- •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
399 |
23 |
23.6 · Particle Analysis
a
EDS
b
c
. Fig. 23.22 Particles deposited on a thin (~20-nm) carbon film supported on a copper grid shown at various magnifications. a Nominal 200 X, field width 351 by 263 micrometers; b nominal 1 kX, field width 70 by 53 micrometers; c nominal 5 kX, field width 14 by 11 micrometers
The Importance of Beam Placement
The placement of the beam on the particle relative to the EDS detector position can have a strong effect on the measured spectrum. For particles of intermediate size where the interaction volume is contained within the particle, placing the
. Fig. 23.23 Schematic illustration of the effect of beam placement on a particle on the length of the absorption path to the EDS detector
beam on the side of the particle away from the EDS results in an extended absorption path. The generated X-rays must pass through a large mass of the particle to reach the detector. This effect is illustrated schematically in . Fig. 23.23, where absorption paths for X-rays generated near the maximum penetration of beam electrons in the particle are compared for three beam positions: top center, and at positions directly facing and away from the EDS. Because absorption follows an exponential dependence on path length and becomes increasingly significant for low energy photons below approximately 4 keV, the low energy portion of the spectrum will show the strongest absorption effects. Spectra recorded at the top of a 5-μm-diameter particle and on the side away from the EDS are compared in . Fig. 23.24 demonstrating a factor of two difference in the intensity measured at the
energy of Mg K-L2,3 (1.254 keV). For a beam placed on the curved side of the particle facing the EDS, the absorption
path length is actually reduced relative to the top center, leading to extra emission from the low energy photons, creating
about 30 % excess for Mg K-L2,3, as shown in the comparison of spectra in . Fig. 23.25. . Figure 23.26 shows the impact of
beam placement on the accuracy of quantitative analysis, as discussed below. It is thus critical that the analyst is always aware of the relative position of the EDS in the SEM image when choosing locations to analyze. A reliable way to locate the EDS is to record an X-ray spectrum image and examine selected X-ray intensity maps, as shown in . Fig. 23.27. The general rule that the source of the apparent illumination
\400 Chapter 23 · Analysis of Specimens with Special Geometry: Irregular Bulk Objects and Particles
Counts
100000 |
K411_sphere_beam-top-center_20kV10nA |
K411_sphere_r/2_away_20kV10nA |
10000
1000
100
10 |
|
|
|
|
|
|
|
|
|
|
0.0 |
1.0 |
2.0 |
3.0 |
4.0 |
5.0 |
6.0 |
7.0 |
8.0 |
9.0 |
10.0 |
Photon energy (keV)
Counts
3000 |
|
|
|
|
|
|
|
|
|
K411_sphere_beam-top-center_20kV10nA |
|
||
|
|
|
|
|
|
|
|
|
|
|
|||
|
|
|
|
|
|
|
|
|
|
K411_sphere_r/2_away_20kV10nA |
|
|
|
2500 |
|
|
|
|
|
|
|
|
K411 |
|
|
|
|
|
|
|
|
|
|
|
|
|
15-µm sphere (20 nm C film on Cu grid) |
|
|||
2000 |
|
|
|
|
|
|
|
|
E0 = 20 keV |
|
|
|
|
|
|
|
|
|
|
|
|
|
Beam position: Top Center |
|
|
||
1500 |
|
|
|
|
|
|
|
|
Beam position: R/2, away from EDS |
|
|
||
|
|
|
|
|
|
|
|
|
|
|
|
|
|
1000 |
|
|
|
|
|
|
|
|
|
|
|
|
|
500 |
|
|
|
|
|
|
|
|
|
|
|
|
|
00.0 |
|
|
|
|
|
|
|
|
|
|
|
||
1.0 |
2.0 |
3.0 |
4.0 |
5.0 |
6.0 |
7.0 |
8.0 |
9.0 |
10.0 |
||||
|
|
|
|
|
|
|
Photon energy (keV) |
|
|
|
|
|
|
. Fig. 23.24 Comparison of EDS spectra recorded at the top center and on the side away from the EDS
appears to come from the position of the detector immediately reveals the true EDS position. For this particular particle, the eclipsing effect of the extended absorption path on the backside of the particle is readily apparent, even in the relatively energetic Co K-L2,3 (6.930 keV) intensity map.
Overscanning
“Overscanning” is a strategy by which the beam is continuously scanned over the particle (or rough surface, heterogeneous material, etc.) while the EDS spectrum is being collected. If the magnification control of the SEM is continuously variable, then the size of the scan raster can be adjusted to bracket the particle, minimizing the fraction of the time that the beam spends on the surrounding substrate, as shown in . Fig. 23.28 (yellow box). Alternatively, the scan raster can be adjusted to fill as much of the particle image as possible while remaining within the bounds of the particle, thus avoiding direct beam placement on the substrate, as shown in
. Fig. 23.28 (green box).
