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ENCYCLOPEDIA OF MATERIALS CHARACTERIZATION C. Richard Brundle Charles A. Evans, Jr. Shaun Wilson a MAT E R I A LS CHARACTER SERIES SURFACES, INTERFACES, THIN FILMS + ENCYCLOPEDIA OF MATERIALS CHARACTERIZATION MATERIALS CHARACTERIZATION SERIES Surfaces, Interfaces, Thin Films Series Editors: C. Richard Brundle and Charles A. Evans, Jr. Series Titles Encyclopedia of Materiah Characterization, C. Richard Brundle, Characterization of Mekth and Alloys, Paul. H. Holloway and P. N. Characterization of Ceramics, Ronald E. Loehman Characterimtion of Pobmers, Ned J. Chou, Stephen P. Kowalczyk, Characterization in Silicon Processing, Yale Strausser Characterization in Compound Semiconductor Processing, Yale Strausser Characterization of Integraed Circuit Packaging Materiah, Thomas M. Moore and Robert G. McKenna Characterization of Cadytic Materiah, Israel E. Wachs Characterization of Composite Materiah, Hatsuo Ishida Characterization of Optical Materiah, Gregory J. Exarhos Characterization of Tribological Materiah, William A. Glaeser Characterization of Organic Thin Films, Abraham Ulman Charles k Evans, Jr., and Shaun Wilson Vaidyanathan Ravi Sard, and Ho-Ming Tong ENCYCLOPEDIA OF MLATERIALS CHARACTERIZATION Surfaces, Interfaces, Thin Films EDITORS C Ricbard Brundle Charles A. Evans, Jr. Sbaun Wihon MANAGING EDITOR Lee E. Fitzpatrick BUTTERWORTH-HEINEMANN Boston London Oxford Singapore Sydney Toronto Wellington MANNING Greenwich This book was acquired, developed, and produced by Manning Publications Co. Copyright Q 1992 by Butxetworch-Heinemann, a division of Reed Publishing CUSA) Inc Au rights rad No parc of this publicarion may be reproduced, scored in a retried system, or transmitted, in any form or by means. electronic, mechanical, photocopying, or orherwise, without prior written permission of the publisher. Recognizing the importance of preserving what has been written, it is the policy of Butterworth-Heinemann and of Manning to have the books they publish printed on acid-free paper, and we exert our best &m to that end. Library of Congress Cataloging-in-Publication Data Brundle, C. R. Encyclopedia of materials characterization: surfaces, interfaces, thin films/C. Richard Brundle, Charles A. Evans, Jr., Sham Wilson. p. un (Materials characterization series) Indudes bibliographical refrrenoa and index. ISBN CL7506-9168-9 1. Surfaces (Tedmoology)-Tes~ I. Evans, Charlak 11. Wilson, Shaun. 111. Title. IV. Series. TA418.7.B73 I992 92-14999 620’.4Pdc20 CIP Butterworth-Heinemann 80 Montvale Avenue Stoneham, MA02180 Manning Publications Co. 3 his Street Greenwich, CT 06830 109 8 7 6 5 4 3 Printed in the Unired States ofAmerica Contents Preface to Series ix Preface x Acronyms Glossary xi Contributors xvi INTRODUCTION AND SUMMARIES 1.0 Introduction I Technique Summaries 7-56 IMAGING TECHNIQUES (MICROSCOPY) 2.0 Introduction 57 2.1 Light Microscopy 60 2.2 Scanning Electron Microscopy, SEM 70 2.3 Scanning Tunneling Microscopy and 2.4 Transmission Electron Microscopy, TEM 99 Scanning Force Microscopy, STM and SFM 85 ELECTRON BEAM INSTRUMENTS 3.0 Introduction 117 3.1 Energy-Dispersive X-Ray Spectroscopy, EDS 120 3.2 Electron Energy-Loss Spectroscopy in the Transmission Electron Microscope, EELS 135 3.3 Cathodoluminescence, CL 149 3.4 Scanning Transmission Electron Microscopy, STEM 161 3.5 Electron Probe X-Ray Microanalysis, EPMA 175 V STRUCTURE DETERMINATION BY DIFFRACTION AND SCATTERING 4.0 Introduction 193 4.1 X-Ray Diffraction, XRD 198 4.2 Extended X-Ray Absorption Fine Structure, EXAFS 214 4.3 Su&ce