Scanning electron microscopy and x-ray microanalysis:
Accompanying CD-ROM includes ... "a database of useful parameters for SEM and X-ray microanalysis calculations and enhancements to the text chapters." -- p. [4] of cover.
Gespeichert in:
| Format: | Buch |
|---|---|
| Sprache: | English |
| Veröffentlicht: |
New York [u.a.]
Kluwer Academic/Plenum Publishers
2003
|
| Ausgabe: | 3. ed. |
| Schlagworte: | |
| Online-Zugang: | Inhaltsverzeichnis |
| Zusammenfassung: | Accompanying CD-ROM includes ... "a database of useful parameters for SEM and X-ray microanalysis calculations and enhancements to the text chapters." -- p. [4] of cover. |
| Beschreibung: | Includes bibliographical references and index |
| Beschreibung: | xix, 689 p. ill. (some col.) : 26 cm 1 CD-ROM (12 cm) |
| ISBN: | 0306472929 |
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| 300 | |a xix, 689 p. |b ill. (some col.) : 26 cm |e 1 CD-ROM (12 cm) | ||
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| 650 | 4 | |a Microanalyse aux rayons X | |
| 650 | 4 | |a Microscopie électronique à balayage | |
| 650 | 4 | |a Electron Probe Microanalysis | |
| 650 | 4 | |a Microscopy, Electron, Scanning | |
| 650 | 4 | |a Scanning electron microscopy | |
| 650 | 4 | |a X-ray microanalysis | |
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Datensatz im Suchindex
| _version_ | 1804129409320353792 |
|---|---|
| adam_text | Contents
1. Introduction 1
1.1. Imaging Capabilities 2
1.2. Structure Analysis 10
1.3. Elemental Analysis 10
1.4. Summary and Outline ofThis Book 17
Appendix A. Overview of Scanning Electron Microscopy 18
Appendix B. Overview of Electron Probe X-Ray Microanalysis . . 19
References 20
2. The SEM and Its Modes of Operation 21
2.1. How the SEM Works 21
2.1.1. Functions of the SEM Subsystems 21
2.1.1.1. Electron Gun and Lenses Produce a Small
Electron Beam 22
2.1.1.2. Deflection System Controls Magnification 22
2.1.1.3. Electron Detector Collects the Signal . . 24
2.1.1.4. Camera or Computer Records the Image . 25
2.1.1.5. Operator Controls 25
2.1.2. SEM Imaging Modes 25
2.1.2.1. Resolution Mode 27
2.1.2.2. High-Current Mode 27
2.1.2.3. Depth-of-Focus Mode 28
2.1.2.4. Low-Voltage Mode 29
2.1.3. Why Learn about Electron Optics? 29
2.2. Electron Guns 29
2.2.1. Tungsten Hairpin Electron Guns 30
2.2.1.1. Filament 30
2.2.1.2. GridCap 31
2.2.1.3. Anode 31
2.2.1.4. Emission Current and Beam Current . . 32
2.2.1.5. Operator Control of the Electron Gun . . 32
2.2.2. Electron Gun Characteristics 33
2.2.2.1. Electron Emission Current 33
2.2.2.2. Brightness 33
2.2.2.3. Lifetime 34
2.2.2.4. Source Size, Energy Spread, Beam Stability 34
2.2.2.5. Improved Electron Gun Characteristics . 34
2.2.3. Lanthanum Hexaboride (LaBö) Electron Guns . . 35
2.2.3.1. Introduction 35
2.2.3.2. Operation oftheLaB6 Source 36
2.2.4. Field Emission Electron Guns 37
2.3. Electron Lenses 40
2.3.1. Making the Beam Smaller 40
2.3.1.1. Electron Focusing 40
2.3.1.2. Demagnification of the Beam 41
2.3.2. Lenses in SEMs 42
2.3.2.1. Condenser Lenses 42
2.3.2.2. Objective Lenses 42
2.3.2.3. Real and Virtual Objective Apertures . . 44
2.3.3. Operator Control of SEM Lenses 44
2.3.3.1. Effectof Aperture Size 45
2.3.3.2. EffectofWorkingDistance 45
2.3.3.3. Effectof Condenser Lens Strength ... 46
2.3.4. Gaussian Probe Diameter 47
2.3.5. Lens Aberrations 48
2.3.5.1. Spherical Aberration 48
2.3.5.2. Aperture Diffraction 49
2.3.5.3. Chromatic Aberration 50
