was a very hot-
tempered young man—the sting of that knowledge prompted him to
attempt cutting his way through regardless of consequences. Then
common sense triumphed. Better to avoid the enemy altogether by
crossing to the farther side of the smaller lake just ahead of him (he
did not know its name) on the wide flat isthmus which separated it
from Loch Lochy. If there were no ambushes on that side he would
yet reach Fort Augustus, since, as the Highlanders did not appear to
have horses, he was safe from mounted pursuit.
It became, however, a question whether he would get to the
isthmus in time to evade the enemy ahead, of whom half a dozen or
so, suspecting his intention, were running down the road towards
him, targe on arm and broadsword in hand, to cut him off. Keith
spurred his horse hard, fired at the foremost figure (which he
missed) and next moment dropped his own pistol with an
exclamation, his arm tingling to the shoulder. A bullet had struck the
barrel, ricocheting off Heaven knew where; in any case it was one of
the nearest escapes which he had ever experienced. For the
moment his right arm was useless; but here, at last, was the end of
the waters of this interminable Loch Lochy. He turned his almost
frantic horse and galloped like mad across the green, spongy
isthmus, pursued now only by ineffectual yells which he soon ceased
to hear.
The neck of land, though narrow, was longer than he
remembered; there were perhaps two miles of it before the next lake
came to separate him from his enemies. But, whether or no the fact
of his having a fast horse deterred them from pursuit, not one
Highlander attempted to cross after him. Possibly they were
reserving their forces undiminished for the attack on the main body
of the Royals, a thought which caused the Englishman to maintain
his headlong pace. Fortunately this side of the lake seemed
deserted; no man was going to stop him now!
And no man did. But he had not gone a mile by the lake side
when a large grey-and-white object flapped up suddenly from the
water’s edge almost under the nose of his excited horse; the beast
shied, swerved, crossed its legs and came heavily down, flinging its
rider against a fallen tree with a force which knocked him senseless.
Captain Windham was not stunned for very long, though to him it
was an unknown space of time that he lay sprawling in the dust by
the side of the pine-trunk. When he dizzily raised himself and looked
about him no human being was in sight, but there on the road, within
a few feet of him, with snorting nostrils and terrified eyes, lay his
unfortunate horse, trying desperately and repeatedly to get to its feet
again, despite a broken foreleg. For an instant Keith stared at the
poor sweating, plunging brute, then, passing a hand over his bruised
and bleeding forehead, he got to his own feet. There was only one
thing to be done; though the sound of a shot would very likely draw
undesirable attention upon himself, he could not leave the animal
there in agony. His remaining pistol was in his holster, and during the
process of extracting it he realized that he had twisted an ankle in his
fall. A moment or two later the sound of a shot went ringing over the
waters of Loch Oich, and the troubles of Captain Windham’s charger
were over.
But his were not; indeed he fancied that they had but just begun.
Dismounted, his brilliant scarlet-and-blue uniform rendering him in
the highest degree conspicuous, his head aching, and in one place
excoriated by contact with the tree-trunk, he saw that he could never
summon reinforcements in time now; it was doubtful whether he
would reach Fort Augustus at all. His ankle, as he soon discovered,
was swollen and painful; moreover he had somehow to get back to
Wade’s road when he reached the end of this lake. With his hand to
his head he glanced in disgust at the prostrate trunk with which it
had just made such painful acquaintance. Detestable country, where
even the wildfowl and the vegetation were in league with the
inhabitants!
Hearing a sound of water, he looked about till he found a tiny ice-
cold spring between the track and the lake, and, dipping his
handkerchief into this, bathed his forehead. Had he known of the
seven gory severed heads which had been washed in that innocent-
looking little source less than a hundred years before, perhaps he
would not have done so. Hardly had he reloaded his pistol, his next
care, when a distant noise, like many running feet, sent him hurriedly
to the shelter of the steep, tree-clad hillside on his left. Here, among
the scanty undergrowth, he crouched as best he could while, some
minutes later, a score of armed Highlanders poured past on the track
below him. So this side of the lake was gathering, too!
Captain Windham waited in his concealment until the way was
clear and silent again, and then descended, since it was impossible
for him to keep in cover if he meant to reach Fort Augustus—and
where else should he make for? Leaning on the branch of oak which
he had broken off to assist his steps, he began to trudge grimly
forward.
There soon came in sight, on its rock by the lake side, the keep
of Invergarry Castle. Captain Windham did not know that it belonged
to the chief of Glengarry, but he was sure that it was the hold of
some robber or other, and that he himself might not improbably see
the inside of it. It looked ruinous, but that was no safeguard—on the
contrary. And here were some dwellings, little, roughly thatched
buildings, but obviously inhabited. Yet all he saw of their occupants
were a few white-haired children who ran screaming away, and one
old woman at her door, who crossed herself devoutly at sight of him.
So, to add to all their other vices, the people of these parts were
Papists!
The next obstacle was a river, which he had to cross as best he
could on insecure and slippery stones, and the difficulties of doing
this with an injured ankle took his mind off remoter possibilities, so
that when he was safely over he was surprised to find the ominous
tower well behind him, and he went on somewhat cheered. The sun
was now getting lower, and though the other side of the glen was in
full warm light, this side felt almost cold. Another peculiarity of this
repulsively mountainous district. Gently swelling hills one could
admire, but masses of rock, scored with useless and inconvenient
torrents, had nothing to recommend them. He did not wonder at the
melancholy complaints he had heard last night from the officers
quartered at Fort Augustus.
And what would the garrison there say when they heard of this
afternoon’s disgrace? Captain Windham’s thoughts went angrily
back to it. What, too, had happened to those chicken-hearted
recruits by this time? He pulled out his watch; to his surprise it was
already after six o’clock. And he still had the watch in his hand when
his ear was caught by the sound of horse’s hoofs behind him. He
