- •Preface
- •Imaging Microscopic Features
- •Measuring the Crystal Structure
- •References
- •Contents
- •1.4 Simulating the Effects of Elastic Scattering: Monte Carlo Calculations
- •What Are the Main Features of the Beam Electron Interaction Volume?
- •How Does the Interaction Volume Change with Composition?
- •How Does the Interaction Volume Change with Incident Beam Energy?
- •How Does the Interaction Volume Change with Specimen Tilt?
- •1.5 A Range Equation To Estimate the Size of the Interaction Volume
- •References
- •2: Backscattered Electrons
- •2.1 Origin
- •2.2.1 BSE Response to Specimen Composition (η vs. Atomic Number, Z)
- •SEM Image Contrast with BSE: “Atomic Number Contrast”
- •SEM Image Contrast: “BSE Topographic Contrast—Number Effects”
- •2.2.3 Angular Distribution of Backscattering
- •Beam Incident at an Acute Angle to the Specimen Surface (Specimen Tilt > 0°)
- •SEM Image Contrast: “BSE Topographic Contrast—Trajectory Effects”
- •2.2.4 Spatial Distribution of Backscattering
- •Depth Distribution of Backscattering
- •Radial Distribution of Backscattered Electrons
- •2.3 Summary
- •References
- •3: Secondary Electrons
- •3.1 Origin
- •3.2 Energy Distribution
- •3.3 Escape Depth of Secondary Electrons
- •3.8 Spatial Characteristics of Secondary Electrons
- •References
- •4: X-Rays
- •4.1 Overview
- •4.2 Characteristic X-Rays
- •4.2.1 Origin
- •4.2.2 Fluorescence Yield
- •4.2.3 X-Ray Families
- •4.2.4 X-Ray Nomenclature
- •4.2.6 Characteristic X-Ray Intensity
- •Isolated Atoms
- •X-Ray Production in Thin Foils
- •X-Ray Intensity Emitted from Thick, Solid Specimens
- •4.3 X-Ray Continuum (bremsstrahlung)
- •4.3.1 X-Ray Continuum Intensity
- •4.3.3 Range of X-ray Production
- •4.4 X-Ray Absorption
- •4.5 X-Ray Fluorescence
- •References
- •5.1 Electron Beam Parameters
- •5.2 Electron Optical Parameters
- •5.2.1 Beam Energy
- •Landing Energy
- •5.2.2 Beam Diameter
- •5.2.3 Beam Current
- •5.2.4 Beam Current Density
- •5.2.5 Beam Convergence Angle, α
- •5.2.6 Beam Solid Angle
- •5.2.7 Electron Optical Brightness, β
- •Brightness Equation
- •5.2.8 Focus
- •Astigmatism
- •5.3 SEM Imaging Modes
- •5.3.1 High Depth-of-Field Mode
- •5.3.2 High-Current Mode
- •5.3.3 Resolution Mode
- •5.3.4 Low-Voltage Mode
- •5.4 Electron Detectors
- •5.4.1 Important Properties of BSE and SE for Detector Design and Operation
- •Abundance
- •Angular Distribution
- •Kinetic Energy Response
- •5.4.2 Detector Characteristics
- •Angular Measures for Electron Detectors
- •Elevation (Take-Off) Angle, ψ, and Azimuthal Angle, ζ
- •Solid Angle, Ω
- •Energy Response
- •Bandwidth
- •5.4.3 Common Types of Electron Detectors
- •Backscattered Electrons
- •Passive Detectors
- •Scintillation Detectors
- •Semiconductor BSE Detectors
- •5.4.4 Secondary Electron Detectors
- •Everhart–Thornley Detector
- •Through-the-Lens (TTL) Electron Detectors
- •TTL SE Detector
- •TTL BSE Detector
- •Measuring the DQE: BSE Semiconductor Detector
- •References
- •6: Image Formation
- •6.1 Image Construction by Scanning Action
- •6.2 Magnification
- •6.3 Making Dimensional Measurements With the SEM: How Big Is That Feature?
- •Using a Calibrated Structure in ImageJ-Fiji
- •6.4 Image Defects
- •6.4.1 Projection Distortion (Foreshortening)
- •6.4.2 Image Defocusing (Blurring)
- •6.5 Making Measurements on Surfaces With Arbitrary Topography: Stereomicroscopy
- •6.5.1 Qualitative Stereomicroscopy
- •Fixed beam, Specimen Position Altered
- •Fixed Specimen, Beam Incidence Angle Changed
- •6.5.2 Quantitative Stereomicroscopy
- •Measuring a Simple Vertical Displacement
- •References
- •7: SEM Image Interpretation
- •7.1 Information in SEM Images
- •7.2.2 Calculating Atomic Number Contrast
- •Establishing a Robust Light-Optical Analogy
- •Getting It Wrong: Breaking the Light-Optical Analogy of the Everhart–Thornley (Positive Bias) Detector
- •Deconstructing the SEM/E–T Image of Topography
- •SUM Mode (A + B)
- •DIFFERENCE Mode (A−B)
- •References
- •References
- •9: Image Defects
- •9.1 Charging
- •9.1.1 What Is Specimen Charging?