2.3.5.4. Astigmatism 51
2.3.5.5. Aberrations in the Objective Lens .... 53
2.4. Electron Probe Diameter versus Electron Probe Current . . 54
2.4.1. Calculation of dmin and zmax 54
2.4.1.1. Minimum Probe Size 54
2.4.1.2. Minimum Probe Size at 10-30 kV ... 54
2.4.1.3. Maximum Probe Current at 10-30 kV . . 55
2.4.1.4. Low-Voltage Operation . 55
2.4.1.5. Graphical Summary 56
2.4.2. Performance in the SEM Modes 56
2.4.2.1. Resolution Mode 56
2.4.2.2. High-Current Mode 58
2.4.2.3. Depth-of-Focus Mode 59
2.4.2.4. Low-Voltage SEM 59
2.4.2.5. Environmental Barriers to High-Resolution
Imaging 59
References 60
3. Electron Beam-Specimen Interactions 61
3.1. The Story So Far 61
3.2. The Beam Enters the Specimen 61
3.3. The Interaction Volume 65
3.3.1. Visualizing the Interaction Volume . 65
3.3.2. Simulating the Interaction Volume 67
3.3.3. Influence of Beam and Specimen Parameters on
the Interaction Volume 68
3.3.3.1. Influence of Beam Energy on the
Interaction Volume 68
3.3.3.2. Influence of Atomic Number on the
Interaction Volume 69
3.3.3.3. Influence of Specimen Surface Tilt on the
Interaction Volume 71
3.3.4. Electron Range: A Simple Measure of the
Interaction Volume 72
3.3.4.1. Introduction 72
3.3.4.2. The Electron Range at Low Beam Energy 73
3.4. Imaging Signals from the Interaction Volume 75
3.4.1. Backscattered Electrons 75
3.4.1.1. Atomic Number Dependence of BSE . . 75
3.4.1.2. Beam Energy Dependence of BSE ... 77
3.4.1.3. Tilt Dependence of BSE 79
3.4.1.4. Angular Distribution of BSE 80
3.4.1.5. Energy Distribution of BSE 82
3.4.1.6. Lateral Spatial Distribution of BSE ... 84
3.4.1.7. SamplingDepthofBSE 86
3.4.2. Secondary Electrons 88
3.4.2.1. Definition and Origin of SE 88
3.4.2.2. SE Yield with Primary Beam Energy . . 89
3.4.2.3. SE Energy Distribution 91
3.4.2.4. Range and Escape DepthofSE 91
3.4.2.5. Relative Contributions of SE, and SE2 . . 93
3.4.2.6. Specimen Composition Dependence of SE 95
3.4.2.7. Specimen Tilt Dependence ofSE .... 96
3.4.2.8. Angular Distribution of SE 97
References 97
4. Image Formation and Interpretation 99
4.1. The Story So Far 99
4.2. The Basic SEM Imaging Process 99
4.2.1. Scanning Action 101
4.2.2. Image Construction (Mapping) 103
4.2.2.1. Line Scans 103
4.2.2.2. Image (Area) Scanning 104
4.2.2.3. Digital Imaging: Collection and Display . 107
4.2.3. Magnification 108
4.2.4. Picture Element (Pixel) Size 110
4.2.5. Low-Magnification Operation 114
4.2.6. DepthofField(Focus) 114
4.2.7. Image Distortion 118
4.2.7.1. Projection Distortion: Gnomonic Projection 118
4.2.7.2. Projection Distortion: Image Foreshortening 119
4.2.7.3. Scan Distortion: Pathological Defects . . 123
4.2.7.4. Moire Effects 125
4.3. Detectors 125
4.3.1. Introduction 125
4.3.2. Electron Detectors 127
4.3.2.1. Everhart-Thornley Detector 128
4.3.2.2. Through-the-Lens (TTL) Detector . . 132
4.3.2.3. Dedicated Backscattered Electron Detectors 133
4.4. The Roles of the Specimen and Detector in Contrast Formation 139
4.4.1. Contrast 139
4.4.2. Compositional (Atomic Number) Contrast .... 141
4.4.2.1. Introduction 141
4.4.2.2. Compositional Contrast with Backscattered
Electrons 141
4.4.3. Topographie Contrast 145
4.4.3.1. Origins of Topographie Contrast .... 146
4.4.3.2. Topographie Contrast with the Everhart-
Thornley Detector 147
4.4.3.3. Light-Optical Analogy 151
4.4.3.4. Interpreting Topographie Contrast with
Other Detectors 158
4.5. Image Quality 173
4.6. Image Processing for the Display of Contrast Information . 178