stopped to listen. The pace, a smart trot, did not seem hurried; the
rider might be some unconcerned traveller. But he might on the other
hand be an enemy. Keith Windham looked for cover, but here there
was none convenient as a while ago, and the best he could do was
to hobble on ahead to where a solitary oak-tree reared itself by the
side of the road, for he was minded to have something to set his
back against if necessary.
When he was nearly there he looked round, and saw the rider, a
big Highlander on a grey horse. He was not alone, for at his heels
came another, keeping up with the horse with long loping strides like
a wolf’s. To Keith one tartan was as yet like another, so, for all he
knew, these two might be of a friendly clan. He awaited them by the
oak-tree.
As the horseman came on Keith saw that he was young,
vigorous-looking and well armed. He wore trews, not a kilt like the
other. But as he came he rose in his stirrups and shouted something
in which Keith clearly caught the word ‘surrender’. So he was not
friendly. Very well then! Captain Windham raised the pistol which he
had ready, and fired—rather at the horse than the rider. The young
Highlander, with a dexterity which he could not but admire, pulled
aside the animal in the nick of time, and the shot missed. Keith’s
sword leapt out as, with a yell, the man on foot flung himself past the
horse towards him, dirk in hand. But the rider called out something in
Gaelic, which had an immediate effect, for the gillie, or whatever he
was, came to an abrupt stop, his eyes glowering and his lips drawn
back, as like a wolf about to spring as possible.
Meanwhile, to Keith’s surprise, the horseman sprang to earth,
flung the reins to his henchman, and came forward empty-handed—
a magnificent specimen of young manhood, as the soldier could not
help admitting.
“I advise you to surrender, sir,” he said courteously, lifting his
bonnet, in which were fastened two eagle’s feathers. “I am sorry to
take advantage of an injured man, but I have my Chief’s orders. You
are completely cut off, and moreover your men are all prisoners—
indeed Captain Scott is at this moment in Lochiel’s custody. If you
will give up your sword I shall be honoured to take you into mine.”
“The deuce you will!” exclaimed Keith, secretly astonished at the
polish of his manner—a man who wore a plaid! “And who are you,
pray?”
“Cameron of Ardroy,” answered the young man. “Lochiel’s
second cousin,” he added.
“I don’t care whose second cousin you are, Mr. Cameron of
Ardroy,” returned Captain Windham to this, “but if you think that you
are going to have my sword for the asking, you and your cut-throat
there, you are vastly mistaken!”
For provided—but it was a big proviso—that the two did not rush
upon him at once he thought that he could deal with each separately.
Splendidly built as this young Highlander was, lean too, and,
doubtless, muscular, he probably knew no more of swordplay than
was required to wield that heavy basket-hilted weapon of his, and
Captain Windham himself was a good swordsman. Yes, provided
Lochiel’s second cousin did not use the pistol that he wore (which so
far he had made no motion to do) and provided that the wolf-like
person remained holding the horse . . .
“Come on and take me,” he said provocatively, flourishing his
sword. “You are not afraid, surely, of a lame man!” And he pointed
with it to the rough staff at his feet.
Under his tan the large young Highlander seemed to flush
slightly. “I know that you are lame; and your forehead is cut. You had
a fall; I came upon your dead horse. That is why I do not wish to fight
you. Give up your sword, sir; it is no disgrace. We are two to one,
and you are disabled. Do not, I pray you, constrain me to disable you
further!”
Hang the fellow, why did he behave so out of his cateran’s rôle?
“You are considerate indeed!” retorted Captain Windham mockingly.
“Suppose you try first whether you can disable me further!—Now, Mr.
Cameron, as I don’t intend to be stopped on my road by mere words,
I must request you to stand out of my way!” And—rashly, no doubt,
since in so doing he no longer had one eye on that murderous-
looking gillie—he advanced sword in hand upon his reluctant
opponent. Frowning, and muttering something under his breath, the
young man with the eagle’s feathers at last drew his own weapon,
and the blades rang together.
Thirty seconds of it, and Keith Windham knew that he had
attacked a swordsman quite as good if not better than himself.
Breathing hard, he was being forced back to the trunk of the oak
again, and neither his aching head nor his damaged ankle was
wholly to blame for this. Who said that broadsword play was not
capable of finesse? This surprisingly scrupulous young barbarian
could have cut him down just then, but he drew back when he had
made the opening. The certitude of being spared irritated the soldier;
he lost his judgment and began to fight wildly, and so the end came,
for his sword was suddenly torn from his hand, sailed up into the
oak-tree above him, balanced a moment on a branch, and then fell a
couple of yards away. And his adversary had his foot upon it in a
second.
As for Keith Windham, he leant back against the oak-tree, his
head all at once going round like a mill-wheel, with the noise of a
sluice, too, in his ears. For a flash everything was blank; then he felt
that someone was supporting him by an arm, and a voice said in his
ear, “Drink this, sir, and accept my apologies. But indeed you forced
me to it.”
Keith drank, and, though it was only water, sight was restored to
him. It was his late opponent who had his arm under his, and who
was looking at him with a pair of very blue eyes.
“Yes, I forced you to it,” confessed Captain Windham, drawing a
long breath. “I surrender—I can do nothing else, Mr. . . . Cameron.”
“Then I will take you home with me, and your hurts can be
dressed,” said the Highlander, showing no trace of elation. “We shall
have to go back as far as the pass, but fortunately I have a horse.
Lachuin, thoir dhomh an t’each!”
The gillie, scowling, brought forward the grey. His captor loosed
Keith’s arm and held the stirrup. “Can you mount, sir?”
“But I am not going to ride your horse!” said Keith, astonished. “It
will not carry two of us—and what will you do yourself?”
“I? Oh, I will walk,” answered the victor carelessly. “I assure you
that I am more accustomed to it. But you would never reach Ardroy
on foot, lame as you are.” And as Keith hesitated, looking at this
disturbing exponent of Highland chivalry, the exponent added,
hesitating a little himself, “There is only one difficulty. If you are
mounted, I fear I must ask you for your parole of honour?”
“I give it you—and that willingly,” answered Keith, with a sudden
spurt of good feeling. “Here’s my hand on it, if you like, Mr.
Cameron!”
CHAPTER II
If to ride along a road in these mountain solitudes was distasteful, to

