Scanning electron microscopy and x-ray microanalysis:
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| Format: | Book |
|---|---|
| Language: | English |
| Published: |
New York, NY
Springer
2007
|
| Edition: | 3. ed., corr. printing |
| Subjects: | |
| Online Access: | Inhaltsverzeichnis |
| Item Description: | Hier auch später erschienene, unveränderte Nachdrucke |
| Physical Description: | XIX, 690 S. Ill., graph. Darst. 1 CD-ROM |
| ISBN: | 9780306472923 |
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| 245 | 1 | 0 | |a Scanning electron microscopy and x-ray microanalysis |c Joseph I. Goldstein ... |
| 250 | |a 3. ed., corr. printing | ||
| 264 | 1 | |a New York, NY |b Springer |c 2007 | |
| 300 | |a XIX, 690 S. |b Ill., graph. Darst. |e 1 CD-ROM | ||
| 336 | |b txt |2 rdacontent | ||
| 337 | |b n |2 rdamedia | ||
| 338 | |b nc |2 rdacarrier | ||
| 500 | |a Hier auch später erschienene, unveränderte Nachdrucke | ||
| 650 | 4 | |a Scanning electron microscopy | |
| 650 | 4 | |a X-ray microanalysis | |
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| _version_ | 1804138641569611776 |
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| adam_text | Contents
1.
Introduction
1.1.
Imaging Capabilities
.................. 2
1.2.
Structure Analysis
................... 10
1.3.
Elemental Analysis
.................. 10
1.4.
Summary and Outline of This Book
........... 17
Appendix A. Overview of Scanning Electron Microscopy
..... 18
Appendix B. Overview of Electron Probe
Х
-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
.1.2.
Deflection System Controls Magnification
22
.1.3.
Electron Detector Collects the Signal
. . 24
. 1.4.
Camera or Computer Records the Image
. 25
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.
Grid Cap
............... 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
VII
Viii
2.2.2.
Electron
Gun
Characteristics
.......... 33
2.2.2.1.
Electron
Emission
Current.......
33
CONTENTS
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 (LaB6) Electron Guns
. . 35
2.2.3.1.
Introduction
............. 35
2.2.3.2.
Operation of the LaB6 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.
Effect of Aperture Size
........ 45
2.3.3.2.
Effect of Working Distance
....... 45
2.3.3.3.
Effect of 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
(/„¡η
and/max
........... 54
2.4.1.1.
Minimum Probe Size
......... 54
2.4.1.2.
Minimum Probe Size at
10-30
k V
... 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 IX
the Interaction Volume
............ 68
3.3.3.1.
Influence of Beam Energy on the CONTENTS
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.
Sampling Depth of BSE
........ 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 Depth of
SE
..... 91
3.4.2.5.
Relative Contributions of SEi and SE2
. . 93
3.4.2.6.
Specimen Composition Dependence of
SE
95
3.4.2.7.
Specimen Tilt Dependence of
SE
.... 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.
Depth of Field (Focus)
............. 114
4.2.7.
Image Distortion
............... 118
4.2.7.1.
Projection Distortion:
Gnomonie
Projection
118
4.2.7.2.
Projection Distortion: Image Foreshortening
119
4.2.7.3.
Scan Distortion: Pathological Defects
. . 123
4.2.7.4.
Moiré
Effects
............. 125
4.3.
Detectors
....................... 125
4.3.1.
Introduction
.................. 125
Χ
4.3.2.
Electron
Detectors
............... 127
4.3.2.1.
Everhart-Thornley Detector
...... 128
CONTENTS
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.
Topographic Contrast
............. 145
4.4.3.1.
Origins of Topographic Contrast
.... 146
4.4.3.2.
Topographic Contrast with the Everhart-
Thornley Detector
.......... 147
4.4.3.3.
Light-Optical Analogy
......... 151
4.4.3.4.
Interpreting Topographic 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
of Thin Specimens
.................. 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.
Units of Gas Pressure
......... 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.
Х
-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
XI
5.7.2.2.
Type
2
Magnetic Contrast
....... 247
5.7.3.
Crystallographic Contrast
............ 247
CONTENTS
5.8.
Electron Backscatter Patterns
.............. 256
5.8.1.
Origin of EBSD 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
Х
-Rays in the
SEM
Specimen
....... 271
6.1.
Continuum
Х
-Ray Production
(Bremsstrahlung)...... 271
6.2.
Characteristic
Х
-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 lonization Energy
........... 278
6.2.7.
Moseley sLaw
................ 279
6.2.8.
Families of Characteristic Lines
......... 279
6.2.9.
Natural Width of Characteristic
Х
-Ray Lines
... 281
6.2.10.
Weights of Lines
............... 282
6.2.11.
Cross Section for Inner Shell lonization
..... 283
6.2.12.
Х
-Ray Production in Thin Foils
......... 284
6.2.13.