- •9.1.3 Techniques to Control Charging Artifacts (High Vacuum Instruments)
- •Observing Uncoated Specimens
- •Coating an Insulating Specimen for Charge Dissipation
- •Choosing the Coating for Imaging Morphology
- •9.2 Radiation Damage
- •9.3 Contamination
- •References
- •10: High Resolution Imaging
- •10.2 Instrumentation Considerations
- •10.4.1 SE Range Effects Produce Bright Edges (Isolated Edges)
- •10.4.4 Too Much of a Good Thing: The Bright Edge Effect Hinders Locating the True Position of an Edge for Critical Dimension Metrology
- •10.5.1 Beam Energy Strategies
- •Low Beam Energy Strategy
- •High Beam Energy Strategy
- •Making More SE1: Apply a Thin High-δ Metal Coating
- •Making Fewer BSEs, SE2, and SE3 by Eliminating Bulk Scattering From the Substrate
- •10.6 Factors That Hinder Achieving High Resolution
- •10.6.2 Pathological Specimen Behavior
- •Contamination
- •Instabilities
- •References
- •11: Low Beam Energy SEM
- •11.3 Selecting the Beam Energy to Control the Spatial Sampling of Imaging Signals
- •11.3.1 Low Beam Energy for High Lateral Resolution SEM
- •11.3.2 Low Beam Energy for High Depth Resolution SEM
- •11.3.3 Extremely Low Beam Energy Imaging
- •References
- •12.1.1 Stable Electron Source Operation
- •12.1.2 Maintaining Beam Integrity
- •12.1.4 Minimizing Contamination
- •12.3.1 Control of Specimen Charging
- •12.5 VPSEM Image Resolution
- •References
- •13: ImageJ and Fiji
- •13.1 The ImageJ Universe
- •13.2 Fiji
- •13.3 Plugins
- •13.4 Where to Learn More
- •References
- •14: SEM Imaging Checklist
- •14.1.1 Conducting or Semiconducting Specimens
- •14.1.2 Insulating Specimens
- •14.2 Electron Signals Available
- •14.2.1 Beam Electron Range
- •14.2.2 Backscattered Electrons
- •14.2.3 Secondary Electrons
- •14.3 Selecting the Electron Detector
- •14.3.2 Backscattered Electron Detectors
- •14.3.3 “Through-the-Lens” Detectors
- •14.4 Selecting the Beam Energy for SEM Imaging
- •14.4.4 High Resolution SEM Imaging
- •Strategy 1
- •Strategy 2
- •14.5 Selecting the Beam Current
- •14.5.1 High Resolution Imaging
- •14.5.2 Low Contrast Features Require High Beam Current and/or Long Frame Time to Establish Visibility
- •14.6 Image Presentation
- •14.6.1 “Live” Display Adjustments
- •14.6.2 Post-Collection Processing
- •14.7 Image Interpretation
- •14.7.1 Observer’s Point of View
- •14.7.3 Contrast Encoding
- •14.8.1 VPSEM Advantages
- •14.8.2 VPSEM Disadvantages
- •15: SEM Case Studies
- •15.1 Case Study: How High Is That Feature Relative to Another?
- •15.2 Revealing Shallow Surface Relief
- •16.1.2 Minor Artifacts: The Si-Escape Peak
- •16.1.3 Minor Artifacts: Coincidence Peaks
- •16.1.4 Minor Artifacts: Si Absorption Edge and Si Internal Fluorescence Peak
- •16.2 “Best Practices” for Electron-Excited EDS Operation
- •16.2.1 Operation of the EDS System
- •Choosing the EDS Time Constant (Resolution and Throughput)
- •Choosing the Solid Angle of the EDS
- •Selecting a Beam Current for an Acceptable Level of System Dead-Time
- •16.3.1 Detector Geometry
- •16.3.2 Process Time
- •16.3.3 Optimal Working Distance
- •16.3.4 Detector Orientation
- •16.3.5 Count Rate Linearity
- •16.3.6 Energy Calibration Linearity
- •16.3.7 Other Items
- •16.3.8 Setting Up a Quality Control Program
- •Using the QC Tools Within DTSA-II
- •Creating a QC Project
- •Linearity of Output Count Rate with Live-Time Dose
- •Resolution and Peak Position Stability with Count Rate
- •Solid Angle for Low X-ray Flux
- •Maximizing Throughput at Moderate Resolution
- •References
- •17: DTSA-II EDS Software
- •17.1 Getting Started With NIST DTSA-II
- •17.1.1 Motivation
- •17.1.2 Platform
- •17.1.3 Overview
- •17.1.4 Design
- •Simulation
- •Quantification
- •Experiment Design
- •Modeled Detectors (. Fig. 17.1)
- •Window Type (. Fig. 17.2)
- •The Optimal Working Distance (. Figs. 17.3 and 17.4)
- •Elevation Angle
- •Sample-to-Detector Distance
- •Detector Area
- •Crystal Thickness
- •Number of Channels, Energy Scale, and Zero Offset
- •Resolution at Mn Kα (Approximate)
- •Azimuthal Angle
- •Gold Layer, Aluminum Layer, Nickel Layer
- •Dead Layer
- •Zero Strobe Discriminator (. Figs. 17.7 and 17.8)
- •Material Editor Dialog (. Figs. 17.9, 17.10, 17.11, 17.12, 17.13, and 17.14)
- •17.2.1 Introduction
- •17.2.2 Monte Carlo Simulation
- •17.2.4 Optional Tables
- •References
- •18: Qualitative Elemental Analysis by Energy Dispersive X-Ray Spectrometry
- •18.1 Quality Assurance Issues for Qualitative Analysis: EDS Calibration
- •18.2 Principles of Qualitative EDS Analysis
- •Exciting Characteristic X-Rays
- •Fluorescence Yield
- •X-ray Absorption
- •Si Escape Peak
- •Coincidence Peaks
- •18.3 Performing Manual Qualitative Analysis
- •Beam Energy
- •Choosing the EDS Resolution (Detector Time Constant)
- •Obtaining Adequate Counts
- •18.4.1 Employ the Available Software Tools
- •18.4.3 Lower Photon Energy Region
- •18.4.5 Checking Your Work
- •18.5 A Worked Example of Manual Peak Identification
- •References
- •19.1 What Is a k-ratio?