4.6.1. The Signal Chain 178
4.6.2. The Visibility Problem 180
4.6.3. Analog and Digital Image Processing 182
4.6.4. Basic Digital Image Processing 184
4.6.4.1. Digital Image Enhancement 187
4.6.4.2. Digital Image Measurements 192
References 192
5. Special Topics in Scanning Electron Microscopy 195
5.1. High-Resolution Imaging 195
5.1.1. The Resolution Problem 195
5.1.2. Achieving High Resolution at High Beam Energy . 197
5.1.3. High-Resolution Imaging at Low Voltage 201
5.2. STEM-in-SEM: High Resolution for the Special Case
ofThinSpecimens 203
5.3. Surface Imaging at Low Voltage 207
5.4. Making Dimensional Measurements in the SEM 209
5.5. Recovering the Third Dimension: Stereomicroscopy .... 212
5.5.1. Qualitative Stereo Imaging and Presentation ... 212
5.5.2. Quantitative Stereo Microscopy 217
5.6. Variable-Pressure and Environmental SEM 220
5.6.1. Current Instruments 221
5.6.2. Gas in the Specimen Chamber 222
5.6.2.1. UnitsofGasPressure 222
5.6.2.2. The Vacuum System 222
5.6.3. Electron Interactions with Gases 225
5.6.4. The Effect of the Gas on Charging 231
5.6.5. Imaging in the ESEM and the VPSEM 236
5.6.6. X-Ray Microanalysis in the Presence of a Gas . . . 241
5.7. Special Contrast Mechanisms 242
5.7.1. Electric Fields 243
5.7.2. Magnetic Fields 245
5.7.2.1. Type 1 Magnetic Contrast 245
5.7.2.2. Type 2 Magnetic Contrast 247
5.7.3. Crystallographic Contrast 247
5.8. Electron Backscatter Patterns 256
5.8.1. OriginofEBSD Patterns 260
5.8.2. Hardware for EBSD 262
5.8.3. Resolution of EBSD 264
5.8.3.1. Lateral Spatial Resolution 264
5.8.3.2. Depth Resolution 266
5.8.4. Applications 267
5.8.4.1. Orientation Mapping 267
5.8.4.2. Phase Identification 267
References 269
6. Generation of X-Rays in the SEM Specimen 271
6.1. Continuum X-Ray Production (Bremsstrahlung) 271
6.2. Characteristic X-Ray Production 274
6.2.1. Origin 274
6.2.2. Fluorescence Yield 275
6.2.3. Electron Shells 276
6.2.4. Energy-Level Diagram 277
6.2.5. Electron Transitions 277
6.2.6. Critical Ionization Energy 278
6.2.7. Moseley s Law 279
6.2.8. Families of Characteristic Lines 279
6.2.9. Natural Widthof Characteristic X-Ray Lines ... 281
6.2.10. Weightsof Lines 282
6.2.11. Cross Section for Inner Shell Ionization 283
6.2.12. X-Ray Production in Thin Foils 284
6.2.13. X-Ray Production in Thick Targets 284
6.2.14. X-Ray Peak-to-Background Ratio 285
6.3. Depth of X-Ray Production (X-Ray Range) 286
6.3.1. Anderson-Hasler X-Ray Range 286
6.3.2. X-Ray Spatial Resolution 286
6.3.3. Sampling Volume and Specimen Homogeneity . . 288
6.3.4. Depth Distribution of X-Ray Production, / (pz) . . 288
6.4. X-Ray Absorption 289
6.4.1. Mass Absorption Coefficient for an Element . . . 290
6.4.2. Effect of Absorption Edge on Spectrum 291
6.4.3. Absorption Coefficient for Mixed-Element Absorbers 291
6.5. X-Ray Fluorescence 292
6.5.1. Characteristic Fluorescence 293
6.5.2. Continuum Fluorescence 294
6.5.3. Range of Fluorescence Radiation 295
References 295
7. X-Ray Spectral Measurement: EDS and WDS 297
7.1. Introduction 297
7.2. Energy-Dispersive X-Ray Spectrometer 297
7.2.1. Operating Principles 297
7.2.2. The Detection Process 301
7.2.3. Charge-to-Voltage Conversion 302
7.2.4. Pulse-Shaping Linear Amplifier and Pileup
Rejection Circuitry 303
7.2.5. The Computer X-Ray Analyzer 308
7.2.6. Digital Pulse Processing 311
7.2.7. Spectral Modification Resulting from the Detection
Process 312
7.2.7.1. Peak Broadening 312
7.2.7.2. Peak Distortion 316