Extended X-Ray Absorption Fine Structure and Near Edge X-Ray Absorption Fine Structure, SEXAFS/NEXAFS Auger Electron Difiction, XPD and AED 227 4.4 X-Ray Photoelectron and 4.5 Low-Energy Electron Diffraction, LEED 252 4.6 Reflection High-Energy Electron Diffraction, WEED 264 240 ELECTRON EMISSION SPECTROSCOPIES 5.0 Introduction 279 5.1 X-Ray Photoelectron Spectroscopy, XPS 282 5.2 Ultraviolet Photoelectron Spectroscopy, UPS 300 5.3 Auger Electron Spectroscopy, AES 310 5.4 Reflected Electron Energy-loss Spectroscopy, REELS 324 X-RAY EMISION TECHNIQUES 6.0 Introduction 335 6.1 X-Ray Fluorescence, XRF 338 6.2 Total Reflection X-Ray Fluorescence Analysis, TXRF 349 6.3 Particle-Induced X-Ray Emission, PIXE 357 VISIBLE/W EMISSION, REFLECTION, AND ABSORPTION 7.0 Introduction 371 7.1 Photoluminescence, PL 373 7.2 Modulation Spectroscopy 385 7.3 Variable Angle Spectroscopic Ellipsometry, VASE 401 VIBRATIONAL SPECTROSCOPIES AND NMR 8.0 Introduction 413 8.1 Fourier Transform Infrared Spectroscopy, FTIR 416 8.2 RamanSpectroscopy 428 8.3 High-Resolution Electron Energy Loss Spectroscopy, HREELS 4-42 8.4 Solid State Nuclear Magnetic Resonance, NMR 460 vi Contents ION SCATTERING TECHNIQUFS 9.0 Introduction 473 9.1 Rutherford Backscattering Spectrometry, RBS 476 9.2 Elastic Recoil Spectrometry, ERS 488 9.3 Medium-Energy Ion Scattering with Channeling and Blocking, MEIS 502 9.4 Ion scattering Spectroscopy, Iss 514 MASS AND OPTICAL SPECTROSCOPIES 10.0 10.1 10.2 10.3 10.4 10.5 10.6 10.7 10.8 10.9 Introduction 527 Dynamic Secondary Ion Mass Spectrometry, Dynamic SIMS Static Secondary Ion Mass Spectrometry, Static SIMS 549 Surfice Analysis by her Ionization, SAL1 Sputtered Neutral Mass Spectrometry, SNMS Laser Ionization Mass Spectrometry, LIMS Spark Source Mass Spectrometry, SSMS 598 Glow-Discharge Mass Spectrometry, GDMS 609 Inductively Coupled Plasma Mass Spectrometry, ICPMS Inductively Coupled Plasma-Optical Emission Spectroscopy, ICP-OES 633 532 559 586 571 624 NEUTRONANDNUCLEARTECHNIQUES 1'1.0 Introduction 645 1 1 .I Neutron Diffraction 648 11.2 Neutron Reflectivity 660 11.3 Neutron Activation Analysis, NAA 671 11.4 Nuclear Reaction Analysis, NRA 680 PHYSICAL AND MAGNETIC PROPERTIES 12.0 Introduction 695 12.1 Surface Roughness: Measurement, Formation by Sputtering, Impact on Depth Profiling 698 12.2 Optical Scatterometry 711 12.3 Magneto-optic Kerr Rotation, MOJSE 723 12.4 Physical and Chemical Adsorption Measurement of Solid Surface Areas 736 Contents vii [...]... Electron Diffraction Scanning Reflection Electron Microscopy SAL1 PISIMS MPNRPI MRRPI RPI MPI SPI SINS SARIS TOFMS SurficeAnalysis by h e r Ionization Post-Ionization Secondary Ion Mass Spectrometry Multi-Photon Nonresonant Post Ionization Multiphoton Resonant Post Ionization Resonant Post Ionization Multi-Photon Ionization Single-Photon Ionization Sputter-Initiated Resonance Ionization Spectroscopy... Ultraviolet Photoelectron Spectroscopy Ultraviolet Photoemission Spectroscopy Molecular Photoelectron Spectroscopy VASE VariableAngle SpectroscopicEllipsometry WDS WDX Wavelength Dispersive &-Ray) Spectroscopy Wavelength Dispersive X-Ray Spectroscopy XAS X-Ray Absorption Spectroscopy XPS X-Ray Photoelectron Spectroscopy X-Ray Photoemission Spectroscopy Electron Spectroscopyfor Chemical Analysis X-Ray Photoelectron... by Resonant Ionization Spectroscopy Time-of-Flight Mass Spectrometer SAM See AES SEM ScanningElectron Microscopy ScanningElectron Microprobe Secondary Electron Miscroscopy SecondaryElectron Backscattered Electron Secondary Electron Microscopywith PolarizationAnalysis Scanning Force