- •19.3 Sets of k-ratios
- •19.5 The Analytical Total
- •19.6 Normalization
- •19.7.1 Oxygen by Assumed Stoichiometry
- •19.7.3 Element by Difference
- •19.8 Ways of Reporting Composition
- •19.8.1 Mass Fraction
- •19.8.2 Atomic Fraction
- •19.8.3 Stoichiometry
- •19.8.4 Oxide Fractions
- •Example Calculations
- •19.9 The Accuracy of Quantitative Electron-Excited X-ray Microanalysis
- •19.9.1 Standards-Based k-ratio Protocol
- •19.9.2 “Standardless Analysis”
- •19.10 Appendix
- •19.10.1 The Need for Matrix Corrections To Achieve Quantitative Analysis
- •19.10.2 The Physical Origin of Matrix Effects
- •19.10.3 ZAF Factors in Microanalysis
- •X-ray Generation With Depth, φ(ρz)
- •X-ray Absorption Effect, A
- •X-ray Fluorescence, F
- •References
- •20.2 Instrumentation Requirements
- •20.2.1 Choosing the EDS Parameters
- •EDS Spectrum Channel Energy Width and Spectrum Energy Span
- •EDS Time Constant (Resolution and Throughput)
- •EDS Calibration
- •EDS Solid Angle
- •20.2.2 Choosing the Beam Energy, E0
- •20.2.3 Measuring the Beam Current
- •20.2.4 Choosing the Beam Current
- •Optimizing Analysis Strategy
- •20.3.4 Ba-Ti Interference in BaTiSi3O9
- •20.4 The Need for an Iterative Qualitative and Quantitative Analysis Strategy
- •20.4.2 Analysis of a Stainless Steel
- •20.5 Is the Specimen Homogeneous?
- •20.6 Beam-Sensitive Specimens
- •20.6.1 Alkali Element Migration
- •20.6.2 Materials Subject to Mass Loss During Electron Bombardment—the Marshall-Hall Method
- •Thin Section Analysis
- •Bulk Biological and Organic Specimens
- •References
- •21: Trace Analysis by SEM/EDS
- •21.1 Limits of Detection for SEM/EDS Microanalysis
- •21.2.1 Estimating CDL from a Trace or Minor Constituent from Measuring a Known Standard
- •21.2.2 Estimating CDL After Determination of a Minor or Trace Constituent with Severe Peak Interference from a Major Constituent
- •21.3 Measurements of Trace Constituents by Electron-Excited Energy Dispersive X-ray Spectrometry
- •The Inevitable Physics of Remote Excitation Within the Specimen: Secondary Fluorescence Beyond the Electron Interaction Volume
- •Simulation of Long-Range Secondary X-ray Fluorescence
- •NIST DTSA II Simulation: Vertical Interface Between Two Regions of Different Composition in a Flat Bulk Target
- •NIST DTSA II Simulation: Cubic Particle Embedded in a Bulk Matrix
- •21.5 Summary
- •References
- •22.1.2 Low Beam Energy Analysis Range
- •22.2 Advantage of Low Beam Energy X-Ray Microanalysis
- •22.2.1 Improved Spatial Resolution
- •22.3 Challenges and Limitations of Low Beam Energy X-Ray Microanalysis
- •22.3.1 Reduced Access to Elements
- •22.3.3 At Low Beam Energy, Almost Everything Is Found To Be Layered
- •Analysis of Surface Contamination
- •References
- •23: Analysis of Specimens with Special Geometry: Irregular Bulk Objects and Particles
- •23.2.1 No Chemical Etching
- •23.3 Consequences of Attempting Analysis of Bulk Materials With Rough Surfaces
- •23.4.1 The Raw Analytical Total
- •23.4.2 The Shape of the EDS Spectrum
- •23.5 Best Practices for Analysis of Rough Bulk Samples
- •23.6 Particle Analysis
- •Particle Sample Preparation: Bulk Substrate
- •The Importance of Beam Placement
- •Overscanning
- •“Particle Mass Effect”
- •“Particle Absorption Effect”
- •The Analytical Total Reveals the Impact of Particle Effects
- •Does Overscanning Help?
