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Scanning Electron Microscopy and X-Ray Microanalysis 3rd ed. P XIX, 689 p. 13

Goldstein, Joseph, Newbury, Dale E., Joy, David C., Lyman, Charles E., Echlin, Patrick, Lifshin, Eric, Sawyer, Linda, Michael, J.R. 　著

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発行年月	2013年05月
出版社／提供元	Springer-Verlag New York
出版国	アメリカ合衆国
言語	英語
媒体	冊子
装丁	paper
ページ数／巻数	XIX, 689 p.
ジャンル	洋書
ISBN	9781461349693
商品コード	1014003112
商品URL	https://kw.maruzen.co.jp/ims/itemDetail.html?itmCd=1014003112

内容

Providing a comprehensive introduction to the capabilities and use of scanning electron microscopes (SEM) and x-ray spectrometers, this highly acclaimed text emphasizes practical aspects of imaging and analysis for a broad audience of students and practitioners whose backgrounds span a wide range of science and technology. Topics discussed include user-controlled functions of scanning electron microscopes and x-ray spectrometers, the characteristics of electron beam - specimen interactions, image formation and interpretation, the use of x-rays for qualitative and quantitative analysis and the methodology for structural analysis using electron back-scatter diffraction. SEM sample preparation methods for hard materials, polymers, and biological specimens are covered in separate chapters. In addition, techniques for the elimination of charging in non-conducting specimens are detailed.This third edition has been extensively revised, including new sections on: Variable-pressure SEM,Electron backscatter diffraction (EBSD),Recent developments in x-ray detectors, and expanded coverage of:Low-voltage SEM,X-ray mapping,Specimen preparation.The text has been used in educating over 3,000 students at the Lehigh Microscopy School SEM short course as well as thousands of undergraduate and graduate students at universities worldwide.

1. Introduction.- 1.1. Imaging Capabilities.- 1.2. Structure Analysis.- 1.3. Elemental Analysis.- 1.4. Summary and Outline of This Book.- Appendix A. Overview of Scanning Electron Microscopy.- Appendix B. Overview of Electron Probe X-Ray Microanalysis.- References.- 2. The SEM and Its Modes of Operation.- 2.1. How the SEM Works.- 2.1.1. Functions of the SEM Subsystems.- 2.1.1.1. Electron Gun and Lenses Produce a Small Electron Beam.- 2.1.1.2. Deflection System Controls Magnification.- 2.1.1.3. Electron Detector Collects the Signal.- 2.1.1.4. Camera or Computer Records the Image.- 2.1.1.5. Operator Controls.- 2.1.2. SEM Imaging Modes.- 2.1.2.1. Resolution Mode.- 2.1.2.2. High-Current Mode.- 2.1.2.3. Depth-of-Focus Mode.- 2.1.2.4. Low-Voltage Mode.- 2.1.3. Why Learn about Electron Optics?.- 2.2. Electron Guns.- 2.2.1. Tungsten Hairpin Electron Guns.- 2.2.1.1. Filament.- 2.2.1.2. Grid Cap.- 2.2.1.3. Anode.- 2.2.1.4. Emission Current and Beam Current.- 2.2.1.5. Operator Control of the Electron Gun.- 2.2.2. Electron Gun Characteristics.- 2.2.2.1. Electron Emission Current.- 2.2.2.2. Brightness.- 2.2.2.3. Lifetime.- 2.2.2.4. Source Size, Energy Spread, Beam Stability.