Introduction to analytical electron microscopy proceedings of a workshop on Analytical Electron Microscopy, held in San Antonio, Texas 1979

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Veröffentlicht: New York [u.a.] Plenum Press 1979
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adam_text TABLE OF CONTENTS CHAPTER 1 PRINCIPLES OF IMAGE FORMATION /.M. cow ley 1.1 Introduction 1 Electron Scattering and Diffration The Physical Optics Analogy Diffraction Patterns Mathematical Formulation 1.2 The Abbe Theory of Imaging 7 Incident Beam Convergence Chromatic Aberration Mathematical Formulation 1.3 Inelastic Scattering 12 1.4 STEM and CTEM 13 STEM Imaging Modes Mathematical Description 1.5 Thin, Weakly Scattering Specimens 18 Beam Convergence and Chromatic Aberration Mathematical Formulation 1.6 Thin, Strongly Scattering Specimens 23 Mathematical Formulation 1.7 Thin, Periodic Objects: Crystals 25 Special Imaging Conditions Mathematical Formulation 1.8 Thicker Crystals 30 Lattice Fringes Mathematical Considerations 1.9 Very Thick Specimens 34 Mathematical Descriptions 1.10 Conclusions 36 Classical and General References Other References CHAPTER 2 INTRODUCTORY ELECTRON OPTICS R.H. ceiss 2.1 Introduction 43 2.2 Geometrical Optics 43 Refraction Cardinal Elements Real and Virtual Images Lens Equations Paraxial Rays 23 Electrostatic Lenses 49 Refraction Action of Electrostatic Lenses Types of Electrostatic Lenses Contents 2.4 Magnetic Lenses 53 Action of a Homogeneous Field Action of an Inhomogeneous Field Paraxial Ray Equations Bell Shaped Field Lens Excitation Parameters CO and k Cardinal Elements of Magnetic Lenses Objective Lenses Lens Aberrations and Defects Special Magnetic Lenses 2.5 Prism Optics 69 Magnetic Sectors Electrostatic Sectors Wein Filter 2.6 Optics of the Electron Microscope 72 Introduction Electron Gun Condenser Lens System Coherence Magnification Lens Systems 2.7 Comparison of CTEM and STEM Optics 77 2.8 Conclusion References CHAPTER 3 PRINCIPLES OF THIN FILM X-RAY MICROANALYSIS /./. GOLDSTEIN 3.1 Introduction 83 3.2 Quantitative X-ray Analysis 84 Primary Emitted X-ray Intensities Quantitative X-ray Analysis Using the Ration Technique and Thin Film Criterion Limitations of the Thin Film Criterion Absorption Correction Fluorescence Correction 3.3 Spatial Resolution 100 Analytical and Computer Models Measurements of Spatial Resolution 3.4 Sensitivity Limits 109 3.5 Summary 117 Acknowledgments References CHAPTER 4 QUANTITATIVE X-RAY MICROANALYSIS: INSTURMENTAL N.J. za L UZEC CONSIDERATIONS AND APPLICATIONS TO MATERIALS SCIENCE 4.1 Introduction 121 4.2 Instrumental Limitations in AEM Based X-ray Microanalysis 121 4.3 Instrumental Artifacts: Systems Background 122 Fluorescence by Uncollimated Radiation: Remote Sources Fluorescence by Uncollimated Radiation: Local Sources Specimen Contamination Detector Artifacts 4.4 Optimum Experimental Conditions for X-ray Analysis 130 Detector/Specimen Geometry Detector Collimation Selection of Incident Beam Energy and Electron Source Imaging and Diffraction Conditions During Analysis Specimen Preparation Artifacts 4.5 Data Reduction for Quantitative Analysis 137 Contents 4.6 Application of Quantitative X-ray Microanalysis: 139 Parameters of Standardless Analysis Absorption Correction 4.7 Applications of Standardless Analysis 149 Standardless Analysis Using the Thin-Film Approximation: Fe-13Cr-40Ni Standardless Analysis Using the Absorption Correction: NiAl 