- •23.6.6 Peak-to-Background (P/B) Method
- •Specimen Geometry Severely Affects the k-ratio, but Not the P/B
- •Using the P/B Correspondence
- •23.7 Summary
- •References
- •24: Compositional Mapping
- •24.2 X-Ray Spectrum Imaging
- •24.2.1 Utilizing XSI Datacubes
- •24.2.2 Derived Spectra
- •SUM Spectrum
- •MAXIMUM PIXEL Spectrum
- •24.3 Quantitative Compositional Mapping
- •24.4 Strategy for XSI Elemental Mapping Data Collection
- •24.4.1 Choosing the EDS Dead-Time
- •24.4.2 Choosing the Pixel Density
- •24.4.3 Choosing the Pixel Dwell Time
- •“Flash Mapping”
- •High Count Mapping
- •References
- •25.1 Gas Scattering Effects in the VPSEM
- •25.1.1 Why Doesn’t the EDS Collimator Exclude the Remote Skirt X-Rays?
- •25.2 What Can Be Done To Minimize gas Scattering in VPSEM?
- •25.2.2 Favorable Sample Characteristics
- •Particle Analysis
- •25.2.3 Unfavorable Sample Characteristics
- •References
- •26.1 Instrumentation
- •26.1.2 EDS Detector
- •26.1.3 Probe Current Measurement Device
- •Direct Measurement: Using a Faraday Cup and Picoammeter
- •A Faraday Cup
- •Electrically Isolated Stage
- •Indirect Measurement: Using a Calibration Spectrum
- •26.1.4 Conductive Coating
- •26.2 Sample Preparation
- •26.2.1 Standard Materials
- •26.2.2 Peak Reference Materials
- •26.3 Initial Set-Up
- •26.3.1 Calibrating the EDS Detector
- •Selecting a Pulse Process Time Constant
- •Energy Calibration
- •Quality Control
- •Sample Orientation
- •Detector Position
- •Probe Current
- •26.4 Collecting Data
- •26.4.1 Exploratory Spectrum
- •26.4.2 Experiment Optimization
- •26.4.3 Selecting Standards
- •26.4.4 Reference Spectra
- •26.4.5 Collecting Standards
- •26.4.6 Collecting Peak-Fitting References
- •26.5 Data Analysis
- •26.5.2 Quantification
- •26.6 Quality Check
- •Reference
- •27.2 Case Study: Aluminum Wire Failures in Residential Wiring
- •References
- •28: Cathodoluminescence
- •28.1 Origin
- •28.2 Measuring Cathodoluminescence
- •28.3 Applications of CL
- •28.3.1 Geology
- •Carbonado Diamond
- •Ancient Impact Zircons
- •28.3.2 Materials Science
- •Semiconductors
- •Lead-Acid Battery Plate Reactions
- •28.3.3 Organic Compounds
- •References
- •29.1.1 Single Crystals
- •29.1.2 Polycrystalline Materials
- •29.1.3 Conditions for Detecting Electron Channeling Contrast
- •Specimen Preparation
- •Instrument Conditions
- •29.2.1 Origin of EBSD Patterns
- •29.2.2 Cameras for EBSD Pattern Detection
- •29.2.3 EBSD Spatial Resolution
- •29.2.5 Steps in Typical EBSD Measurements
- •Sample Preparation for EBSD
- •Align Sample in the SEM
- •Check for EBSD Patterns
- •Adjust SEM and Select EBSD Map Parameters
- •Run the Automated Map
- •29.2.6 Display of the Acquired Data
- •29.2.7 Other Map Components
- •29.2.10 Application Example
- •Application of EBSD To Understand Meteorite Formation
- •29.2.11 Summary
- •Specimen Considerations
- •EBSD Detector
- •Selection of Candidate Crystallographic Phases
- •Microscope Operating Conditions and Pattern Optimization
- •Selection of EBSD Acquisition Parameters
- •Collect the Orientation Map
- •References
- •30.1 Introduction
- •30.2 Ion–Solid Interactions
- •30.3 Focused Ion Beam Systems
- •30.5 Preparation of Samples for SEM
- •30.5.1 Cross-Section Preparation
- •30.5.2 FIB Sample Preparation for 3D Techniques and Imaging
- •30.6 Summary
- •References
- •31: Ion Beam Microscopy
- •31.1 What Is So Useful About Ions?
