Nanocharacterisation / edited by Angus I. Kirkland and John L. Hutchison.

Format:

Book

Contributor:

Kirkland, Angus.

Hutchison, John.

Royal Society of Chemistry (Great Britain)

Series:

RSC nanoscience & nanotechnology

Language:

English

Subjects (All):

Nanotechnology.

Electron microscopy.

Physical Description:

xiii, 304 pages : illustrations (some color) ; 24 cm.

Place of Publication:

Cambridge, UK : RSC Publishing, [2007]

Summary:

Chemical characterisation techniques have been essential tools in underpinning the explosion in nanotechnology in recent years and nanocharacterisation is a rapidly developing field. Contributions in this book from leading teams across the globe provide an overview of the different microscopic techniques now in regular use for the characterisation of nanostructures. Essentially a handbook to all working in the field, this indispensable resource provides a survey of microscopy based techniques with experimental procedures and extensive examples of state-of-the-art characterisation methods including: Transmission Electron Microscopy, Electron Tomography, Tunnelling Microscopy, Electron Holography, Electron Energy Loss Spectroscopy. This timely publication will appeal to academics, professionals and anyone working fields related to the research and development of nanocharacterisation and nanotechnology.

Contents:

Chapter 1 Characterisation of Nanomaterials Using Transmission Electron Microscopy / D. J. Smith

1.2 Imaging 3

1.2.1 Transmission Electron Microscopy 3

1.2.2 High-Resolution Electron Microscopy 3

1.2.3 Basis of High-Resolution Imaging 5

1.2.4 Resolution Limits 7

1.2.5 Lattice Imaging or Atomic Imaging 9

1.2.6 Instrumental Parameters 9

1.3 Survey of Applications 10

1.3.1 Developments in HREM 10

1.3.2 Small Particles and Precipitates 12

1.3.3 Two-Dimensional Objects 13

1.3.4 One-Dimensional Objects 14

1.3.5 Zero-Dimensional Objects 15

1.3.6 Surfaces and Interfaces 16

1.4 Emerging Trends and Practical Concerns 18

1.4.1 Atomic Location and Quantitative Imaging 18

1.4.2 Detection and Correction of Aberrations 19

1.4.3 The Stobbs' Factor 22

1.4.4 Radiation Damage 22

1.5 Prospects 24

Chapter 2 Scanning Transmission Electron Microscopy / A. R. Lupini, S. N. Rashkeev, M. Varela, A. Y. Borisevich, M. P. Oxley, K. van Benthem, Y. Peng, N. de Jonge, G. M. Veith, S. T. Pantelides, M. F. Chisholm, S. J. Pennycook

2.1.1 Basic Description 29

2.1.2 Detectors 30

2.1.3 Electron Energy-loss Spectroscopy 31

2.2 Aberration Corrected STEM 35

2.2.1 The Aberration Function 35

2.2.2 Spherical and Chromatic Aberration 36

2.2.3 Aberration Correctors 38

2.2.4 What Do We See in a Stem? 39

2.2.5 Measuring Aberrations 45

2.2.6 Phonons 46

2.2.7 Resolution 47

2.2.8 Three-Dimensional Microscopy 48

2.2.9 Channeling 50

2.3 Applications to Nanostructure Characterisation in Catalysis 51

2.3.1 Anomalous Pt-Pt Distances in Pt/alumina Catalytic Systems 51

2.3.2 La Stabilisation of Catalytic Supports 53

2.3.3 CO Oxidation by Supported Noble-Metal Nanoparticles 56

2.4 Summary and Outlook 59

Chapter 3 Scanning Tunneling Microscopy of Surfaces and Nanostructures / M. R. Castell

3.1 History of the STM 66

3.2 The Tunneling Interaction and Basic Operating Principles of STM 67

3.3 Atomic-Resolution Imaging of Surface Reconstructions 70

3.4 Imaging of Surface Nanostructures 74

3.5 Manipulation of Adsorbed Atoms and Molecules 78

3.6 Influence of the Surface Electronic States on STM Images 83

3.7 Tunneling Spectroscopy 86

3.8 Tip Artefacts in STM Imaging 88

Chapter 4 Electron Energy-loss Spectroscopy and Energy Dispersive X-Ray Analysis / R. Brydson