7.2.7.3. Silicon X-Ray Escape Peaks 317
7.2.7.4. Absorption Edges 318
7.2.7.5. Silicon Internal Fluorescence Peak . . . 320
7.2.8. Artifacts from the Detector Environment 321
7.2.9. SummaryofEDS Operation and Artifacts .... 322
7.3. Wavelength-Dispersive Spectrometer 323
7.3.1. Introduction 323
7.3.2. Basic Description 324
7.3.3. Diffraction Conditions 325
7.3.4. Diffracting Crystals 327
7.3.5. The X-Ray Proportional Counter 330
7.3.6. Detector Electronics 333
7.4. Comparison of Wavelength-Dispersive Spectrometers with
Conventional Energy-Dispersive Spectrometers 340
7.4.1. Geometrie Collection Efficiency 340
7.4.2. Quantum Efficiency 341
7.4.3. Resolution 342
7.4.4. Spectral Acceptance Range 344
7.4.5. Maximum Count Rate 344
7.4.6. Minimum Probe Size 344
7.4.7. Speed ofAnalysis 346
7.4.8. Spectral Artifacts 346
7.5. Emerging Detector Technologies 347
7.5.1. X-Ray Microcalorimetery 347
7.5.2. Silicon Drift Detectors 349
7.5.3. Parallel Optic Diffraction-Based Spectrometers . . 350
References 353
8. Qualitative X-Ray Analysis 355
8.1. Introduction 355
8.2. EDS Qualitative Analysis 357
8.2.1. X-Ray Peaks 357
8.2.2. Guidelines for EDS Qualitative Analysis 366
8.2.2.1. General Guidelines for EDS Qualitative
Analysis 368
8.2.2.2. Specific Guidelines for EDS Qualitative
Analysis 369
8.2.3. Examplesof Manual EDS Qualitative Analysis . . 372
8.2.4. Pathological Overlaps in EDS Qualitative
Analysis 374
8.2.5. Advanced Qualitative Analysis: Peak Stripping . . 379
8.2.6. Automatic Qualitative EDS Analysis 381
8.3. WDS Qualitative Analysis 382
8.3.1. Wavelength-Dispersive Spectrometry of X-Ray Peaks 382
8.3.2. Guidelines for WDS Qualitative Analysis 388
References 390
9. Quantitative X-Ray Analysis: The Basics 391
9.1. Introduction 391
9.2. Advantages of Conventional Quantitative X-Ray Microanalysis
intheSEM 392
9.3. Quantitative Analysis Procedures: Flat-Polished Samples . . 393
9.4. The Approach to X-Ray Quantitation: The Need for Matrix
Corrections 402
9.5. The Physical Origin of Matrix Effects 403
9.6. ZAF Factors in Microanalysis 404
9.6.1. Atomic number effect, Z 404
9.6.1.1. Effect of Backscattering (R) and
Energy Loss (S) 404
9.6.1.2. X-Ray Generation with Depth, 4 (pz) . . 406
9.6.2. X-Ray Absorption Effect, A 411
9.6.3. X-Ray Fluorescence, F 415
9.7. Calculation ofZ4F Factors 416
9.7.1. Atomic Number Effect, Z 417
9.7.2. Absorption correction, A 417
9.7.3. Characteristic Fluorescence Correction, F .... 418
9.7.4. Calculation of ZAF 418
9.7.5. The Analytical Total 420
9.8. Practical Analysis 421
9.8.1. Examples of Quantitative Analysis 421
9.8.1.1. Al-CuAlloys 421
9.8.1.2. Ni-10wt%FeAlloy 423
9.8.1.3. Ni-38.5wt%Cr-3.0wt%AlAlloy ... 423
9.8.1.4. Pyroxene: 53.5 wt% SiQ , 1.11 wt%
A12O3, 0.62 wt% Cr2O3, 9.5 wt%
FeO, 14.1 wt% MgO, and 21.2 wt% CaO 425
9.8.2. Standardless Analysis 427
9.8.2.1. First-Principles Standardless Analysis . . 429
9.8.2.2. Fitted-Standards Standardless Analysis 433
9.8.3. Special Procedures for Geological Analysis .... 436
9.8.3.1. Introduction 436
9.8.3.2. Formulation of the Bence-Albee Procedure 437
9.8.3.3. Application of the Bence-Albee Procedure 438
9.8.3.4. Specimen Conductivity 439
9.8.4. Precision and Sensitivity in X-Ray Analysis .... 440
9.8.4.1. Statistical Basis for Calculating Precision
and Sensitivity 440
9.8.4.2. Precision of Composition 442
9.8.4.3. Sample Homogeneity 444
9.8.4.4. Analytical Sensitivity 445
9.8.4.5. Trace Element Analysis 446