- 2.2.2.5. Improved Electron Gun Characteristics.- 2.2.3. Lanthanum Hexaboride (LaB6) Electron Guns.- 2.2.3.1. Introduction.- 2.2.3.2. Operation of the LaB6 Source.- 2.2.4. Field Emission Electron Guns.- 2.3. Electron Lenses.- 2.3.1. Making the Beam Smaller.- 2.3.1.1. Electron Focusing.- 2.3.1.2. Demagnification of the Beam.- 2.3.2. Lenses in SEMs.- 2.3.2.1. Condenser Lenses.- 2.3.2.2. Objective Lenses.- 2.3.2.3. Real and Virtual Objective Apertures.- 2.3.3. Operator Control of SEM Lenses.- 2.3.3.1. Effect of Aperture Size.- 2.3.3.2. Effect of Working Distance.- 2.3.3.3. Effect of Condenser Lens Strength.- 2.3.4. Gaussian Probe Diameter.- 2.3.5. Lens Aberrations.- 2.3.5.1. Spherical Aberration.- 2.3.5.2. Aperture Diffraction.- 2.3.5.3. Chromatic Aberration.- 2.3.5.4. Astigmatism.- 2.3.5.5. Aberrations in the Objective Lens.- 2.4. Electron Probe Diameter versus Electron Probe Current.- 2.4.1. Calculation of dmin and imax.- 2.4.1.1. Minimum Probe Size.- 2.4.1.2. Minimum Probe Size at 10-30 kV.- 2.4.1.3. Maximum Probe Current at 10-30 kV.- 2.4.1.4. Low-Voltage Operation.- 2.4.1.5. Graphical Summary.- 2.4.2. Performance in the SEM Modes.- 2.4.2.1. Resolution Mode.- 2.4.2.2. High-Current Mode.- 2.4.2.3. Depth-of-Focus Mode.- 2.4.2.4. Low-Voltage SEM.- 2.4.2.5. Environmental Barriers to High-Resolution Imaging.- References.- 3. Electron Beam–Specimen Interactions.- 3.1. The Story So Far.- 3.2. The Beam Enters the Specimen.- 3.3. The Interaction Volume.- 3.3.1. Visualizing the Interaction Volume.- 3.3.2. Simulating the Interaction Volume.- 3.3.3. Influence of Beam and Specimen Parameters on the Interaction Volume.- 3.3.3.1. Influence of Beam Energy on the Interaction Volume.- 3.3.3.2. Influence of Atomic Number on the Interaction Volume.- 3.3.3.3. Influence of Specimen Surface Tilt on the Interaction Volume.- 3.3.4. Electron Range: A Simple Measure of the Interaction Volume.- 3.3.4.1. Introduction.- 3.3.4.2. The Electron Range at Low Beam Energy.- 3.4. Imaging Signals from the Interaction Volume.- 3.4.1. Backscattered Electrons.- 3.4.1.1. Atomic Number Dependence of BSE.- 3.4.1.2. Beam Energy Dependence of BSE.- 3.4.1.3. Tilt Dependence of BSE.- 3.4.1.4. Angular Distribution of BSE.- 3.4.1.5. Energy Distribution of BSE.- 3.4.1.6. Lateral Spatial Distribution of BSE.- 3.4.1.7. Sampling Depth of BSE.- 3.4.2. Secondary Electrons.- 3.4.2.1. Definition and Origin of SE.- 3.4.2.2. SE Yield with Primary Beam Energy.- 3.4.2.3. SE Energy Distribution.- 3.4.2.4. Range and Escape Depth of SE.- 3.4.2.5. Relative Contributions of SE1 and SE2.- 3.4.2.6. Specimen Composition Dependence of SE.- 3.4.2.7. Specimen Tilt Dependence of SE.- 3.4.2.8. Angular Distribution of SE.- References.- 4. Image Formation and Interpretation.- 4.1. The Story So Far.- 4.2. The Basic SEM Imaging Process.- 4.2.1. Scanning Action.- 4.2.2. Image Construction (Mapping).- 4.2.2.1. Line Scans.- 4.2.2.2. Image (Area) Scanning.- 4.2.2.3. Digital Imaging: Collection and Display.- 4.2.3. Magnification.- 4.2.4. Picture Element (Pixel) Size.