be following a mere track (and that a very steep one) in amongst
their very folds was worse. When first he had seen the path which
they were to ascend, and the V-shaped depression, sharp against
the sunset sky, up to which it led, Captain Windham had with
difficulty repressed an exclamation of alarm. However, he could not
really believe that Mr. Cameron of Ardroy was taking him up this
terrifying route in order to slay him, since he could already have
done this with so much less trouble on level ground. Therefore,
though he had raised his eyebrows, he had said nothing. After all, it
was the horse, and not he, who had to do the climbing. And now
they were half-way up.
The wolf-like attendant, carrying the surrendered sword, kept in
the rear, but Captain Windham was almost physically conscious of
his frown behind him. This unattractive person was, he felt, no willing
party to his capture; he would much have preferred that the redcoat
should have been left cold beneath the oak-tree. Meanwhile his
master, the young chieftain, or whatever he was, walked with a
mountaineer’s elastic step at the horse’s head, occasionally taking
hold of the bridle; rather silent, but uncommonly well-made and
good-looking, thought his captive again, glancing down at him.
Captain Windham’s own dark, rather harsh features were not
unpleasing, save when he frowned, which he was somewhat given
to doing, nor were they devoid of a certain distinction, and he had
really fine hazel eyes. But his mouth had already taken a cynical
twist unusual in a young man of thirty. If he had a passion left in life,
it was military ambition. Earlier he had known others, and they had
brought him nothing but unhappiness. As a boy he had had an
extraordinary devotion to his lovely mother—whom he had not been
alone in thinking fair. But she, too, was ambitious, and her second
marriage, to the Earl of Stowe, with its attendant advantages, was
more to her than the claims of her own son. Then the beautiful boy
she bore to Lord Stowe usurped the place which Keith had never
had in her heart. So, in respect of affection, sometimes even of
ordinary attention, he had passed through a neglected childhood and
a starved boyhood, and they had left an indelible mark on him—
more indelible, though he did not guess it, than the scars of another
woman’s betrayal of him four years ago.
The consequence was that at thirty, with a nature at bottom
passionate and impulsive, he had become as disillusioned, as little
prone to enthusiasms, as a man of twice his age. His creed was that
it was a mistake to desire anything very much—a fatal mistake to
desire a place in any person’s affections, or to admit anyone, man or
woman, to a place in your own. By the end of life, no doubt, every
human being had discovered this truth; he had done so early, and
could count himself the more fortunate.
At the same time it needed a rather different kind of detachment
to take his present situation philosophically; and yet, to his own
surprise, Keith Windham knew that he was doing so, even though he
had by now gleaned from his captor the later history of the day’s
disaster, and had learnt its mortifying completeness. Matters had
fallen out for the unfortunate recruits almost exactly as Captain
Windham had afterwards feared; for another body of Highlanders
was following them unseen on the hillside, and near the head of
Loch Lochy further progress had been barred by those who had
attempted to stay Keith himself. Though Captain Scott too had tried
to cross the isthmus, it was impossible, since more Highlanders were
hastening to the spot from that direction also. Too tired and panic-
stricken to use their muskets to good effect, the redcoats had, on the
contrary, received a fire which had killed five of them and wounded a
dozen, including Captain Scott himself. Some leader called
‘Keppoch’, Captain Windham heard, had then called on the Royals
to surrender, or they would be cut to pieces, and to save his men
Captain Scott had done so. Immediately on this had come up Ewen
Cameron’s chief, Lochiel (who had been asked for assistance), with
a number of his clan, including the present narrator, had taken
charge of the prisoners, and marched them off to his house of
Achnacarry. But as the Highlanders from the far side of Loch Oich
reported having seen a dead charger on the road, and one company
of the redcoats was plainly captainless, Lochiel had sent his young