Microscopy Scanning Force Microscope RBS SE BSE SEMPA SFM AFM SPM Atomic Force Microscopy Scanning Probe Microscopy SIMS... subject of individual articles in this volume AAS AA VPD-AAS GFAA FAA AES Auger SAM SAM AED ADAM K.E CMA Atomic Absorption Spectroscopy Atomic Absorption Vapor Phase Decomposition-AtomicAbsorption Spectroscopy Graphite Furnace Atomic Absorption Flame Atomic Absorption Auger Electron Spectroscopy Auger Electron Spectroscopy Scanning Auger Microscopy Scanning Auger Microprobe Auger Electron Diffraction Angular... Bevolo Ames Laboratory, Iowa State University Ames, IA Reflected Electron Energy-Loss Spectro~copy J B Bindell AT&T Bell Laboratories Allentown, PA Scanning Electron Microscopy Filippo Radicati di Brozolo Charles Evans &Associates Redwood City, CA Laser Ionizarion Mass Spectrometry C R Brundle X-Ray Photoelectron Spectroscopy; Ultraviolet Photoelectron Spectroscopy IBM Almaden Research Center San Jose,... Zaluzec Argonne National Laboratory Argonne, IL Electron Energy-Loss Spectroscopy in the Transmission Electron Microscope Contributors xix I INTRODUCTION AND SUMMARIES 1. 0 INTRODUCTION Though a wide range of analytical techniques is covered in this volume there are certain traits common to many of them Most involve either electrons, photons, or ions as a probe beam striking the material to be analyzed The... Olesik Ohio State University Columbus, OH InductivelyCoupled Plasma-Optical Emission Spectroscopy Fred H Pollak Brooklyn College, CUNY New York, NY Modulation spectroscopy Thomas P Russell IBM A l d e n Research Center San Jose, CA Neutron Reflectivity Donald E Savage University of Wisconsin Madison, W I Reflection High-EnergyElectron Diffraction K r E Si& ut Los Alamos National Laboratory LosAlamos,NM... 3 1 Y a a m 1Pn 0 o 0 m a m 1 nm a 3A 1o ow Few % All, m s l polymer oty Y 3 2 Y 3A 10 0 nrn PPb-PPrn AU, mostly inorg Y 3 3 N Compilation of Comparative Information on the AnalyticalTechniques Discussedin This Volume 0, 6 Maill ~ n l l a t i ~ Depth probed (typical) ArrideTechnique No 10 .4 10 .5 10 .6 10 .7 10 .8 10 .9 2 0 0 C 0 : z v) P U GDMS ICPMS ICPOES ll.' 5 SNMS LIMS ;E20ll 11 .2 ;l;g;v SSMS 11 .3... foils in TEM Main use To add analytical capability to SEM, EPMA and TEM cost $25,000- $10 0,000, depending on accessories (not including the electron microscope) 11 Electron Energy-Loss Spectroscopy in the Transmission Electron Microscope (EELS) 1. 3.2 In Electron Energy-Loss Spectroscopy (EELS) a nearly monochromatic beam of electrons is directed through an ultrathin specimen, usually in a Transmission... transparent to electrons and 10 0-2000 thick - a Main use Light element spectroscopy for concentration, electronic, and chemical structure andysis at ultrahigh lateral resolution in a TEM or STEM cost As an accessory to a TEM or STEM: $50,000 $15 0,000 (does not include electron microscope cost) 12 INTRODUCTIONAND SUMMARIES Chapter 1 Cathodoluminescence (CL) 1. 3.3 In Cathodoluminescence (CL) analysis, electron-beam . Post-Ionization Secondary Ion Mass Spectrometry Multi-Photon Nonresonant Post Ionization Multiphoton Resonant Post Ionization Resonant Post Ionization Multi-Photon Ionization Single-Photon Ionization. Atomic Absorption Spectroscopy Atomic Absorption Vapor Phase Decomposition-Atomic Absorption Spectroscopy Graphite Furnace Atomic Absorption Flame Atomic Absorption Auger Electron Spectroscopy. Loss Spectroscopy High-Resolution Electron Energy-Loss Spectroscopy Reflected Electron Energy-Loss Spectroscopy Reflection Electron Energy-Loss Microscopy Low-Energy Electron-Loss Spectroscopy