- 4.2.5. Low-Magnification Operation.- 4.2.6. Depth of Field (Focus).- 4.2.7. Image Distortion.- 4.2.7.1. Projection Distortion: Gnomonic Projection.- 4.2.7.2. Projection Distortion: Image Foreshortening.- 4.2.7.3. Scan Distortion: Pathological Defects.- 4.2.7.4. Moiré Effects.- 4.3. Detectors.- 4.3.1. Introduction.- 4.3.2. Electron Detectors.- 4.3.2.1. Everhart–Thornley Detector.- 4.3.2.2. “Through-the-Lens” (TTL) Detector.- 4.3.2.3. Dedicated Backscattered Electron Detectors.- 4.4. The Roles of the Specimen and Detector in Contrast Formation.- 4.4.1. Contrast.- 4.4.2. Compositional (Atomic Number) Contrast.- 4.4.2.1. Introduction.- 4.4.2.2. Compositional Contrast with Backscattered Electrons.- 4.4.3. Topographic Contrast.- 4.4.3.1. Origins of Topographic Contrast.- 4.4.3.2. Topographic Contrast with the Everhart–Thornley Detector.- 4.4.3.3. Light-Optical Analogy.- 4.4.3.4. Interpreting Topographic Contrast with Other Detectors.- 4.5. Image Quality.- 4.6. Image Processing for the Display of Contrast Information.- 4.6.1. The Signal Chain.- 4.6.2. The Visibility Problem.- 4.6.3. Analog and Digital Image Processing.- 4.6.4. Basic Digital Image Processing.- 4.6.4.1. Digital Image Enhancement.- 4.6.4.2. Digital Image Measurements.- References.- 5. Special Topics in Scanning Electron Microscopy.- 5.1. High-Resolution Imaging.- 5.1.1. The Resolution Problem.- 5.1.2. Achieving High Resolution at High Beam Energy.- 5.1.3. High-Resolution Imaging at Low Voltage.- 5.2. STEM-in-SEM: High Resolution for the Special Case of Thin Specimens.- 5.3. Surface Imaging at Low Voltage.- 5.4. Making Dimensional Measurements in the SEM.- 5.5. Recovering the Third Dimension: Stereomicroscopy.- 5.5.1. Qualitative Stereo Imaging and Presentation.- 5.5.2. Quantitative Stereo Microscopy.- 5.6. Variable-Pressure and Environmental SEM.- 5.6.1. Current Instruments.- 5.6.2. Gas in the Specimen Chamber.- 5.6.2.1. Units of Gas Pressure.- 5.6.2.2. The Vacuum System.- 5.6.3. Electron Interactions with Gases.- 5.6.4. The Effect of the Gas on Charging.- 5.6.5. Imaging in the ESEM and the VPSEM.- 5.6.6. X-Ray Microanalysis in the Presence of a Gas.- 5.7. Special Contrast Mechanisms.- 5.7.1. Electric Fields.- 5.7.2. Magnetic Fields.- 5.7.2.1. Type 1 Magnetic Contrast.- 5.7.2.2. Type 2 Magnetic Contrast.- 5.7.3. Crystallographic Contrast.- 5.8. Electron Backscatter Patterns.- 5.8.1. Origin of EBSD Patterns.- 5.8.2. Hardware for EBSD.- 5.8.3. Resolution of EBSD.- 5.8.3.1. Lateral Spatial Resolution.- 5.8.3.2. Depth Resolution.- 5.8.4. Applications.- 5.8.4.1. Orientation Mapping.- 5.8.4.2. Phase Identification.- References.- 6. Generation of X-Rays in the SEM Specimen.- 6.1. Continuum X-Ray Production (Bremsstrahlung).- 6.2. Characteristic X-Ray Production.- 6.2.1. Origin.- 6.2.2. Fluorescence Yield.- 6.2.3. Electron Shells.- 6.2.4. Energy-Level Diagram.- 6.2.5. Electron Transitions.- 6.2.6. Critical Ionization Energy.- 6.2.7. Moseley’s Law.- 6.2.8. Families of Characteristic Lines.- 6.2.9. Natural Width of Characteristic X-Ray Lines.