Abstract: 1 Introduction- 11 Evolution of the Scanning Electron Microscope- 12 Evolution of the Electron Probe Microanalyzer- 13 Outline of This Book- 2 Electron Optics- 21 Electron Guns- 211 Thermionic Emission- 212 Tungsten Cathode- 213 The Lanthanum Hexaboride (LaB6) Cathode- 214 Field Emission Gun- 22 Electron Lenses- 221 General Properties of Magnetic Lenses- 222 Production of Minimum Spot Size- 223 Aberrations in the Electron Optical Column- 23 Electron Probe Diameter, dp, vs Electron Probe Current i- 231 Calculation of dmin and imax- 232 Measurement of Microscope Parameters (dp, i, ?)- 233 High-Resolution Scanning Electron Microscopy- 3 Electron-Beam-Specimen Interactions- 31 Introduction- 32 Scattering- 321 Elastic Scattering- 322 Inelastic Scattering- 33 Interaction Volume- 331 Experimental Evidence- 332 Monte Carlo Calculations- 34 Backscattered Electrons- 341 Atomic Number Dependence- 342 Energy Dependence- 343 Tilt Dependence- 344 Angular Distribution- 345 Energy Distribution- 346 Spatial Distribution- 347 Sampling Depth- 35 Signals from Inelastic Scattering- 351 Secondary Electrons- 352 X-Rays- 353 Auger Electrons- 354 Cathodoluminescence- 36 Summary- 4 Image Formation in the Scanning Electron Microscope- 41 Introduction- 42 The Basic SEM Imaging Process- 421 Scanning Action- 422 Image Construction (Mapping)- 423 Magnification- 424 Picture Element (Picture Point)- 425 Depth of Field- 426 Image Distortions- 43 Stereomicroscopy- 44 Detectors- 441 Electron Detectors- 442 Cathodoluminescence Detectors- 45 The Roles of Specimen and Detector in Contrast Formation- 451 Contrast- 452 Atomic Number (Compositional) Contrast (Backscattered Electron Signal)- 453 Compositional Contrast (Secondary-Electron Signal)- 454 Contrast Components- 455 Topographic Contrast- 46 Image Quality- 461 Signal Quality and Contrast Information- 462 Strategy in SEM Imaging- 463 Resolution Limitations- 47 Signal Processing for the Display of Contrast Information- 471 The Visibility Problem- 472 Signal Processing Techniques- 473 Combinations of Detectors- 474 Beam Energy Effects- 475 Summary- 5 X-Ray Spectral Measurement: WDS and EDS- 51 Introduction- 52 Wavelength-Dispersive Spectrometer- 521 Basic Design- 522 The X-Ray Detector- 523 Detector Electronics- 53 Energy-Dispersive X-Ray Spectrometer- 531 Operating Principles- 532 The Detection Process- 533 Artifacts of the Detection Process- 534 The Main Amplifier and Pulse Pileup Rejection- 535 Artifacts from the Detector Environment- 536 The Multichannel Analyzer- 537 Summary of EDS Operation and Artifacts- 54 Comparison of Wavelength-Dispersive Spectrometers with Energy-Dispersive Spectrometers- 541 Geometrical Collection Efficiency- 542 Quantum Efficiency- 543 Resolution- 544 Spectral Acceptance Range- 545 Maximum Count Rate- 546 Minimum Probe Size- 547 Speed of Analysis- 548 Spectral Artifacts- Appendix: Initial Detector Setup and Testing- 6 Qualitative X-Ray Analysis- 61 Introduction- 62 EDS Qualitative Analysis- 621 X-Ray Lines- 622 Guidelines for EDS Qualitative Analysis- 623 Pathological Overlaps in EDS Qualitative Analysis- 624 Examples of EDS Qualitative Analysis- 63 WDS Qualitative Analysis- 631 Measurement of X-Ray Lines- 632 Guidelines for WDS Qualitative Analysis- 64 X-Ray Scanning- 7 Quantitative X-Ray Microanalysis- 71 Introduction- 72 ZAF Technique- 721 Introduction- 722 The Absorption Factor, A- 723 The Atomic Number Factor, Z- 724 The Characteristic Fluorescence Correction, F- 725 The Continuum Fluorescence Correction- 726 Summary Discussion of the ZAF Method- 73 The Empirical Method- 74 Quantitative Analysis with Nonnormal Electron Beam Incidence- 75 Analysis of Particles and Rough Surfaces- 751 Geometric Effects- 752 Compensating for Geometric Effects- 753 Summary- 76 Analysis of Thin Films and Foils- 761 Thin Foils- 762 Thin Films on Substrates- 77 Quantitative Analysis of Biological Material- 771 Introduction- 772 Mass Loss and Artifacts during Analysis- 773 Bulk Samples- 774 Thick Sections on Bulk Substrates- 775 Thin Samples- 776 The Continuum Method- 777 Thick Specimens on Very Thin Supports- 778 Microdroplets- 779 Standards- 7710 Conclusion- Appendix A: Continuum Method- Appendix B: Worked Examples of Quantitative Analysis of Biological Material- Notation- 8 Practical Techniques of X-Ray Analysis- 81 General Considerations of Data Handling- 82 Background Shape- 821 Background Modeling- 822 Background Filtering- 83 Peak Overlap- 831 Linearity- 832 Goodness of