- •31.2 Generating Ion Beams
- •31.3 Signal Generation in the HIM
- •31.5 Patterning with Ion Beams
- •31.7 Chemical Microanalysis with Ion Beams
- •References
- •Appendix
- •A Database of Electron–Solid Interactions
- •A Database of Electron–Solid Interactions
- •Introduction
- •Backscattered Electrons
- •Secondary Yields
- •Stopping Powers
- •X-ray Ionization Cross Sections
- •Conclusions
- •References
- •Index
- •Reference List
- •Index
547 AA–EP
Index
A
Aluminum wire failures 482–483 Anaglyph stereo pair presentation 218 Ancient impact zircons 493
Angular distribution, backscattered electrons 24–25
Auger electron emission 48 Auger electron spectroscopy 37 Avogadro’s number 4
B
Backscattered electrons (BSEs) 2, 549, vii
–– angular distribution 24–25
–– atomic number contrast 19–20
–– energy distribution 29–30
–– η vs. atomic number, Z 17–19
–– η vs. surface tilt, θ 21–23
–– numerical measure 16
–– origin 16
–– spatial distribution 25–29
–– topographic contrast—number effects 23–24 Backscattered electron yield data 584–563 Beam convergence angle, α 80–81
Beam current 79–80, 214 Beam current density 80 Beam diameter 79
Beam energy 78–79, 297, 330. See also Low beam energy SEM; Low beam energy X-ray microanalysis
–– compositional contrast with backscattered electrons 213
–– high resolution SEM imaging 214
–– vs. secondary electrons (SE) yield 40
–– topographic contrast
–– with backscattered electrons 213
–– with secondary electrons 213 Beam placement 414
Beam solid angle 81–83 Bethe expression 2, 3 Brightness equation 83
BSEs. See Backscattered electrons (BSEs)
Bulk biological and organic specimens 355–356 Bulk specimens
–– origins of geometric effects 396–397
–– particle analysis
–– optimum spectra 410–414
–– quantitative analysis of particles 415–420
–– uncertainty in 420–422
–– X-ray measurements 408–410
–– X-ray spectrum imaging (XSI) 414–415
–– with rough surfaces 399–401
C
Carbonado diamond 492–493 CASINO simulation 5–7 Cathodoluminescence (CL)
–– applications of
–– geology 492–493
–– materials science 493–495
–– organic compounds 495–497
–– collection of 491
–– detection of 491–492
–– measurement 491
–– origin 490–491 Compositional mapping
–– limitations of 427–429
–– MAXIMUM PIXEL spectrum 433–435
–– quantitative compositional mapping 436–441
–– SUM spectrum 431–433
–– total intensity region-of-interest mapping 426–427
–– X-ray spectrum imaging (XSI) 429–431
–– EDS dead-time 441–443
–– elemental mapping data collection 441–450
–– flash mapping 444–445
–– high count mapping 445–450
–– pixel density 443–444
–– pixel dwell time 444–450 Concentration limit of detection (CDL)
–– reference value 362–363
–– trace or minor constituent 359–362 Continuous energy loss approximation 2
D
A Database of Electron-Solid Interactions (Joy) 37 Detective quantum efficiency (DQE) 101–103 DTSA-II EDS software
–– design 255
–– fundamental concepts 256–264
–– GUI 267–279
–– Monte Carlo simulation 267
–– motivation 254
–– optional tables 279–283
–– overview 254–255
–– platform 254
–– simulation 264–267
–– three-leg stool
–– experiment design 256
–– quantification 255
–– simulation 255
E
EDS. See Energy dispersive X-ray spectrometry (EDS) Electron backscattering diffraction (EBSD) xiii
–– align sample 510–511
–– check for EBSD patterns 511–512
–– checklist
–– acquisition parameters 522
–– candidate crystallographic phases 522
–– EBSD detector 521–522
–– microscope operating conditions 522
–– orientation map 522–523
–– pattern optimization 522
–– specimen considerations 521
–– index patterns 508–509
–– map parameters 512
–– measurements 509–510
–– origin of 505–506
–– pattern detection 506–507
–– sample preparation for 510
–– spatial resolution 507–508
Electron beam, interaction volume change
–– elastic scattering 3–4
–– elastic scattering cross section 4
–– inelastic scattering 2–3
–– Monte Carlo calculations
–– beam electron interaction volume 7–8
–– composition 8–9
–– electron interaction volume 7
–– electron trajectory simulation 4–5
–– incident beam energy 9–10
–– Monte Carlo simulation (CASINO simulation) 5–7
–– size of the interaction volume 11–12
–– specimen tilt 10–11
–– specimen atoms 2
Electron-excited X-ray microanalysis, geometric effects 398
Electron interaction volume 363–364 Electron optical brightness, β 83 Electron optical parameters
–– astigmatism 85–87
–– beam convergence angle, α 80–81
–– beam current 79–80
–– beam current density 80
–– beam diameter 79
–– beam energy 78–79
–– beam solid angle 81–83
–– electron optical brightness, β 83
–– focus 83–87
Electron probe microanalyzers (EPMAs) 91 Electron–solid interactions, database of 548 Energy dispersive X-ray microanalysis checklist
–– analytical procedure 477
–– calibrating the EDS detector
–– detector position 473–474
–– energy calibration 472–473
–– probe current 474
–– pulse process time constant 472
–– quality control 473
–– sample orientation 473
–– working distance/pecimen-to-EDS distance 473
–– collecting data
–– collecting peak-fitting references 475
–– collecting spectra from unknown 475–476
–– collecting standards 475
–– experiment optimization 474
–– exploratory spectrum 474
–– reference spectra 475
–– selecting standards 474
–– data analysis 476
–– instrumentation
–– conductive coater 471
–– EDS detector 470–471
–– SEM 470