- 6.2.10. Weights of Lines.- 6.2.11. Cross Section for Inner Shell Ionization.- 6.2.12. X-Ray Production in Thin Foils.- 6.2.13. X-Ray Production in Thick Targets.- 6.2.14. X-Ray Peak-to-Background Ratio.- 6.3. Depth of X-Ray Production (X-Ray Range).- 6.3.1. Anderson–Hasler X-Ray Range.- 6.3.2. X-Ray Spatial Resolution.- 6.3.3. Sampling Volume and Specimen Homogeneity.- 6.3.4.Depth Distribution of X-Ray Production, ?(?z).- 6.4. X-Ray Absorption.- 6.4.1. Mass Absorption Coefficient for an Element.- 6.4.2. Effect of Absorption Edge on Spectrum.- 6.4.3. Absorption Coefficient for Mixed-Element Absorbers.- 6.5. X-Ray Fluorescence.- 6.5.1. Characteristic Fluorescence.- 6.5.2. Continuum Fluorescence.- 6.5.3. Range of Fluorescence Radiation.- References.- 7. X-Ray Spectral Measurement: EDS and WDS.- 7.1. Introduction.- 7.2. Energy-Dispersive X-Ray Spectrometer.- 7.2.1. Operating Principles.- 7.2.2. The Detection Process.- 7.2.3. Charge-to-Voltage Conversion.- 7.2.4. Pulse-Shaping Linear Amplifier and Pileup Rejection Circuitry.- 7.2.5. The Computer X-Ray Analyzer.- 7.2.6. Digital Pulse Processing.- 7.2.7. Spectral Modification Resulting from the Detection Process.- 7.2.7.1. Peak Broadening.- 7.2.7.2. Peak Distortion.- 7.2.7.3. Silicon X-Ray Escape Peaks.- 7.2.7.4. Absorption Edges.- 7.2.7.5. Silicon Internal Fluorescence Peak.- 7.2.8. Artifacts from the Detector Environment.- 7.2.9. Summary of EDS Operation and Artifacts.- 7.3. Wavelength-Dispersive Spectrometer.- 7.3.1. Introduction.- 7.3.2. Basic Description.- 7.3.3. Diffraction Conditions.- 7.3.4. Diffracting Crystals.- 7.3.5. The X-Ray Proportional Counter.- 7.3.6. Detector Electronics.- 7.4. Comparison of Wavelength-Dispersive Spectrometers with Conventional Energy-Dispersive Spectrometers.- 7.4.1. Geometric Collection Efficiency.- 7.4.2. Quantum Efficiency.- 7.4.3. Resolution.- 7.4.4. Spectral Acceptance Range.- 7.4.5. Maximum Count Rate.- 7.4.6. Minimum Probe Size.- 7.4.7. Speed of Analysis.- 7.4.8. Spectral Artifacts.- 7.5. Emerging Detector Technologies.- 7.5.1. X-Ray Microcalorimetery.- 7.5.2. Silicon Drift Detectors.- 7.5.3. Parallel Optic Diffraction-Based Spectrometers.- References.- 8. Qualitative X-Ray Analysis.- 8.1. Introduction.- 8.2. EDS Qualitative Analysis.- 8.2.1. X-Ray Peaks.- 8.2.2. Guidelines for EDS Qualitative Analysis.- 8.2.2.1. General Guidelines for EDS Qualitative Analysis.- 8.2.2.2. Specific Guidelines for EDS Qualitative Analysis.- 8.2.3. Examples of Manual EDS Qualitative Analysis.- 8.2.4. Pathological Overlaps in EDS Qualitative Analysis.- 8.2.5. Advanced Qualitative Analysis: Peak Stripping.- 8.2.6. Automatic Qualitative EDS Analysis.- 8.3. WDS Qualitative Analysis.- 8.3.1. Wavelength-Dispersive Spectrometry of X-Ray Peaks.- 8.3.2. Guidelines for WDS Qualitative Analysis.- References.- 9. Quantitative X-Ray Analysis: The Basics.- 9.1. Introduction.- 9.2. Advantages of Conventional Quantitative X-Ray Microanalysis in the SEM.- 9.3. Quantitative Analysis Procedures: Flat-Polished Samples.- 9.4. The Approach to X-Ray Quantitation: The Need for Matrix Corrections.