Fit- 833 The Linear Methods- 834 The Nonlinear Methods- 835 Error Estimation- 84 Dead-Time Correction- 85 Example of Quantitative Analysis- 86 Precision and Sensitivity in X-Ray Analysis- 861 Statistical Basis for Calculating Precision and Sensitivity- 862 Sample Homogeneity- 863 Analytical Sensitivity- 864 Trace Element Analysis- 87 Light Element Analysis- 9 Materials Specimen Preparation for SEM and X-Ray Microanalysis- 91 Metals and Ceramics- 911 Scanning Electron Microscopy- 912 X-Ray Microanalysis- 92 Particles and Fibers- 93 Hydrous Materials- 931 Soils and Clays- 932 Polymers- 10 Coating Techniques for SEM and Microanalysis- 101 Introduction- 1011 Specimen Characteristics- 1012 Alternatives to Coating- 1013 Thin-Film Technology- 102 Thermal Evaporation- 1021 High-Vacuum Evaporation- 1022 Low-Vacuum Evaporation- 103 Sputter Coating- 1031 Ion Beam Sputtering- 1032 Diode or Direct Current Sputtering- 1033 Cool Diode Sputtering- 1034 Sputtering Techniques- 1035 Choice of Target- 1036 Coating Thickness- 1037 Advantages of Sputter Coating- 1038 Artifacts Associated with Sputter Coating- 104 Specialized Coating Methods- 1041 High-Resolution Coating- 1042 Low-Temperature Coating- 105 Determination of Coating Thickness- 1051 Estimation of Coating Thickness- 1052 Measurement during Coating- 1053 Measurement after Coating- 1054 Removing Coating Layers- 11 Preparation of Biological Samples for Scanning Electron Microscopy- 111 Introduction- 112 Compromising the Microscope- 1121 Environmental Stages- 1122 Nonoptimal Microscope Performance- 113 Compromising the Specimen- 1131 Correlative Microscopy- 1132 Specimen Selection- 1133 Specimen Cleaning- 1134 Specimen Stabilization- 1135 Exposure of Internal Surfaces- 1136 Localizing Areas of Known Physiological Activity- 1137 Specimen Dehydration- 1138 Specimen Supports- 1139 Specimen Conductivity- 11310 Heavy Metal Impregnation- 11311 Interpretation and Artifacts- 12 Preparation of Biological Samples for X-Ray Microanalysis- 121 Introduction- 1211 The Nature and Enormity of the Problem- 1212 Applications of X-Ray Microanalysis- 1213 Types of X-Ray Analytical Investigations- 1214 Types of Biological Specimens- 1215 Strategy- 1216 Criteria for Satisfactory Specimen Preparation- 122 Ambient Temperature Preparative Procedures- 1221 Before Fixation- 1222 Fixation- 1223 Histochemical Techniques- 1224 Precipitation Techniques- 1225 Dehydration- 1226 Embedding- 1227 Sectioning and Fracturing- 1228 Specimen Supports- 1229 Specimen Staining- 12210 Specimen Coating- 123 Low-Temperature Preparative Procedures- 1231 Specimen Pretreatment- 1232 Freezing Procedures- 1233 Movement of Elements within a Given Cellular Compartment- 1234 Postfreezing Procedures- 1235 Frozen-Hydrated and Partially Frozen-Hydrated Material- 1236 Freeze Drying- 1237 Freeze Substitution- 1238 Sectioning- 1239 Fracturing- 12310 Specimen Handling- 124 Microincineration- 13 Applications of the SEM and EPMA to Solid Samples and Biological Materials- 131 Study of Aluminum-Iron Electrical Junctions- 132 Study of Deformation in Situ in the Scanning Electron Microscope- 133 Analysis of Phases in Raney Nickel Alloy- 134 Quantitative Analysis of a New Mineral, Sinoite- 135 Determination of the Equilibrium Phase Diagram for the Fe-Ni-C System- 136 Study of Lunar Metal Particle 63344,1- 137 Observation of Soft Plant Tissue with a High Water Content- 138 Study of Multicellular Soft Plant Tissue with High Water Content- 139 Examination of Single-Celled, Soft Animal Tissue with High Water Content- 1310 Observation of Hard Plant Tissue with a Low Water Content- 1311 Study of Single-Celled Plant Tissue with a Hard Outer Covering and Relatively Low Internal Water Content- 1312 Examination of Medium Soft Animal Tissue with a High Water Content- 1313 Study of Single-Celled Animal Tissue of High Water Content- 14 Data Base- Table 141 Atomic Number, Atomic Weight, and Density of Metals- Table 142 Common Oxides of the Elements- Table 143 Mass Absorption Coefficients for K? Lines- Table 144 Mass Absorption Coefficients for L? Lines- Table 145 Selected Mass Absorption Coefficients- Table 146 K Series X-Ray Wavelengths and Energies- Table 147 L Series X-Ray Wavelengths and Energies- Table 148 M Series X-Ray Wavelengths and Energies- Table 149 Fitting Parameters for Duncumb-Reed Backscattering Correction Factor R- Table 1410 J Values and Fluorescent Yield, ?, Values- Table 1411 Important Properties of Selected Coating Elements- References