–– peak reference materials 472
–– quality check 476–477
–– quantification 476
–– results 477
–– sample preparation 471
–– standard materials 472
548\ Index
Energy dispersive X-ray spectrometry (EDS) xi
–– adequate counts 297–298
–– beam current 330–332
–– beam energy 297, 330
–– coincidence peaks 294–295
–– detection process
–– coincidence peaks 231–233
–– peak broadening 228–231
–– Si absorption edge 233–234
–– Si-escape peak 231
–– Si internal fluorescence peak 233–234
–– detector dead-time 297
–– detector time constant 297
–– electron-excited EDS operation
–– beam current 235–237
–– channel width and number 235
–– EDS time constant 234
–– solid angle 235
–– exciting characteristic X-rays 287–288
–– fluorescence yield 288
–– lower photon energy region 300–301
–– manual peak identification 301–305
–– manual qualitative analysis 296–297
–– minor and trace constituents 301
–– parameters
–– calibration 330
–– solid angle 330
–– spectrum channel energy width 328–329
–– spectrum energy span 328–329
–– time constant 329–330
–– pathological electron scattering
–– trace analysis artifacts 364–369
–– peaks, identifying 299
–– principles, qualitative EDS analysis 287
–– QC project 246–249
–– QC tools within DTSA-II 246
–– quality assurance issues 286
–– quality measurement environment
–– detector geometry 237–240
–– detector orientation 240–245
–– energy calibration linearity 245
–– optimal working distance 240
–– process time 240
–– Si escape peak 293
–– silicon drift detector (SDD)
–– low X-ray flux 250–251
–– moderate resolution 251
–– output count rate with live-time dose 249–250
–– resolution and peak position stability 250
–– software tools 298–299
–– trace level measurement 363–364
–– X-ray absorption 288–289
–– X-ray energy database 289–292 Energy distribution, backscattered
electrons 29–30
EPMAs. See Electron probe microanalyzers (EPMAs)
Everhart–Thornley detector 99–100, 128, 129–130, 213, 215
F
Fiji 204–206
Focused ion beams (FIB), xiii
–– cross-section preparation 530–532
–– focused ion beam systems 527–528
–– imaging with ions 528–529
–– ion–solid interactions 526–527
–– SEM, sample preparation 530
–– 3D techniques and imaging 532–536
G
Geometric factors
–– bulk specimens 396–397
–– electron-excited X-ray microanalysis 398
–– useful indicators of
–– EDS spectrum 404–406
–– raw analytical total 401–404
–– rough bulk samples 406–408 Graphical user interface (GUI) 90, 204
H
Hard-facing alloy bearing surface 480–482 Helium ion microscope (HIM) xiv
High resolution imaging
–– achieving visibility 178
–– beam footprint 162–164
–– delocalized signals 162–164
–– instrumentation considerations 162
–– pathological specimen and instrumentation behavior
–– contamination 179
–– instabilities 179
–– pathological specimen behavior 178–179
–– pixel size 162–164
–– secondary electron contrast 164–165
–– beam range 167
–– bright edge effect 167
–– critical dimension metrology 167–169
–– isolated edges 165–167
–– with secondary electrons 169–171
–– beam energy strategies 171–173
–– low loss BSEs 176–178
–– SE1 signal 173–176
–– SEM 162
HIM. See Helium ion microscope (HIM)
I
Image defects
–– charging
–– control charging artifacts 153–155
–– define 148–149
–– in SEM images 149–152
–– contamination 157–158
–– image defocusing (blurring) 113–117
–– Moiré effects 158–159
–– projection distortion (foreshortening) 111–113
–– radiation damage 155–157 Image formation
–– calibrating the image 107–109
–– image defects
–– image defocusing (blurring) 113–117
–– projection distortion (foreshortening) 111–113
–– image dimensions 107
–– ImageJ-Fiji, calibrated structure in 109–110
–– ImageJ-Fiji, routine linear measurements with 110
–– magnification 107
–– scale bars 107
–– by scanning action 106–107
–– stereomicroscopy
–– qualitative stereomicroscopy 118–121
–– quantitative stereomicroscopy 121–124
–– surface measurement 117–118 ImageJ-Fiji
–– calibrated structure in 109–110
–– routine linear measurements with 110 ImageJ universe 204
Imaging crystalline materials
–– acquired data 512–513
–– application 518–521
–– cleaning EBSD data 516–517
–– electron channeling contrast
–– electron backscattering diffraction (EBSD) 504–512
–– instrument conditions 504
–– specimen preparation 504
–– map components 513–516
–– polycrystalline materials 502–503
–– single crystals 500–502
–– transmission Kikuchi diffraction (TKD) 517–518
Incident beam energy 9–10 Ink-Jet printer deposits 224–226
International Union of Pure and Applied Chemistry (IUPAC) 51
Ion beam microscopy
–– chemical microanalysis 546
–– generating ion beams 541–542
–– helium ion microscope (HIM)
–– current generation and data collection 543–545
–– operating the 545–546
–– patterning with 545
–– signal generation in 542–543
–– patterning with ion 545
–– usefulness 538–541
J
Java Runtime Environment (JRE) 205
K
Kanaya–Okayama range 11–12, 60, 182 k-ratio
–– analytical total 310
–– converting sets of 310
–– define 308–309
–– element by difference 311
–– estimate CZ 310–311
–– matrix corrections 316–317
–– matrix effects, physical origin of 317
–– normalization 310
–– oxygen by assumed stoichiometry 311
–– quantitative electron-excited X-ray microanalysis
–– standardless analysis 314–316
–– standards-based k-ratio protocol 313–314
–– reporting composition
–– atomic fraction 312