- 9.5. The Physical Origin of Matrix Effects.- 9.6. ZAF Factors in Microanalysis.- 9.6.1. Atomic number effect, Z.- 9.6.1.1. Effect of Backscattering (R) and Energy Loss (S ).- 9.6.1.2. X-Ray Generation with Depth, ?(?z).- 9.6.2. X-Ray Absorption Effect, A.- 9.6.3. X-Ray Fluorescence, F.- 9.7. Calculation of ZAF Factors.- 9.7.1. Atomic Number Effect, Z.- 9.7.2. Absorption correction, A.- 9.7.3. Characteristic Fluorescence Correction, F.- 9.7.4. Calculation of ZAF.- 9.7.5. The Analytical Total.- 9.8. Practical Analysis.- 9.8.1. Examples of Quantitative Analysis.- 9.8.1.1. Al–Cu Alloys.- 9.8.1.2. Ni–10 wt% Fe Alloy.- 9.8.1.3. Ni–38.5 wt% Cr–3.0 wt% Al Alloy.- 9.8.1.4. Pyroxene: 53.5 wt% SiO2, 1.11 wt% Al2O3, 0.62 wt% Cr2O3, 9.5 wt% FeO, 14.1 wt% MgO, and 21.2 wt% CaO.- 9.8.2. Standardless Analysis.- 9.8.2.1. First-Principles Standardless Analysis.- 9.8.2.2. “Fitted-Standards” Standardless Analysis.- 9.8.3. Special Procedures for Geological Analysis.- 9.8.3.1. Introduction.- 9.8.3.2. Formulation of the Bence–Albee Procedure.- 9.8.3.3. Application of the Bence–Albee Procedure.- 9.8.3.4. Specimen Conductivity.- 9.8.4. Precision and Sensitivity in X-Ray Analysis.- 9.8.4.1. Statistical Basis for Calculating Precision and Sensitivity.- 9.8.4.2. Precision of Composition.- 9.8.4.3. Sample Homogeneity.- 9.8.4.4. Analytical Sensitivity.- 9.8.4.5. Trace Element Analysis.- 9.8.4.6. Trace Element Analysis Geochronologic Applications.- 9.8.4.7. Biological and Organic Specimens.- References.- 10. Special Topics in Electron Beam X-Ray Microanalysis.- 10.1. Introduction.- 10.2. Thin Film on a Substrate.- 10.3. Particle Analysis.- 10.3.1. Particle Mass Effect.- 10.3.2. Particle Absorption Effect.- 10.3.3. Particle Fluorescence Effect.- 10.3.4. Particle Geometric Effects.- 10.3.5. Corrections for Particle Geometric Effects.- 10.3.5.1. The Consequences of Ignoring Particle Effects.- 10.3.5.2. Normalization.- 10.3.5.3. Critical Measurement Issues for Particles.- 10.3.5.4. Advanced Quantitative Methods for Particles.- 10.4. Rough Surfaces.- 10.4.1. Introduction.- 10.4.2. Rough Specimen Analysis Strategy.- 10.4.2.1. Reorientation.- 10.4.2.2. Normalization.- 10.4.2.3. Peak-to-Background Method.- 10.5. Beam-Sensitive Specimens (Biological, Polymeric).- 10.5.1. Thin-Section Analysis.- 10.5.2. Bulk Biological and Organic Specimens.- 10.6. X-Ray Mapping.- 10.6.1. Relative Merits of WDS and EDS for Mapping.- 10.6.2. Digital Dot Mapping.- 10.6.3. Gray-Scale Mapping.- 10.6.3.1. The Need for Scaling in Gray-Scale Mapping.- 10.6.3.2. Artifacts in X-Ray Mapping.- 10.6.4. Compositional Mapping.- 10.6.4.1. Principles of Compositional Mapping.- 10.6.4.2. Advanced Spectrum Collection Strategies for Compositional Mapping.- 10.6.5. The Use of Color in Analyzing and Presenting X-Ray\ Maps.- 10.6.5.1. Primary Color Superposition.- 10.6.5.2. Pseudocolor Scales.- 10.7. Light Element Analysis.- 10.7.1. Optimization of Light Element X-Ray Generation.- 10.7.2. X-Ray Spectrometry of the Light Elements.- 10.7.2.1. Si EDS.