4.8 Standardless Analysis in Complex Systems 155 Analysis of Totally Buried Peaks Quantitative Analysis of Precipitated Phases Procedures for Analysis of Radioactive Specimens 4.9 Summary Acknowledgments References Tables CHAPTER 5 EDS QUANTITATION AND APPLICATION TO BIOLOGY T.A. Hall and B.L. GUPTA 5.1 Introduction 169 5.2 Measurements on Thin or Ultrathin Sections Mounted on Thin Films 170 Elemental Ratios Millimoies of Element Per Unit Volume Millimoles of Element Per kg of Dried Tissue (Continuum Method) Millimoies of Element Per kg Wet Weight (Continuum Method, Frozen-Hydrated Sections) Dry-Weight and Aqueous Fractions Conversion to mM of Element Per Litre of Water Absorption Corrections Standards 5.3 Effects of Contamination Within the Microscope Column 180 5.4 Effects of Beam Damage 181 5.5 Specimen Preparation 182 5.6 Specimens Other Than Sections Mounted on Thin Film 183 Main Literature References List of Symbols Used in this Article Subscripts References Appendix I Derivation of Equation 5.12 for Dry-Weight Determination Appendix II Sample Calculations Calculations CHAPTER 6 MONTE CARLO SIMULATION IN ANALYTICAL ELECTRON MICROSCOPY DAVID F.KYSER 6.1 Introduction 199 6.2 Basic Physical Concepts in Monte Carlo Simulation 200 Electron Scattering Energy Loss Between Elastic Scattering Events Sequence of Calculations Spatial Distribution of Energy Loss and X-ray Production 63 Design, Implementation, and Output of a Monte Carlo Program 206 Computer Generation and Utilization of Random Numbers Computational Time and Its Control Condensation and Output of Results Obtained 6.4 Applications to X-ray Microanalysis 208 Depth Distribution of X-ray Production Total X-ray Production in Foils Radial Distribution of X-ray Production Electron Trajectory Plotting Contents 6.5 Summaiy 219 Acknowledgments References CHAPTER 7 THE BASIC PRINCIPLES OF ELECTRON ENERGY LOSS SPECTROSCOPY DA VID C.JOY 7.1 What is Electron Energy Loss Spectroscopy? 223 7.2 What is Required? 223 7.3 Describing the Energy Loss Spectrum 225 7.4 The Micro-Analytical Information in the EEL Specimen 227 Region 1 - Around Zero-Loss Region 2 - Hie Low-Loss Region Region 3 - Higher Energy Losses 7.5 Collecting the Energy Loss Spectrum 236 7.6 Recording and Analyzing the Data 239 7.7 The Effects of Specimen Thickness 241 7.8 To Summarize 242 References CHAPTER 8 ENERGY LOSS SPECTROMETRY FOR BIOLOGICAL RESEARCH DALE E. JOHNSON 8.1 Introduction 245 8.2 Characteristics of a Typical Spectrum 245 8.3 Sensitivity of ELS Techniques 247 Elemental Microanalysis Chemical and Molecular Microanalysis 8.4 Approaches to the Quantitative Use of ELS 248 Elemental Microanalysis Chemical Microanalysis Molecular Microanalysis Dielectric Constant Determination 8.5 Examples of Typical Experimental Results 249 Experimental Spectra Low Z Elemental Mapping Molecular Species Mapping Extended Fine Structure (EXAFS) 8.6 Practical Limitations 253 Radiation Damage i Mass Loss ii Bond Scission Specimen Thickness i Effect on Background and Peak Heights ii Specimen Mass Thickness Effects in Mapping 8.7 Summary 257 References Classic References CHAPTER 9 ELEMENTAL ANALYSIS USING INNER-SHELL EXCITATIONS: A MICROANALYTICAL TECHNIQUE FOR MATERIALS CHARACTERIZATION dennis M. Ma her 9.1 Introduction 259 9.2 Basic Considerations 260 Spectrum Dynamic Range Spectral Background Edge Shapes Contents 9.3 Progress in Quantitation 265 Analysis Methods Method 1: Efficiency Factors Method 2: Calculated