Х
-Ray Production in Thick Targets
....... 284
6.2.14.
Х
-Ray Peak-to-Background Ratio
........ 285
6.3.
Depth ofX-Ray Production
(Х
-Ray Range)
........ 286
6.3.1.
Anderson-Hasler
Х
-Ray Range
......... 286
6.3.2.
Х
-Ray Spatial Resolution
............ 286
6.3.3.
Sampling Volume and Specimen Homogeneity
. . 288
6.3.4.
Depth Distribution of
Х
-Ray Production,
φ(ρζ)
. . 288
6.4.
Х
-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.
Х
-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.
Х
-Ray Spectral Measurement: EDS and WDS
....... 297
7.1.
Introduction
...................... 297
7.2.
Energy-Dispersive
Х
-Ray Spectrometer
......... 297
7.2.1.
Operating Principles
.............. 297
ХИ
7.2.2.
The Detection Process
............. 301
7.2.3.
Charge-to-Voltage Conversion
.......... 302
CONTENTS
7.2.4.
Pulse-Shaping Linear Amplifier and Pileup
Rejection Circuitry
.............. 303
7.2.5.
The Computer
Х
-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
Х
-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.
Summary of EDS 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
Х
-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.
Geometric 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 of Analysis
............... 346
7.4.8.
Spectral Artifacts
............... 346
7.5.
Emerging Detector Technologies
............. 347
7.5.1.
Х
-Ray Microcalorimetery
........... 347
7.5.2.
Silicon Drift Detectors
............. 349
7.5.3.
Parallel Optic Diffraction-Based Spectrometers
. . 350
References
......................... 353
8.
Qualitative
Х
-Ray Analysis
................ 355
8.1.
Introduction
...................... 355
8.2.
EDS Qualitative Analysis
................ 357
8.2.1.
Х
-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.
Examples of Manual EDS Qualitative Analysis
. . 372
8.2.4.
Pathological Overlaps in EDS Qualitative
Analysis
................... 374
8.2.5.
Advanced
Qualitative
Analysis: Peak Stripping
. . 379
ХІІІ
8.2.6.
Automatic Qualitative EDS Analysis
....... 381
8.3.
WDS Qualitative Analysis
............... 382
CONTENTS
8.3.1.
Wavelength-Dispersive Spectrometry of
Х
-Ray Peaks
382
8.3.2.
Guidelines for WDS Qualitative Analysis
..... 388
References
......................... 390
9.
Quantitative
Х
-Ray Analysis: The Basics
......... 391
9.1.
Introduction
...................... 391
9.2.
Advantages of Conventional Quantitative
Х
-Ray Microanalysis
in the
SEM ..................... 392
9.3.
Quantitative Analysis Procedures: Flat-Polished Samples
. . 393
9.4.
The Approach to
Х
-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.
Х
-Ray Generation with Depth,
φ(ρζ)
. . 406
9.6.2.
Х
-Ray Absorption Effect, A
........... 411
9.6.3.
Х
-Ray Fluorescence,
F
............. 415
9.7.
Calculation of ZAF Factors
............... 416
9.7.1.
Atomic Number Effect,
Ζ
............ 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.
ΑΙ
-Cu
Alloys
............. 421
9.8.1.2.
Ni-lOwf/oFe Alloy
.......... 423
9.8.1.3. N1-38.5^%
Cr^.Owf/o
Al
Alloy
... 423
9.8.1.4.
Pyroxene:
53.5
wt% SiO^,
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 oftheBence-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
Х
-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
XÎV
9.8.4.5.
Trace
Element
Analysis
........ 446
9.8.4.6.
Trace Element Analysis
Geochronologie
CONTENTS Applications
............. 448
9.8.4.7.
Biological and Organic Specimens
. . . 449
References
......................... 449
10.
Special Topics in Electron Beam
Х
-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 Geometric Effects
........... 465
10.3.5.
Corrections for Particle Geometric 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.
Х
-Ray Mapping
.................... 485
10.6.1.
Relative Merits ofWDS 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
Х
-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-RayMaps
................. 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
Х
-Ray Generation
. 499
10.7.2.
Х
-Ray Spectrometry of the Light Elements
.... 503
10.7.2.1.
Si EDS
............... 503
10.7.2.2.
WDS
................ 507
10.7.3.
Special Measurement Problems for the Light Elements
511
10.7.3.1.
Contamination
............ 511
10.7.3.2.
Overvoltage
Effects
.......... 512
XV
10.7.3.3.
Absorption Effects
.......... 514
10.7.4.
Light Element Quantification
.......... 515
CONTENTS
10.8.
Low-Voltage Microanalysis
............... 518
10.8.1.
Low-Voltage versus Conventional Microanalysis
518
10.8.2.
Х
-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
Х
-Ray Range under
Low-Voltage Conditions
........ 523
10.8.3.