–– mass fraction 311–312
–– oxide fractions 312–313
–– stoichiometry 312
Index
–– sets of 309
–– uncertainties in 309
–– waters of crystallization 311
–– ZAF factors, microanalysis 317–324 k-ratio/matrix correction protocol
–– alkali element migration 349–353
–– Ba-Ti interference 337–338
–– beam-sensitive specimens 349
–– complex metal alloy, IN100 340, 341
–– with DTSA II 333–334
–– Hall method 353–356
–– instrumentation requirements 328
–– iterative qualitative and quantitative analysis strategy 338–339
–– major constituents 334–336
–– repeated qualitative–quantitative analysis sequences 343–347
–– specimen and standards 328
–– specimen homogeneous 347–349
–– stainless steel 340–343
L
Landing energy 79
Lead-acid battery plate reactions 494–495 Light-optical analogy, Everhart–Thornley
(positive bias) detector 131–133 Long-range secondary X-ray fluorescence 364 Low beam energy SEM
–– backscattered electron signal characteristics 182–185
–– constituent 182
–– extremely low beam energy imaging 187
–– high depth resolution SEM 185–186
–– for high lateral resolution SEM 185
–– Kanaya–Okayama range 182
–– secondary electron 182–185
Low beam energy X-ray microanalysis
–– advantage of
–– improved spatial resolution 381–382
–– low atomic number elements 382–385
–– reduced matrix absorption correction 382
–– challenges and limitations
–– reduced access to elements 385–387
–– surface layers 388–393
–– vertical heterogeneity 387–388
–– constitutes 376–380
–– low beam energy analysis range 381
–– peak selection strategy 380–381
M
Magnification vs. pixel dimension 163 Manganese nodule 483–488 Modeled detectors
–– aluminum layer 261–263
–– azimuthal angle 261
–– crystal thickness 261
–– dead layer 263
–– detector area 261
–– elevation angle 261
–– energy scale 261
–– gold layer 261–263
–– material editor dialog 264–266
–– Mn Kα, resolution at 261
–– nickel layer 261–263
–– number of channels 261
–– optimal working distance 259–260
–– panel containing properties 256, 257
–– sample-to-detector distance 261
–– window type 258–259
–– zero offset 261
–– zero strobe discriminator 263 Monte Carlo calculations
–– beam electron interaction volume 7–8
–– composition 8–9
–– electron interaction volume 7
–– electron trajectory simulation 4–5
–– incident beam energy 9–10
–– Monte Carlo simulation (CASINO simulation) 5–7
–– size of the interaction volume 11–12
–– specimen tilt 10–11
Monte Carlo electron trajectory simulation 4–5
Monte Carlo simulation 5–7
–– DTSA-II EDS software 267
–– X-ray generation 62–63
N
National Institutes of Health (NIH) 204 NIST DTSA II simulation 364
O
Open Microscopy Environment
(OME) 204
Overscanning 414
P
Particle absorption effect 415–420 Particle analysis
–– optimum spectra 410–414
–– quantitative analysis of particles 415–420
–– uncertainty in 420–422
–– X-ray measurements 408–410
–– X-ray spectrum imaging (XSI) 414–415 Particle mass effect 415
Particle sample preparation 413–414 Plugins 206–209
Q
Quantitative compositional mapping, 436–441
R
Robust light-optical analogy 131
S
Scanning electron microscope (SEM)
–– compositional microstructure ix
–– crystal structure xii–xiii
–– dual-beam platforms, combined electron and ion beams xiii–xiv
–– electron-optical parameters vii–ix
–– elemental composition x–xii
–– specimen property information ix–x
549 AE–SP
–– three-dimensional structure ix–x
–– topography ix, x
Scanning electron microscope (SEM) image interpretation
–– compositional microstructure
–– atomic number contrast, calculation 127–128
–– atomic number contrast with backscattered electrons 126–127
–– BSE atomic number contrast with Everhart–Thornley detector 128
–– information in 126
–– specimen topography 128–129
–– Everhart–Thornley detector 129–130
–– light-optical analogy 130–133
–– with semiconductor BSE detector 133–136
Scanning electron microscope (SEM) images
–– Rose visibility criterion 139
–– signal quality 138–145
–– signal-to-noise ratio 138
Scanning electron microscope (SEM) imaging checklist
–– beam current
–– high resolution imaging 214
–– low contrast features 214
–– beam energy
–– compositional contrast with backscattered electrons 213
–– high resolution SEM imaging 214
–– topographic contrast with backscattered electrons 213
–– topographic contrast with secondary electrons 213
–– electron detector
–– backscattered electron detectors 213
–– Everhart–Thornley detector 213
–– electron signals available
–– backscattered electrons 212
–– beam electron range 212
–– secondary electrons (SEs) 212–213
–– image interpretation
–– annular BSE detector 215
–– contrast encoding 215
–– direction of illumination 214
–– Everhart–Thornley detector 215
–– observer’s point of view 214
–– semiconductor BSE detector 215
–– image presentation
–– live display adjustments 214
–– post-collection processing 214
–– specimen considerations 212
–– VPSEM 215
Scanning electron microscope (SEM) instrumentation
–– detective quantum efficiency (DQE) 101–103
–– detector characteristics
–– bandwidth 97
–– electron detectors, angular measures for 96–97
–– energy response 97
–– electron beam parameters 78
–– electron detectors
–– abundance 95
–– angular distribution 95
–– backscattered electrons 97–99
–– kinetic energy response 95–96
550\ Index
Scanning electron microscope (SEM) instrumentation (cont.)