Partial Cross Sections Method 3: Standards Tests of Analysis Methods Stability of Quantitation Methods Relative Accuracy of Atomic Ratios Absolute Accuracy of Quantitation Future Considerations 9.4 Elemental Identification 281 Threshold Energy Shape Analysis Elemental Maps 9.5 Detection limits 285 Importance of ($ Minimum Detectable Limits 9.6 Summary 287 References CHAPTER 10 ANALYSIS OF THE ELECTRONIC STRUCTURE OF SOLIDS JOHN siLCOX 10.1 Introduction 295 10.2 Scattering Kinematics 296 10.3 Inner-Core Excitations 300 10.4 Valence Electron Excitations 302 Final Comments Acknowledgments References CHAPTER 11 STEM IMAGING OE CRYSTALS AND DEFECTS c.j. Humphreys 11.1 Introduction 305 11.2 Principle of Reciprocity in STEM and CTEM 306 Reciprocity of Electron Microscopes Reciprocity and the Coherence of the Source and Detector The Inapplicability of Reciprocity for Thick Specimens Qualitative Reciprocity of the Top-Bottom Effect Procedure if Reciprocity is not Applicable 11.3 Image Recording and Signal/Noise 310 Signal/Noise and Reciprocity Z-Contrast Applied to Materials 11.4 The Optimum Beam Divergences for Imaging Crystal Defects 312 Typical Values of a and 0 in CTEM and STEM Effects of Varying /3S on STEM Images Two-Beam Dynamical Theory Interpretation Choice of Optimum /?s Value 11.5 The Identification of Crystal Defects 317 Properties of Dislocation Images Properties of Stacking Fault Images 11.6 The Breakdown of the Column Approximation in STEM 320 The Nature of the Column Approximation High Resolution STEM Image Calculations Without the Column Approximation 11.7 Penetration in Crystals Using CTEM and STEM 323 Definition of Penetration Factors Limiting the Penetration of CTEM (W Filament) Penetration in STEM The Penetration in STEM and CTEM The Top-Bottom Effect xii Contents 11.8 Current Developments in the STEM Imaging of Defects 3 27 Post Specimen Lenses On-Line Optical Image Processing Lattice Imaging High Voltage STEM In-Situ Imaging and Analysis Acknowledgments References Classical References CHAPTER 12 BIOLOGICAL SCANNING TRANSMISSION ELECTRON MICROSCOPY I. WALL 12.1 Introduction 333 12.2 Quantitative Measurement with the STEM 335 Length Mass Substrate Noise Heavy Atom Signal Resolution Specimen Modification During Imaging 12.3 Conclusion 341 Acknowledgments References CHAPTER 13 ELECTRON MICROSCOPY OF INDIVIDUAL ATOMS M. ISAACSON, M.OHTSUKI and M. UTLA UT 13.1 Introduction 343 13.2a Basics - Electron Scattering 344 13.2b Basics - Operation 346 13.3a Practical Considerations - Electron Optics 347 Probe Formation Further Stability Requirements 13.3b Practical Considerations - Specimen Preparation 352 Low Noise Support Films 13.3c Practical Considerations - Clean Support Films 355 Heavy Atom Contamination 13.3d Practical Considerations - Organic Contaminants 357 13.4 How to Visualize an Atom 357 13.5 Some Examples of Single Atom Microscopy 360 13.6 Conclusion 366 Acknowledgment References I.B. WARREN 369 371 373 375 377 383 References CHAPTER 14 MICRODIFFRACTION 14.1 Introduction 14.2 Focused Probe Microdiffraction 14.3 Focused Aperture Microdiffraction 14.4 Rocking Beam Microdiffraction 14.5 Applications 14.6 Summary Contents CHAPTER IS CONVERGENT BEAM ELECTRON DIFFRACTION /. w. steeds 15.1 Introduction 387 Development of Convergent Beam Diffraction The Microscope TEM Mode STEM Mode Intermediate Configurations Effects Connected with the Specimen Beam Broading Beam Heating Perfection of the Specimen