_STP_596-1976.pdf

SURFACE ANALYSIS TECHNIQUES FOR METALLURGICAL APPLICATIONS A symposium sponsored by ASTM Subcommittee E02.02 on Surface Analysis of ASTM Committee E-2 on Emission Spectroscopy AMERICAN SOCIETY FOR TESTING AND MATERIALS Cleveland,Ohio,4 March 1975 ASTM SPECIAL TECHNICAL PUBLICATION 596 R.S.Carbonara and J.R.Cuthill,editors List price$15.00 04-596000-28 AMERICAN SOCIETY FOR TESTING AND MATERIALS 1916 Race Street,Philadelphia,Pa.19103 by American Society for Testing and Materials 1976 Library of Congress Catalog Card Number:75-39442 NOTE The Society is not responsible,as a body,for the statements and opinions advanced in this publication.Printed in Baltimore,Md.March 1976 Foreword The symposium on Surface Analysis Techniques for Metallurgical Applications was held in conjunction with the 1975 Pittsburgh Analytical Conference in Cleveland,Ohio,4 March 1975.Subcommittee E02.02 on Surface Analysis of Committee E-2 on Emission Spectroscopy sponsored the symposium.G.L.Mason,Canada Center for Mineral and Energy Technology,served as organizing chairman of the symposium.J.R.Cuthill,National Bureau of Standards,presided as symposium chairman at the morning session,and A.H.Gillieson,Canada Center for Mineral and Energy Technology,presided at the afternoon session.R.S.Carbonara,Battelle Columbus Laboratories,and R.J.Koch,Armco Steel Corporation,along with Mason and CuthiU,served as the symposium committee.Related ASTM Publications Metallography-A Practical Tool for Correlating the Structural Properties of Materials,STP 557(1974),$24.25,04-557000-28 Manual on Electron Metallography Techniques,STP 547(1973),$5.25,04-547000-28 Electron Beam Microanalysis,STP 506(1972),$3.75,04-506000-28 A Note of Appreciation to Reviewers This publication is made possible by the authors and,also,the unheralded efforts of the reviewers.This body of technical experts whose dedication,sacrifice of time and effort,and collective wisdom in review-ing the papers must be acknowledged.The quality level of ASTM publications is a direct function of their respected opinions.On behalf of ASTM we acknowledge their contribution with appreciation.ASTM Committee on Publications Editorial Staff Jane B.Wheeler,Managing Editor Helen M.Hoersch,Associate Editor Charlotte E.DeFranco,Senior Assistant Editor Ellen J.McGlinchey,Assistant Editor Contents Introduction Chemical Analysis of Surfaces-R.L.PARK Some Quantitative Aspects of the X-Ray Photoelectron Spectroscopy Analysis of Metal and Oxide Surfaces-N.s.MCINTYRE AND M.G.COOK ESCA Studies of Nickel-Boron Electroless Coatings-R.s.SWINGLE,II,C.R.GINNARD,AND G.I.MADDEN Composition of Protective Films Formed on Iron and Stainless Steeis-J.B.LUMSDEN AND R.W.STAEHLE Quantitative Auger Electron Spectroscopy with Elemental Sensitivity Factors-L.E.DAVIS AND A.JOSHI Application of Anger Electron Spectroscopy to the Study of Embrlttlement in Niekel-J.M.WALSH AND N.P.ANDERSON Determination of the Low Temperature Diffusion of Chromium Through Gold Films by Ion Scattering Spectroscopy and Auger Electron Spectroscopy-G.C.NELSON AND P.H.HOLLOWAY Comparison of Evaporated Surface Coatings Using the Ion Scattering Spectrometer and the Auger Electron Spectrometer-w.D.BINGLE Chemistry of Metal and Alloy Adherends by Secondary Ion Mass Spectroscopy,Ion Scattering Spectroscopy,and Auger Electron Spectroscopy-w.L.BAUN,N.T.MCDEVITT,AND J.S.SOLOMON Errors Observed in Quantitative Ion Microprobe Analysis-D.E.NEWBURY,K.F.J.HEINRICH,AND R.L.MYKLEBUST Small Area Depth Profiling with the Ion Microprobe-T.A.WHATLEY,D.J.COMAFORD,JOHN COLBY,AND PAUL MILLER Analysis of Solids Using A Quadrupole Mass Fiiter-R.D.FRALICK,H.J.RODEN,AND J.R.HINTHORNE Summary Index 18 28 39 52 58 68 79 86 101 114 126 141 145 STP596-EB/Mar.1976 Introduction The 12 papers in this volume,which were presented at the Symposium on Surface Analysis Techniques for Metallurgical Applications in Cleve-land,March 1975,embrace the following four surface analysis techniques:(1)ion scattering spectroscopy(ISS),(2)Auger electron spectroscopy(AES),(3)electron spectroscopy for chemical analysis(ESCA),which is also known as X-ray-induced electron spectroscopy(XPS),and(4)ion microprobe mass analysis/secondary ion mass spectroscopy(IMMA/SIMS).These techniques,using commercial equipment,have been per-fected only during the last decade.These are powerful analytical techniques that have been shown to have application to many types of metallurgical problems that are dependent upon surface composition.Their use is now expanding beyond the bounds of the fundamental research laboratories and into industrial control laboratories.This has prompted the establishment of ASTM Subcommittee E02.02 on Surface Analysis.This symposium,presenting state-of-the-art applications of these surface analysis techniques to an illustrative range of metallurgical surface problems,was one of the first activities of this Subcommittee.But the purpose of this symposium was more than just to illustrate the range of app