4.1 What is Nanoanalysis? 94

4.2 Nanoanalysis in the Electron Microscope 95

4.2.1 General Instrumentation 96

4.3 X-Ray Analysis in the TEM 99

4.3.1 Basics of X-Ray Analysis 99

4.3.2 Analysis and Quantification of X-Ray Emission Spectra 102

4.3.3 Application to the Analysis of Nanometre Volumes in the S/TEM 104

4.3.4 Related Photon Emission Techniques in the TEM 108

4.4 Basics of EELS 108

4.4.1 Instrumentation for EELS 108

4.4.2 Basics of the EEL Spectrum 112

4.4.3 Quantification of EELS - The Determination of Chemical Composition 116

4.4.4 Determination of Electronic Structure and Bonding 118

4.4.5 Application to the Analysis of Nanometre Volumes in the S/TEM 127

4.5 EELS Imaging 131

4.6 Radiation Damage 133

4.7 Emerging Techniques 135

Chapter 5 Electron Holography of Nanostructured Materials / R. E. Dunin-Borkowski, T. Kasama, R. J. Harrison

5.1.1 Basis of Off-Axis Electron Holography 139

5.1.2 Experimental Considerations 143

5.2 The Mean Inner Potential Contribution to the Phase Shift 144

5.3 Measurement of Magnetic Fields 146

5.3.1 Early Experiments 146

5.3.2 Experiments Involving Digital Acquisition and Analysis 146

5.4 Measurement of Electrostatic Fields 162

5.4.1 Electrically Biased Nanowires 162

5.4.2 Dopant Potentials in Semiconductors 164

5.4.3 Space-Charge Layers at Grain Boundaries 170

5.5 High-Resolution Electron Holography 171

5.6 Alternative Forms of Electron Holography 173

5.7 Discussion, Prospects for the Future and Conclusions 175

Chapter 6 Electron Tomography / M. Weyland, P. A. Midgley

6.2 Theory of Electron Tomography 187

6.2.1 From Projections to Reconstructions 187

6.2.2 Backprojection: Real-Space Reconstruction 191

6.2.3 Constrained Reconstructions 192

6.2.4 Reconstruction Resolution 196

6.2.5 Measuring Reconstruction Resolution 197

6.2.6 The Projection Requirement 198

6.3 Acquiring Tilt Series 200

6.3.1 Instrumental Considerations 201

6.3.2 Specimen Support and Positioning 204

6.3.3 Specimen Considerations 204

6.4 Alignment of Tilt Series 208

6.4.1 Alignment by Tracking of Fiducial Markers 210

6.4.2 Alignment by Cross-Correlation 210

6.4.3 Rotational Alignment without Fiducial Markers 213

6.4.4 Other Markerless Alignment Techniques 218

6.5 Visualisation, Segmentation and Data Mining 218

6.5.1 Visualisation Techniques 218

6.5.2 Segmentation 221

6.5.3 Quantitative Analysis 224

6.6 Imaging Modes 225

6.6.1 Bright-Field TEM 225

6.6.2 Dark-Field (DF) Tomography 234

6.6.3 HAADF STEM 236

6.6.4 Meeting the Projection Requirement 237

6.6.5 Experimental Considerations 238

6.6.6 Limitations 242

6.6.7 Core-Loss (Chemical Mapping) EFTEM 246

6.6.8 Low-Loss EFTEM 252

6.6.9 Energy Dispersive X-Ray (EDX) Mapping 252

6.6.10 Holographic Tomography 254

6.7 New Techniques 254

6.7.1 Electron Energy-Loss Spectroscopy (EELS) Spectrum Imaging 254

6.7.2 Confocal STEM 255

6.7.3 Atomistic Tomography 256

Chapter 7 In-situ Environmental Transmission Electron Microscopy / P. L. Gai

7.3 Recent Advances in Atomic-Resolution In-Situ ETEM 270

7.4 Impact of Atomic-Resolution In-Situ ETEM and Applications 273

7.5 Applications of Atomic-Resolution In-Situ ETEM to Studies of Gas-Catalyst and Liquid-Catalyst Reactions 274

7.5.1 Liquid-Phase Hydrogenation and Polymerisation Reactions 274

7.5.2 Development of Nanocatalysts for Novel Hydrogenation Chemistry and Dynamic Imaging of Desorbed Organic Products in Liquid-Phase Reactions 275

7.5.3 Butane Oxidation Technology 278

7.5.4 In-Situ Observations of Carbon Nanotubes in Chemical and Thermal Environments 284.

Notes:

Includes bibliographical references and index.

ISBN:

0854042415

9780854042418

OCLC:

124025889