9.8.4.6. Trace Element Analysis Geochronologic
Applications 448
9.8.4.7. Biological and Organic Specimens . . . 449
References 449
10. Special Topics in Electron Beam X-Ray Microanalysis . 453
10.1. Introduction 453
10.2. Thin Film on a Substrate 454
10.3. Particle Analysis 462
10.3.1. Particle Mass Effect 463
10.3.2. Particle Absorption Effect 463
10.3.3. Particle Fluorescence Effect 464
10.3.4. Particle Geometrie Effects 465
10.3.5. Corrections for Particle Geometrie Effects .... 466
10.3.5.1. The Consequences of Ignoring Particle
Effects 466
10.3.5.2. Normalization 466
10.3.5.3. Critical Measurement Issues for Particles 468
10.3.5.4. Advanced Quantitative Methods for
Particles 470
10.4. Rough Surfaces 476
10.4.1. Introduction 476
10.4.2. Rough Specimen Analysis Strategy 479
10.4.2.1. Reorientation 479
10.4.2.2. Normalization 479
10.4.2.3. Peak-to-Background Method 479
10.5. Beam-Sensitive Specimens (Biological, Polymeric) .... 480
10.5.1. Thin-Section Analysis 480
10.5.2. Bulk Biological and Organic Specimens 483
10.6. X-Ray Mapping 485
10.6.1. Relative Meritsof WDS and EDS for Mapping . . 486
10.6.2. Digital Dot Mapping 487
10.6.3. Gray-Scale Mapping 488
10.6.3.1. The Need for Scaling in Gray-Scale Mapping 489
10.6.3.2. Artifacts in X-Ray Mapping 491
10.6.4. Compositional Mapping 492
10.6.4.1. Principles of Compositional Mapping . . 492
10.6.4.2. Advanced Spectrum Collection Strategies
for Compositional Mapping 494
10.6.5. The Use of Color in Analyzing and Presenting
X-Ray Maps 497
10.6.5.1. Primary Color Superposition 497
10.6.5.2. Pseudocolor Scales 497
10.7. Light Element Analysis 499
10.7.1. Optimization of Light Element X-Ray Generation . 499
10.7.2. X-Ray Spectrometry ofthe Light Elements .... 503
10.7.2.1. SiEDS 503
10.7.2.2. WDS 507
10.7.3. Special Measurement Problems forthe Light Elements 511
10.7.3.1. Contamination 511
10.7.3.2. Overvoltage Effects 512
10.7.3.3. Absorption Effects 514
10.7.4. Light Element Quantification 515
10.8. Low-Voltage Microanalysis 518
10.8.1. Low-Voltage versus Conventional Microanalysis 518
10.8.2. X-Ray Production Range 519
10.8.2.1. Contribution of the Beam Size to the X-Ray
Analytical Resolution 520
10.8.2.2. A Consequence of the X-Ray Range under
Low-Voltage Conditions 523
10.8.3. X-Ray Spectrometry in Low-Voltage Microanalysis 525
10.8.3.1. The Oxygen and Carbon Problem . ... 526
10.8.3.2. Quantitative X-Ray Microanalysis at Low
Voltage 528
10.9. Report ofAnalysis 531
References 535
11. Specimen Preparation of Hard Materials: Metals,
Ceramics, Rocks, Minerals, Microelectronic and
Packaged Devices, Particles, and Fibers 537
11.1. Metals 537
11.1.1. Specimen Preparation for Surface Topography . . 537
11.1.2. Specimen Preparation for Microstructural and
Microchemical Analysis 538
11.1.2.1. Initial Sample Selection and Specimen
Preparation Steps 538
11.1.2.2. Final Polishing Steps 539
11.1.2.3. Preparation for Microanalysis 540
11.2. Ceramics and Geological Samples 541
11.2.1. Initial Specimen Preparation: Topography and
Microstructure 542
11.2.2. Mounting and Polishing for Microstructural and
Microchemical Analysis 542
11.2.3. Final Specimen Preparation for Microstructural and
Microchemical Analysis 542
11.3. Microelectronics and Packages 543
11.3.1. Initial Specimen Preparation 543
11.3.2. Polishing 544
11.3.3. Final Preparation 545
11.4. Imaging of Semiconductors 545
11.4.1. Voltage Contrast 546
11.4.2. Charge Collection 546