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Time resolved electron diffraction for chemistry

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List of Contributors XIII

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2 Conventional and Advanced Electron Transmission Microscopy 39

3 Dynamic Transmission Electron Microscopy 71

3.6.4 Aberration Correction 93

4 Formation of Surface Patterns Observed with Reflection

Part II Growth and Interactions 123

5 Electron and Ion Irradiation 125

6 Observing Chemical Reactions Using Transmission Electron

6.3.1 Oxidation and Reduction (Redox) Reactions 150

7 In-Situ TEM Studies of Vapor- and Liquid-Phase Crystal Growth 171

8 In-Situ TEM Studies of Oxidation 191

8.2.1 Environmental Cells 192

Part III Mechanical Properties 209

9 Mechanical Testing with the Scanning Electron Microscope 211

10 In-Situ TEM Straining Experiments: Recent Progress in Stages

10.3.3 Dislocation Nucleation and Multiplication in Thin Films 236

11 In-Situ Nanoindentation in the Transmission Electron Microscope 255

Part IV Physical Properties 279

12 Current-Induced Transport: Electromigration 281

12.5.2 Reﬂective High-Energy Electron Diffraction (RHEED) 296

13 Cathodoluminescence in Scanning and Transmission

14 In-Situ TEM with Electrical Bias on Ferroelectric Oxides 321

15 Lorentz Microscopy 347

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The electron–optical system in a scanning electron microscope is actually designed

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electrons is brought to a focus by the electrostatic ﬁeld and then accelerated by an