Contamination Goniometry 15.2 The Dimensional Electron Diffraction 395 Higher Order Laue Zones Diameters of Holz Rings Indexing and Origin of Holz Lines i Indexing ii Origin of Lines Lattice Parameter Determination Determination of the Reciprocal Lattice Space Group Determination Measurement of Chemical Variations and Strains 15.3 Crystal Point and Space Groups 406 Use of High Symmetry Zone Axes Point Group Determination Determination of the Reciprocal Lattice Space Group Determination Handedness of a Cry stal 15.4 Atomic Arrangements 412 Intensities of Holz Reflections Atomic String Approximation 15.5 Finger Printing Techniques 416 15.6 Crystal Potential and Thickness Determination 417 Acknowledgments References CHAPTER 16 RADIATION DAMAGE WITH BIOLOGICAL SPECIMENS AND ORGANIC MATERIALS ROBERTM. GLAESER 16.1 Introduction 423 16.2 Primary Events in Radiation Physics and Radiation Chemistry 425 16.3 Empirical Studies of Radiation Damage Effects Measured Under Conditions Used in the Electron Microscope 428 16.4 Signal-to-Noise Considerations at Safe Electron Exposures 429 16.5 Additional Processes of Radiation Damage that Occur at Very High Electron Exposures 432 Acknowledgments References CHAPTER 17 RADIATION EFFECTS IN ANALYSIS OF INORGANIC SPECIMENS BY TEM L. W. HOBBS 17.1 Introduction 437 Radiation Damage in Compact Lattices Electron-Atom Inelastic Interaction Electron-Beam Heating Charge Acquisition by Insulating Specimens Contents 17.2 Knock-On Displacement ** Displacement Energy Momentum Transfer 17.3 Radiolysris 450 Electronic Excitations Energy-to-Momentum Conversion Influence of Temperature, Impurity and Radiation Flux 17.4 Degradation Kinetics 457 17.5 Radiation-Induced Structural Changes During Analysis 460 Frenkel Defect Condensation i Planar Aggregates ii Volume Inclusions Ordering and Disordering Segregation and Precipitation 17.6 Minimizing The Effects of Irradiation 472 Reducing the Electron Dose Reducing the Temperature 17.7 Conclusions 476 References CHAPTER 18 BARRIERS TO AEM: CONTAMINATION AND ETCHING /./. HREN 18.1 Introduction 481 18.2 Some Definitions 481 18.3 Early Observations of Contamination 482 18.4 The Nature of the Contaminant 483 18.5 Relationship Between Contamination and Etching 484 18.6 Surface Diffusion and Beam Size Effects 486 18.7 Recent Studies of Contamination and Etching 487 18.8 Summary of Phenomenological Observations 490 18.9 The Mechanisms of Contamination 491 Phy siosorption of Hydrocarbon Molecules Surface Diffusion of Hydrocarbon Molecules Polymerization and Fragmentation of Hydrocarbon Molecules in the Electron Beam Beam Induced Thermal Gradients Electrical Gradients in the Surface 18.10 The Mechanisms of Etching 495 Physiosorption of a Potentially Reactive Gas Activation of the Reactive Gas by Electrons Specimen or Contaminant Molecules that Will React with the Excited Physiosorbed Gas The Reactant Molecules must be Volatile 18.11 Working Solutions: Proven and Potential 497 18.12 Some Effects of Contamination and Etching on AEM 500 References CHAPTER 19 MICROANALYSIS BY LATTICE IMAGING ROBERT SINCLAIR 19.1 Introduction 507 19.2 Theoretical Considerations 508 Fringe Imaging Specimen-Related Parameters Microscope Parameters Multi-Beam Imaging 19.3 Experimental Procedures 515 19.4 Analysis of Fringe Images 520 19.5 Composition Determination 521 19.6 Experimental Examples 524 19.7 Future Directions 527 Contents 19.8 Summary 530 Acknowledgments References Note on Key