11.5. Preparation for Electron Diffraction in the SEM 547
11.5.1. Channeling Patterns and Channeling Contrast . . . 547
11.5.2. Electron Backscatter Diffraction 547
11.6. Special Techniques 551
11.6.1. Plasma Cleaning 551
11.6.2. Focused-Ion-Beam Sample Preparation for SEM . 553
11.6.2.1. Application ofFIB for Semiconductors . 554
11.6.2.2. Applications ofFIB in Materials
Science 555
11.7. Particles and Fibers 557
11.7.1. Particle Substrates and Supports 559
11.7.1.1. BulkParticle Substrates 559
11.7.1.2. Thin Particle Supports 560
11.7.2. Particle Mounting Techniques 560
11.7.3. Particles Collected on Filters 562
11.7.4. Particles in a Solid Matrix 563
11.7.5. Transfer oflndividual Particles 563
References 564
12. Specimen Preparation of Polymer Materials 565
12.1. Introduction 565
12.2. Microscopyof Polymers 565
12.2.1. Radiation Effects 566
12.2.2. Imaging Compromises 567
12.2.3. Metal Coating Polymers for Imaging 567
12.2.4. X-Ray Microanalysis of Polymers 570
12.3. Specimen Preparation Methods for Polymers 570
12.3.1. Simple Preparation Methods 571
12.3.2. Polishingof Polymers 571
12.3.3. Microtomyof Polymers 572
12.3.4. Fracture of Polymer Materials 573
12.3.5. Stainingof Polymers 576
12.3.5.1. Osmium Tetroxide and Ruthenium
Tetroxide 578
12.3.5.2. Ebonite 578
12.3.5.3. Chlorosulfonic Acid and Phosphotungstic
Acid 578
12.3.6. Etchingof Polymers 579
12.3.7. Replication of Polymers 580
12.3.8. Rapid Cooling and Drying Methods for Polymers . 580
12.3.8.1. Simple Cooling Methods 580
12.3.8.2. Freeze-Drying 581
12.3.8.3. Critical-Point Drying 581
12.4. Choosing Specimen Preparation Methods 581
12.4.1. Fibers 582
12.4.2. Films and Membranes 582
12.4.3. Engineering Resins and Plastics 583
12.4.4. Emulsions and Adhesives 587
12.5. Problem-Solving Protocol 588
12.6. Image Interpretation and Artifacts 589
References 590
13. Ambient-Temperature Specimen Preparation
of Biological Material 591
13.1. Introduction 591
13.2. Preparative Procedures for the Structural SEM of Single
Cells, Biological Particles, and Fibers 592
13.2.1. Particulate, Cellular, and Fibrous Organic Material . 592
13.2.2. Dry Organic Particles and Fibers 593
I
13.2.2.1. Organic Particles and Fibers on a Filter . 594
13.2.2.2. Organic Particles and Fibers Entrained
within a Filter 594
13.2.2.3. Organic Particulate Matter Suspended in a
Liquid 594
13.2.2.4. Manipulating Individual Organic Particles 595
13.3. Preparative Procedures for the Structural Observation of
Large Soft Biological Specimens 596
13.3.1. Introduction 596
13.3.2. Sample Handling before Fixation 596
13.3.3. Fixation 596
13.3.4. Microwave Fixation 597
13.3.5. Conductive Infiltration 597
13.3.6. Dehydration 597
13.3.7. Embedding 602
13.3.8. Exposing the Internal Contents of Bulk Specimens 602
13.3.8.1. Mechanical Dissection 602
13.3.8.2. High-Energy-Beam Surface Erosion . . . 602
13.3.8.3. Chemical Dissection 603
13.3.8.4. Surface Replicas and Corrosion Casts . . 604
13.3.9. Specimen Supports and Methods of Sample
Attachment 605
13.3.10. Artifacts 607
13.4. Preparative Procedures for the in Situ Chemical Analysis
of Biological Specimens in the SEM 607
13.4.1. Introduction 607
13.4.2. Preparative Procedures for Elemental Analysis Using
X-Ray Microanalysis 608
13.4.2.1. The Nature and Extentof the Problem . . 608
13.4.2.2. Typesof Sample That May be Analyzed . 609
13.4.2.3. The General Strategy for Sample
Preparation 609
13.4.2.4. Criteria for Judging Satisfactory Sample
Preparation 610