23 While useful for gaining qualitative information on the constituents of a particle, overscanning only has utility if the particle (or other target object) is homogeneous. Overscanning discards valuable information on any possible inhomogeneous
structure within the particle. As described below, overscanning is NOT a means by which an “average” composition can be found by quantitative microanalysis.
23.6.3\ X-ray Spectrum Imaging:
Understanding Heterogeneous
Materials
X-ray spectrum imaging (XSI) involves collecting a complete EDS spectrum at every pixel location visited by the scanned beam. When applied to particle analysis, the XSI provides the analyst with an abundance of information which can be recovered by post-collection processing of the XSI datacube. Composition heterogeneity down to the single pixel level can be detected and interpreted. The particle X-ray intensity images shown in . Fig. 23.27a, b were extracted from an XSI, and the localization of Ti and Mo in inclusions is immediately obvious. Solidification dendrites
are outlined in the Ti K-L2,3 map, a feature that is not obvious in any of the other elemental intensity maps. Software
tools enable the analyst to extract spectra that are representative of individual components of the microstructure, such
23.6 · Particle Analysis |
|
|
|
|
|
|
|
|
401 |
|
23 |
|||
|
|
|
|
|
|
|
|
|
|
|
|
|||
|
|
|
|
|
|
|
|
|
|
|
|
|||
|
100000 |
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
K411_sphere_beam-top-center_20kV10nA |
|
||||
|
|
|
|
|
|
|
|
|
|
|
||||
|
|
|
|
|
|
|
|
|
|
K411_sphere_r/2_toward_20kV10nA |
|
|
|
|
|
10000 |
|
|
|
|
|
|
|
|
|
|
|
|
|
Counts |
1000 |
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
100 |
|
|
|
|
|
|
|
|
|
|
|
|
|
|
10 |
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
0.0 |
1.0 |
2.0 |
3.0 |
4.0 |
5.0 |
6.0 |
7.0 |
8.0 |
9.0 |
10.0 |
|||
|
|
|
|
|
|
|
Photon energy (keV) |
|
|
|
|
|
|
|
Counts
|
|
|
|
|
|
|
|
|
|
|
K411_sphere_beam-top-center_20kV10nA |
|
|||
6000 |
|
|
|
|
|
|
|
|
|
|
K411_sphere_r/2_toward_20kV10nA |
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
5000 |
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
K411 |
|
|
|
|
|
||||
|
|
|
|
|
|
|
|
|
|
|
|
|
|
||
4000 |
|
|
|
|
|
|
|
|
15-µm sphere (20 nm C film on Cu grid) |
|
|
||||
|
|
|
|
|
|
|
|
E0 |
= 20 keV |
|
|
|
|
||
|
|
|
|
|
|
|
|
|
|
|
|
|
|||
3000 |
|
|
|
|
|
|
|
|
Beam position: Top Center |
|
|
|
|
||
|
|
|
|
|
|
|
|
Beam position: R/2, toward EDS |
|
|
|
||||
|
|
|
|
|
|
|
|
|
|
|
|
||||
2000 |
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
100 |
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
00.0 |
|
|
|
|
|
|
|
|
|
|
|
|
|
||
1.0 |
2.0 |
3.0 |
4.0 |
5.0 |
6.0 |
|
7.0 |
8.0 |
9.0 |
10.0 |
|||||
|
|
|
|
|
|
|
Photon energy (keV) |
|
|
|
|
|
|
|
|
. Fig. 23.25 Comparison of EDS spectra recorded at the top center and on the side facing the EDS
. Fig. 23.26 Quantitative analysis performed at the static beam locations indicated; relative errors observed for the normalized concentrations (oxygen calculated by stoichiometry)
EDS
Location |
Mg rel err % |
Si rel err % |
Ca rel err % |
Fe rel err % |
|
|
R/2 toward |
29 % |
6 % |
-19 % |
-24 % |
|
|
Top Center |
9 % |
3 % |
-5 % |
-8 % |
5 mm |
|
R/2 away |
-27 % |
-8 % |
27 % |
36 % |
||
|
||||||
|
|
|
|
|
|
\402 Chapter 23 · Analysis of Specimens with Special Geometry: Irregular Bulk Objects and Particles
BSE |
Al |
|
50 µm |
|
Cr |
EDS |
Co |
|
a
Mo |
Ti |
Ni |
EDS |
Mo Ti Ni |
|
||
|
|
|
23 |
b |
50 µm |
|
|
|
. Fig. 23.27 a SEM BSE image and X-ray intensity maps for Al K-L2,3, Cr K-L2,3, and Co K-L2,3. Note the shadowing effect of the particle thickness causing attenuation of X-ray intensity. b X-ray intensity maps for
Mo L3-M4,5, and Ni K-L2,3, and a color overlay with Mo L3-M4,5 = red, Ti K-L2,3 = green, and Ni K-L2,3 = blue. Note the localization of Ti and Mo in inclusions, and the solidification dendrites outlined by Ti