References CHAPTER 20 WEAK-BEAM MICROSCOPY JOHN B. VANDER sande 20.1 Introduction 535 20.2 Theoretical Background 536 Strong-Beam Images Weak-Beam Images 20.3 The Practice of Weak-Beam Microscopy 539 Instrumental Needs Establishing a Weak-Beam Condition i The Ewald Sphere Construction for Strong-Beam Microscopy ii The Ewald Sphere Construction for Weak-Beam Microscopy iii Determining the Deviation Parameter, s 20.4 Applications of Weak-Beam Microscopy 543 Separation of Partial Dislocations Dense Defect Arrays: Dislocation Dipoles, Dislocation Tangles, and Dislocation Cell Walls Precipitation on Dislocation Lines: Second Phase Particle Interfaces Comments Acknowledgments References CHAPTER 21 THE ANALYSIS OF DEFECTS USING COMPUTER SIMULATED IMAGES PETER HUMBLE 21.1 Introduction 551 21.2 Theory and Computational Considerations 552 21.3 Experimental Method and the Collection of Information 559 21.4 Examples of the Use of Simulated Images in the Analysis of Defects 560 21.5 The Context of this Technique in AEM 571 References Major References CHAPTER 22 THE STRATEGY OF ANALYSIS RON ANDERSON andj.N. ramsey 22.1 Introduction 575 22.2 Where to Begin? 575 22.3 Specimen Type Strategy 576 22.4 Identification-Solving Unknown Phases and Structures with AEM Input 583 22.5 AEM and Complimentary Technique Examples 586 Al-Cu Thin Film Corrosion Al-Cr Films and Al-Hf Films Organic Residue on Fired Thick Film Conductors Premature Collector - Base Breakdown Acknowledgments References
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spellingShingle Introduction to analytical electron microscopy proceedings of a workshop on Analytical Electron Microscopy, held in San Antonio, Texas 1979
Microscopie électronique
Electron microscopy
Microscopy, Electron
Elektronenmikroskopie (DE-588)4014327-2 gnd
subject_GND (DE-588)4014327-2
(DE-588)1071861417
title Introduction to analytical electron microscopy proceedings of a workshop on Analytical Electron Microscopy, held in San Antonio, Texas 1979
title_auth Introduction to analytical electron microscopy proceedings of a workshop on Analytical Electron Microscopy, held in San Antonio, Texas 1979
title_exact_search Introduction to analytical electron microscopy proceedings of a workshop on Analytical Electron Microscopy, held in San Antonio, Texas 1979
title_full Introduction to analytical electron microscopy proceedings of a workshop on Analytical Electron Microscopy, held in San Antonio, Texas 1979 edited by John J. Hren ...
title_fullStr Introduction to analytical electron microscopy proceedings of a workshop on Analytical Electron Microscopy, held in San Antonio, Texas 1979 edited by John J. Hren ...
title_full_unstemmed Introduction to analytical electron microscopy proceedings of a workshop on Analytical Electron Microscopy, held in San Antonio, Texas 1979 edited by John J. Hren ...
title_short Introduction to analytical electron microscopy
title_sort introduction to analytical electron microscopy proceedings of a workshop on analytical electron microscopy held in san antonio texas 1979
title_sub proceedings of a workshop on Analytical Electron Microscopy, held in San Antonio, Texas 1979
topic Microscopie électronique
Electron microscopy
Microscopy, Electron
Elektronenmikroskopie (DE-588)4014327-2 gnd
topic_facet Microscopie électronique
Electron microscopy
Microscopy, Electron
Elektronenmikroskopie
Konferenzschrift 1979 San Antonio Tex.
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