13.4.2.5. Fixation and Stabilization 610
13.4.2.6. Precipitation Techniques 611
13.4.2.7. Procedures for Sample Dehydration,
Embedding, and Staining 611
13.4.2.8. Specimen Supports 611
13.4.3. Preparative Procedures for Localizing
Molecules Using Histochemistry 612
13.4.3.1. Staining and Histochemical Methods . . 612
13.4.3.2. Atomic Number Contrast with
Backscattered Electrons 613
13.4.4. Preparative Procedures for Localizing Macromolecues
Using Immunocytochemistry 614
13.4.4.1. Introduction 614
13.4.4.2. The Antibody-Antigen Reaction .... 614
13.4.4.3. General Features of Specimen Preparation
for Immunocytochemistry 615
13.4.4.4. Imaging Procedures in the SEM .... 616
References 618
14. Low Temperature Specimen Preparation 621
14.1. Introduction 621
14.2. The Properties of Liquid Water and Ice 622
14.3. Conversionof Liquid Water to Ice 623
14.4. Specimen Pretreatment before Rapid (Quench) Cooling . . 624
14.4.1. Minimizing Sample Size and Specimen Holders . . 624
14.4.2. Maximizing Undercooling 626
14.4.3. Altering the Nucleation Process 626
14.4.4. Artificially Depressing the Sample Freezing Point . 626
14.4.5. Chemical Fixation 626
14.5. Quench Cooling 627
14.5.1. Liquid Cryogens 627
14.5.2. Solid Cryogens 628
14.5.3. Methods for Quench Cooling 629
14.5.4. Comparisonof Quench Cooling Rates 630
14.6. Low-Temperature Storage and Sample Transfer 631
14.7. Manipulation of Frozen Specimens: Cryosectioning,
Cryofracturing, and Cryoplaning 631
14.7.1. Cryosectioning 631
14.7.2. Cryofracturing 633
14.7.3. Cryopolishing or Cryoplaning 634
14.8. Ways to Handle Frozen Liquids within the Specimen .... 635
14.8.1. Frozen-Hydrated and Frozen Samples 636
14.8.2. Freeze-Drying 637
14.8.2.1. Physical Principles Involved in
Freeze-Drying 637
14.8.2.2. Equipment Needed for Freeze-Drying . . 638
14.8.2.3. Artifacts Associated with Freeze-Drying . 639
14.8.3. Freeze Substitution and Low-Temperature
Embedding 639
14.8.3.1. Physical Principles Involved in Freeze
Substitution and Low-Temperature
Embedding 639
14.8.3.2. Equipment Needed for Freeze Substitution
and Low-Temperature Embedding . . . 640
14.9. Procedures for Hydrated Organic Systems 640
14.10. Procedures for Hydrated Inorganic Systems 641
14.11. Procedures for Nonaqueous Liquids 642
14.12. Imaging and Analyzing Samples at Low Temperatures . . . 643
References 644
15. Procedures for Elimination of Charging
in Nonconducting Specimens 647
15.1. Introduction 647
15.2. Recognizing Charging Phenomena 650
15.3. Procedures for Overcoming the Problems of Charging . . . 656
15.4. Vacuum Evaporation Coating 657
15.4.1. High-Vacuum Evaporation Methods 658
15.4.2. Low-Vacuum Evaporation Methods 661
15.5. Sputter Coating 661
15.5.1. Plasma Magnetron Sputter Coating 662
15.5.2. Ion Beam and Penning Sputtering 664
15.6. High-Resolution Coating Methods 667
15.7. Coating for Analytical Studies 669
15.8. Coating Procedures for Samples Maintained
at Low Temperatures 669
15.9. Coating Thickness 670
15.10. Damage and Artifacts on Coated Samples 672
15.11. Summaryof Coating Guidelines 673
References 673
Index 675
Enhancements CD
|
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| id | DE-604.BV014651216 |
| illustrated | Illustrated |
| indexdate | 2024-07-09T19:04:41Z |
| institution | BVB |
| isbn | 0306472929 |
| language | English |
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| physical | xix, 689 p. ill. (some col.) : 26 cm 1 CD-ROM (12 cm) |
