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