–– electron optical parameters
–– astigmatism 85–87
–– beam convergence angle, α 80–81
–– beam current 79–80
–– beam current density 80
–– beam diameter 79
–– beam energy 78–79
–– beam solid angle 81–83
–– electron optical brightness, β 83
–– focus 83–87
–– imaging modes 87–88
–– high-current mode 90–92
–– high mode 88–90
–– low-voltage mode 94–95
–– resolution mode 93–94
–– secondary electron detectors
–– Everhart–Thornley detector 99–100
–– through-the-lens (TTL) electron detectors 100
–– specimen current 100–101
Scanning electron microscopist and X-ray microanalyst (SEMXM) 204
Scanning transmission electron microscope (STEM) image 175–176
Secondary electron energy spectrum 34–35
Secondary electrons (SE) 2, 549, vii
–– angular distribution of 39–40
–– energy distribution 34–35
–– escape depth 35–37
–– origin 34
–– spatial characteristics of 40–43
–– yield vs. atomic number 37–38
–– yield vs. beam energy 40
–– yield vs. specimen tilt 38–39 Secondary electron yield data 553–584 Secondary yields 549
SEM/EDS
–– limits of detection for 358–359
–– remote excitation sources 370–373 Semiconductors 493–494
Shallow surface relief 222–224 Silicon drift detector (SDD)
–– low X-ray flux 250–251
–– moderate resolution 251
–– output count rate with live-time dose 249–250
–– resolution and peak position stability 250 Single pixel measurement 222
Spatial distribution, backscattered electrons
–– depth distribution 26–28
–– Monte Carlo simulation 25
–– radial distribution 28–29 Spectrum imaging (SI) xi Stopping powers 549–550
T
Thin section analysis 353–355 3D viewer plugin tool 218, 219
Transmission Kikuchi diffraction (TKD) 517–518
V
Variable pressure scanning electron microscopy (VPSEM) vii
–– contrast in 200–201
–– conventional SEM high vacuum environment
–– beam integrity 190
–– difference from 190–191
–– Everhart–Thornley secondary electron detector 190
–– minimizing contamination 190
–– stable electron source operation 190
–– EDS collimator 456–458
–– elevated pressure microscopy, detectors for
–– backscattered electrons, passive scintillator detector 198–199
–– secondary electrons, gas amplification detector 199–200
–– favorable sample characteristics 461–462
–– gas scattering effects in 452–456, 460–461
–– scanning electron microscopy at elevated pressures
–– focused electron beam 193–196
–– image resolution 196–198
–– specimen charging 191–192
–– water environment of specimen 192–193
–– solve practical problems 461
–– unfavorable sample characteristics 462–468
–– X-ray spectrometry 458–460
X
X-ray ionization cross sections 550 X-rays
–– characteristic of
–– families 50–51
–– fluorescence yield 48–50
–– intensity 53–56
–– isolated atoms 53–54
–– nomenclature 51
–– origin 46–47
–– thick, solid specimens 55–56
–– thin foils 54–55
–– weights of lines 51–53
–– continuum (bremsstrahlung) 56–57
–– absorption 65–75
–– continuum intensity 57–58
–– depth distribution function,Φ(ρz) 64–65
–– electron-excited X-ray spectrum 58–59
–– fluorescence 75–76
–– Monte Carlo simulation 62–63
–– range of 60–62
X-ray spectrum imaging (XSI)
–– compositional mapping 429–431
–– EDS dead-time 441–443
–– elemental mapping data collection 441–450
–– flash mapping 444–445
–– high count mapping 445–450
–– pixel density 443–444
–– pixel dwell time 444–450
–– particle analysis 414–415