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| spelling | Scanning electron microscopy and x-ray microanalysis Joseph I. Goldstein ... 3. ed. New York [u.a.] Kluwer Academic/Plenum Publishers 2003 xix, 689 p. ill. (some col.) : 26 cm 1 CD-ROM (12 cm) txt rdacontent n rdamedia nc rdacarrier Includes bibliographical references and index Accompanying CD-ROM includes ... "a database of useful parameters for SEM and X-ray microanalysis calculations and enhancements to the text chapters." -- p. [4] of cover. Microanalyse aux rayons X Microscopie électronique à balayage Electron Probe Microanalysis Microscopy, Electron, Scanning Scanning electron microscopy X-ray microanalysis Elektronenstrahlmikroanalyse (DE-588)4151898-6 gnd rswk-swf Rasterelektronenmikroskopie (DE-588)4048455-5 gnd rswk-swf Werkstoff (DE-588)4065579-9 gnd rswk-swf Raster-Transmissions-Elektronenmikroskopie (DE-588)4320991-9 gnd rswk-swf Rasterelektronenmikroskopie (DE-588)4048455-5 s DE-604 Elektronenstrahlmikroanalyse (DE-588)4151898-6 s Werkstoff (DE-588)4065579-9 s 1\p DE-604 Raster-Transmissions-Elektronenmikroskopie (DE-588)4320991-9 s 2\p DE-604 Goldstein, Joseph 1939-2015 Sonstige (DE-588)1023852381 oth HBZ Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=009945332&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis 1\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk 2\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk |
| spellingShingle | Scanning electron microscopy and x-ray microanalysis Microanalyse aux rayons X Microscopie électronique à balayage Electron Probe Microanalysis Microscopy, Electron, Scanning Scanning electron microscopy X-ray microanalysis Elektronenstrahlmikroanalyse (DE-588)4151898-6 gnd Rasterelektronenmikroskopie (DE-588)4048455-5 gnd Werkstoff (DE-588)4065579-9 gnd Raster-Transmissions-Elektronenmikroskopie (DE-588)4320991-9 gnd |
| subject_GND | (DE-588)4151898-6 (DE-588)4048455-5 (DE-588)4065579-9 (DE-588)4320991-9 |
| title | Scanning electron microscopy and x-ray microanalysis |
| title_auth | Scanning electron microscopy and x-ray microanalysis |
| title_exact_search | Scanning electron microscopy and x-ray microanalysis |
| title_full | Scanning electron microscopy and x-ray microanalysis Joseph I. Goldstein ... |
| title_fullStr | Scanning electron microscopy and x-ray microanalysis Joseph I. Goldstein ... |
| title_full_unstemmed | Scanning electron microscopy and x-ray microanalysis Joseph I. Goldstein ... |
| title_short | Scanning electron microscopy and x-ray microanalysis |
| title_sort | scanning electron microscopy and x ray microanalysis |
| topic | Microanalyse aux rayons X Microscopie électronique à balayage Electron Probe Microanalysis Microscopy, Electron, Scanning Scanning electron microscopy X-ray microanalysis Elektronenstrahlmikroanalyse (DE-588)4151898-6 gnd Rasterelektronenmikroskopie (DE-588)4048455-5 gnd Werkstoff (DE-588)4065579-9 gnd Raster-Transmissions-Elektronenmikroskopie (DE-588)4320991-9 gnd |
| topic_facet | Microanalyse aux rayons X Microscopie électronique à balayage Electron Probe Microanalysis Microscopy, Electron, Scanning Scanning electron microscopy X-ray microanalysis Elektronenstrahlmikroanalyse Rasterelektronenmikroskopie Werkstoff Raster-Transmissions-Elektronenmikroskopie |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=009945332&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
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