Х
-Ray Spectrometry in Low-Voltage Microanalysis
525
10.8.3.1.
The Oxygen and Carbon Problem
. ... 526
10.8.3.2.
Quantitative
Х
-Ray Microanalysis at Low
Voltage
............... 528
10.9.
Report of Analysis
................... 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 of FIB for Semiconductors
. 554
11.6.2.2.
Applications of FIB in Materials
Science
............... 555
XVÎ
11.7.
Particles and Fibers
.................. 557
11.7.1.
Particle Substrates and Supports
......... 559
CONTENTS
11.7.1.1.
Bulk Particle 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 of Individual Particles
......... 563
References
......................... 564
12.
Specimen Preparation of Polymer Materials
....... 565
12.1.
Introduction
...................... 565
12.2.
Microscopy of 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.
Х
-Ray Microanalysis of Polymers
........ 570
12.3.
Specimen Preparation Methods for Polymers
....... 570
12.3.1.
Simple Preparation Methods
.......... 571
12.3.2.
Polishing of Polymers
............. 571
12.3.3.
Microtomy of Polymers
............ 572
12.3.4.
Fracture of Polymer Materials
.......... 573
12.3.5.
Staining of 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.
Etching of 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.
Paniculate, Cellular, and Fibrous Organic Material
. 592
13.2.2.
Dry Organic Particles and Fibers
........ 593
13.2.2.1.
Organie
Particles and Fibers on a Filter
. 594
XVH
13.2.2.2.
Organic Particles and Fibers Entrained
within a Filter
............ 594
CONTENTS
13.2.2.3.
Organic Paniculate 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
Х
-Ray Microanalysis
............. 608
13.4.2.1.
The Nature and Extent of the Problem
. . 608
13.4.2.2.
Types of 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
xviii 14.
Low-Temperature
Specimen
Preparation
......... 621
14.1.
Introduction
...................... 621
CONTENTS 142 The Properties of Liquid Water and Ice
.......... 622
14.3.
Conversion of 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.
Comparison of 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
ХІХ
15.5.1.
Plasma Magnetron Sputter Coating
....... 662
15.5.2.
Ion Beam and Penning Sputtering
........ 664
CONTENTS
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.
Summary of Coating Guidelines
............. 673
References
......................... 673
Index
............................. 675
Enhancements CD
|
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| indexdate | 2024-07-09T21:31:25Z |
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| language | English |
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| owner | DE-19 DE-BY-UBM DE-355 DE-BY-UBR DE-29T DE-20 DE-92 DE-384 |
| owner_facet | DE-19 DE-BY-UBM DE-355 DE-BY-UBR DE-29T DE-20 DE-92 DE-384 |
| physical | XIX, 690 S. Ill., graph. Darst. 1 CD-ROM |
| publishDate | 2007 |
| publishDateSearch | 2007 |
| publishDateSort | 2007 |
| publisher | Springer |
| record_format | marc |
| spelling | Scanning electron microscopy and x-ray microanalysis Joseph I. Goldstein ... 3. ed., corr. printing New York, NY Springer 2007 XIX, 690 S. Ill., graph. Darst. 1 CD-ROM txt rdacontent n rdamedia nc rdacarrier Hier auch später erschienene, unveränderte Nachdrucke Scanning electron microscopy X-ray microanalysis Elektronenstrahlmikroanalyse (DE-588)4151898-6 gnd rswk-swf Raster-Transmissions-Elektronenmikroskopie (DE-588)4320991-9 gnd rswk-swf Rasterelektronenmikroskopie (DE-588)4048455-5 gnd rswk-swf Werkstoff (DE-588)4065579-9 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 Digitalisierung UB Regensburg application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=017134272&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 Scanning electron microscopy X-ray microanalysis Elektronenstrahlmikroanalyse (DE-588)4151898-6 gnd Raster-Transmissions-Elektronenmikroskopie (DE-588)4320991-9 gnd Rasterelektronenmikroskopie (DE-588)4048455-5 gnd Werkstoff (DE-588)4065579-9 gnd |
| subject_GND | (DE-588)4151898-6 (DE-588)4320991-9 (DE-588)4048455-5 (DE-588)4065579-9 |
| 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 | Scanning electron microscopy X-ray microanalysis Elektronenstrahlmikroanalyse (DE-588)4151898-6 gnd Raster-Transmissions-Elektronenmikroskopie (DE-588)4320991-9 gnd Rasterelektronenmikroskopie (DE-588)4048455-5 gnd Werkstoff (DE-588)4065579-9 gnd |
| topic_facet | Scanning electron microscopy X-ray microanalysis Elektronenstrahlmikroanalyse Raster-Transmissions-Elektronenmikroskopie Rasterelektronenmikroskopie Werkstoff |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=017134272&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT goldsteinjoseph scanningelectronmicroscopyandxraymicroanalysis |