- 10.7.2.2. WDS.- 10.7.3. Special Measurement Problems for the Light Elements.- 10.7.3.1. Contamination.- 10.7.3.2. Overvoltage Effects.- 10.7.3.3. Absorption Effects.- 10.7.4.Light Element Quantification.- 10.8. Low-Voltage Microanalysis.- 10.8.1. “Low-Voltage” versus “Conventional” Microanalysis.- 10.8.2. X-Ray Production Range.- 10.8.2.1. Contribution of the Beam Size to the X-Ray Analytical Resolution.- 10.8.2.2. A Consequence of the X-Ray Range under Low-Voltage Conditions.- 10.8.3. X-Ray Spectrometry in Low-Voltage Microanalysis.- 10.8.3.1. The Oxygen and Carbon Problem.- 10.8.3.2. Quantitative X-Ray Microanalysis at Low Voltage.- 10.9. Report of Analysis.- References.- 11. Specimen Preparation of Hard Materials: Metals, Ceramics, Rocks, Minerals, Microelectronic and Packaged Devices, Particles, and Fibers.- 11.1. Metals.- 11.1.1. Specimen Preparation for Surface Topography.- 11.1.2. Specimen Preparation for Microstructural and Microchemical Analysis.- 11.1.2.1. Initial Sample Selection and Specimen Preparation Steps.- 11.1.2.2. Final Polishing Steps.- 11.1.2.3. Preparation for Microanalysis.- 11.2. Ceramics and Geological Samples.- 11.2.1. Initial Specimen Preparation: Topography and Microstructure.- 11.2.2. Mounting and Polishing for Microstructural and Microchemical Analysis.- 11.2.3. Final Specimen Preparation for Microstructural and Microchemical Analysis.- 11.3. Microelectronics and Packages.- 11.3.1. Initial Specimen Preparation.- 11.3.2. Polishing.- 11.3.3. Final Preparation.- 11.4. Imaging of Semiconductors.- 11.4.1. Voltage Contrast.- 11.4.2. Charge Collection.- 11.5. Preparation for Electron Diffraction in the SEM.- 11.5.1. Channeling Patterns and Channeling Contrast.- 11.5.2. Electron Backscatter Diffraction.- 11.6. Special Techniques.- 11.6.1. Plasma Cleaning.- 11.6.2. Focused-Ion-Beam Sample Preparation for SEM.- 11.6.2.1. Application of FIB for Semiconductors.- 11.6.2.2. Applications of FIB in Materials Science.- 11.7.Particles and Fibers.- 11.7.1. Particle Substrates and Supports.- 11.7.1.1. Bulk Particle Substrates.- 11.7.1.2. Thin Particle Supports.- 11.7.2. Particle Mounting Techniques.- 11.7.3. Particles Collected on Filters.- 11.7.4. Particles in a Solid Matrix.- 11.7.5. Transfer of Individual Particles.- References.- 12. Specimen Preparation of Polymer Materials.- 12.1. Introduction.- 12.2. Microscopy of Polymers.- 12.2.1. Radiation Effects.- 12.2.2. Imaging Compromises.- 12.2.3. Metal Coating Polymers for Imaging.- 12.2.4. X-Ray Microanalysis of Polymers.- 12.3. Specimen Preparation Methods for Polymers.- 12.3.1. Simple Preparation Methods.- 12.3.2. Polishing of Polymers.- 12.3.3. Microtomy of Polymers.- 12.3.4. Fracture of Polymer Materials.- 12.3.5. Staining of Polymers.- 12.3.5.1. Osmium Tetroxide and Ruthenium Tetroxide.- 12.3.5.2. Ebonite.- 12.3.5.3. Chlorosulfonic Acid and Phosphotungstic Acid.- 12.3.6. Etching of Polymers.- 12.3.7. Replication of Polymers.- 12.3.8. Rapid Cooling and Drying Methods for Poly

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